A method for full-field high-throughput in-situ characterization of microstructure of ceramic materials across scales

Abstract

The application discloses a kind of ceramic material microstructure full field of view high flux cross-scale in-situ characterization method, comprising: ceramic and ceramic matrix composite sampling and cutting;Ceramic and ceramic matrix composite mechanical grinding and surface polishing;Ceramic sample test area positioning mark;Ceramic and ceramic matrix composite sample to be measured region surface three-dimensional topography height information high flux high-precision acquisition;Surface three-dimensional topography height information acquisition result post-processing and analysis, obtain a kind of ceramic and ceramic matrix composite microstructure full field of view high flux cross-scale in-situ characterization method.The application is based on ceramic material surface metallographic polishing, combined with white light interferometer test surface three-dimensional topography height information and acquisition information result filtering analysis and other post-processing, realize based on ceramic and ceramic matrix composite composition phase three-dimensional surface information difference analysis microstructure full field of view high flux cross-scale in-situ characterization.

Description

Technical Field

[0001] This invention relates to the field of high-throughput analysis and characterization of material microstructure, and particularly to a full-field, high-throughput, multi-scale, in-situ characterization method for the microstructure of ceramic materials. Background Technology

[0002] Material microstructure analysis and characterization techniques serve as a fundamental supporting technology for materials research and new materials development, providing an important pathway for revealing the internal structural characteristics of materials. To date, various material microstructure analysis and characterization techniques have been developed based on different principles. Examples include optical microscopes invented based on the principles of light reflection, transmission, and diffraction coherence; scanning electron microscopes (SEM), transmission electron microscopes (TEM), and scanning transmission electron microscopes (STEM) that receive information containing material structure based on the interaction between a focused electron beam and matter; and synchrotron radiation three-dimensional microstructure characterization techniques based on high-energy X-ray diffraction.

[0003] With the widespread attention given to the Materials Genome Initiative in recent years, its "data-driven" approach and the goal of halving both the R&D cycle and cost have become important guiding principles for the future development of new materials. Against the backdrop of the rise of the Materials Genome Initiative, developing novel microstructure analysis and characterization methods based on high-throughput principles has become a crucial approach for accurate, efficient, rapid, and comprehensive analysis. New high-throughput microstructure characterization technologies, such as high-throughput optical metallurgical microscopy and high-throughput field emission scanning electron microscopy, offer analytical and characterization efficiencies several times greater than traditional optical or field emission scanning electron microscopy. They enable high-precision and rapid characterization of the microstructure across the entire field of view, providing impetus and technical support for accelerating materials R&D. Developing new high-throughput microstructure characterization technologies provides powerful scientific research tools for new materials research. This invention utilizes high-precision acquisition technology of three-dimensional morphology height information of material surfaces (such as white light interferometry three-dimensional profilometry), combined with the analysis and processing of three-dimensional morphology height information data, to provide a new method for high-throughput characterization of the microstructure of ceramics and ceramic matrix composites across the entire field of view. Since the hardness and wear resistance of each phase in ceramics and ceramic matrix composites differ, the degree of wear of each phase is slightly different during the grinding and polishing process. By collecting three-dimensional surface height information and combining it with data processing software analysis, it is expected to obtain correlated data results that reflect the microstructure information, and realize the full-field high-throughput in-situ analysis and characterization of the microstructure of ceramics and ceramic matrix composites. Summary of the Invention

[0004] To address the existing technical problems, the purpose of this invention is to provide a full-field, high-throughput, multi-scale, in-situ characterization method for the microstructure of ceramic materials. Based on mechanical grinding and surface polishing of ceramics and ceramic matrix composites, a white light interferometer is used to acquire the three-dimensional morphology height information of the material surface in a full-field, high-throughput manner. Commercial data processing software is used to filter, analyze, and interpret the acquired data. By detecting the differences in the three-dimensional morphology data of each phase of the ceramic composition, the two-dimensional morphology information of the material's microstructure is reflected, thus achieving full-field, high-throughput, multi-scale, and in-situ analysis and characterization of ceramics and ceramic matrix composites.

[0005] To achieve the above-mentioned technical objectives, this invention provides a high-throughput, multi-scale, in-situ characterization method for the microstructure of ceramic materials across the entire field of view, comprising the following main steps:

[0006] Ceramic materials are sampled and cut to generate sample materials;

[0007] After preprocessing the sample material, high-throughput and high-precision acquisition of the three-dimensional surface height information of the entire field of view is performed to obtain the three-dimensional surface height information of each constituent phase of the sample material;

[0008] Based on the differences in three-dimensional surface height information, the two-dimensional microstructure of the same region corresponding to the three-dimensional surface height information is characterized.

[0009] Preferably, in the process of generating sample materials, the ceramic material is ceramic or ceramic-based material;

[0010] Based on the shape, hardness, wear resistance, conductivity, and sampling location or direction requirements of the ceramic material, sampling rules are formulated. By selecting the sample cutting method and setting the processing parameters, the ceramic material is sampled and cut.

[0011] Preferably, during the pretreatment of the sample material, the cross-section of the sample material is ground by using sandpaper and polishing liquid, and setting the abrasive particle size, so that the cross-section achieves a mirror-like reflective gloss and no obvious scratches are observed under an optical microscope, thus meeting the characterization requirements.

[0012] Preferably, after pretreatment of the sample material, the surface of the sample material is marked using a microhardness tester and a nanoindenter. When the surface feature areas of the sample material are numerous and easily identifiable, the marking may not be necessary.

[0013] Based on the sample material after positioning and marking, obtain the three-dimensional surface height information.

[0014] Preferably, in the process of characterizing the two-dimensional microstructure, the three-dimensional surface height information is processed by filtering analysis, etc., to retain the local height information of the microstructure in the micro-region. By the difference in the three-dimensional height information of the wear of each component phase, the two-dimensional microstructure of each component phase in the approximate projection area is obtained. By adjusting the Z-axis display height, the full field-of-view high-throughput characterization of the microstructure of the sample material is obtained, which is used to characterize the two-dimensional microstructure of the sample material.

[0015] Preferably, the characterization system for realizing a high-throughput, multi-scale, in-situ characterization method for the full field of view of ceramic material microstructure includes:

[0016] The sample cutting module is used to sample and cut ceramic materials to generate sample materials;

[0017] The sample preprocessing module is used to preprocess sample materials;

[0018] The data acquisition module is used to perform high-throughput and high-precision acquisition of the surface three-dimensional height information of the preprocessed sample material across the entire field of view, and to obtain the three-dimensional surface height information of each constituent phase of the sample material.

[0019] The two-dimensional microstructure characterization module is used to characterize the two-dimensional microstructure of the same region corresponding to the three-dimensional surface height information based on the differences in three-dimensional surface height information.

[0020] The display module is used to display three-dimensional surface height information and two-dimensional microstructure.

[0021] The present invention discloses the following technical effects:

[0022] First, compared with traditional microstructure analysis and characterization techniques, such as scanning electron microscopy and optical microscopy, its characterization speed, efficiency, and sample size are greatly improved. It utilizes a white light interferometer to achieve high-throughput and high-precision acquisition of centimeter-level sample surface composition phase wear height information differences across the entire field of view.

[0023] Secondly, since the sample contour shape information interferes with the high-throughput characterization of local height information, in order to achieve full-field, high-throughput, cross-scale, and in-situ characterization of the sample's two-dimensional microstructure, this invention uses analytical characterization, such as filtering analysis of the differences in three-dimensional height information of each component phase on the polished surface of ceramic materials, to filter the sample's macroscopic shape information and retain local height information. By selectively displaying this information, the three-dimensional height information can be approximately projected into two-dimensional microstructure information, thus achieving full-field, high-throughput, cross-scale, and in-situ characterization of the sample's two-dimensional microstructure.

[0024] Third, the present invention has the advantages of no need for vacuuming, no need for gold / carbon / platinum spraying, no damage, direct observation, clearer display, and high-throughput characterization of any micro-area in the full field of view of the sample. Attached Figure Description

[0025] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0026] Figure 1 This is a flowchart illustrating a specific implementation of the present invention;

[0027] Figure 2 This invention provides a full-field, high-throughput, high-precision acquisition (contour map) of the three-dimensional morphology height information of the polished surface region of the directional solidified B4C-TiB2 eutectic ceramic self-generated composite material section as described in this embodiment.

[0028] Figure 3 for Figure 2 The elevation information along the cut line is shown in the three-dimensional elevation information contour map of the area shown.

[0029] Figure 4 The result (contour map) is the result of filtering and analysis of the three-dimensional morphology height information of the self-generated B4C-TiB2 eutectic ceramic composite material surface described in the embodiments of the present invention.

[0030] Figure 5 The image shows local area information (contour map) after filtering and analyzing the three-dimensional morphology height information of the self-generated B4C-TiB2 eutectic ceramic composite material surface described in the embodiments of the present invention.

[0031] Figure 6 for Figure 5 Changes in the height of the region along the intercept;

[0032] Figure 7 This is a selective display of micro-area information after filtering and analysis of the three-dimensional morphology height information of the directionally solidified B4C-TiB2 eutectic ceramic composite material surface described in this embodiment of the invention. Figure 5 (corresponding area);

[0033] Figure 8 The image shows the light intensity distribution grayscale of the directional solidification B4C-TiB2 eutectic ceramic composite material described in this embodiment of the invention. Figure 5 (corresponding area);

[0034] Figure 9These are scanning electron microscope (SEM) images of the micro-area corresponding to the directional solidification B4C-TiB2 eutectic ceramic composite material described in the embodiments of the present invention. Detailed Implementation

[0035] To make the objectives, technical solutions, and advantages of the embodiments of this application clearer, the technical solutions of the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this application, and not all embodiments. The components of the embodiments of this application described and shown in the accompanying drawings can generally be arranged and designed in various different configurations. Therefore, the following detailed description of the embodiments of this application provided in the accompanying drawings is not intended to limit the scope of the claimed application, but merely represents selected embodiments of this application. All other embodiments obtained by those skilled in the art based on the embodiments of this application without inventive effort are within the scope of protection of this application.

[0036] like Figure 1-9 As shown, this invention provides a high-throughput, multi-scale, in-situ characterization method for the microstructure of ceramic materials across the entire field of view, comprising the following main steps:

[0037] Ceramic materials are sampled and cut to generate sample materials;

[0038] After preprocessing the sample material, high-throughput and high-precision acquisition of the three-dimensional surface height information of the entire field of view is performed to obtain the three-dimensional surface height information of each constituent phase of the sample material;

[0039] Based on the differences in three-dimensional surface height information, the two-dimensional microstructure of the same region corresponding to the three-dimensional surface height information is characterized.

[0040] More preferably, in the process of generating sample materials, the ceramic material is ceramic or ceramic-based material;

[0041] Based on the shape, hardness, wear resistance, conductivity, and sampling location or direction requirements of the ceramic material, sampling rules are formulated. By selecting the sample cutting method and setting the processing parameters, the ceramic material is sampled and cut.

[0042] More preferably, during the pretreatment of the sample material, the cross-section of the sample material is ground using sandpaper and polishing liquid (with selected abrasive particle size) to achieve a mirror-like reflective gloss and to ensure that no obvious scratches are observed under an optical microscope, thus meeting the requirements for testing and characterization.

[0043] More preferably, after pretreatment of the sample material, the surface of the sample material is marked using a microhardness tester and a nanoindenter. When the surface feature areas of the sample material are numerous and easily identifiable, the marking may not be necessary.

[0044] Based on the sample material after positioning and marking, obtain the three-dimensional surface height information.

[0045] More preferably, in the process of characterizing the two-dimensional microstructure, the three-dimensional surface height information is filtered and analyzed. By the difference in the three-dimensional height information of the wear of each component phase, the two-dimensional microstructure of each component phase in the approximate projection area is obtained. By adjusting the Z-axis display height, the full-field high-throughput characterization of the microstructure of the sample material is obtained, which is used to characterize the two-dimensional microstructure of the sample material.

[0046] This invention also discloses a full-field, high-throughput, multi-scale in-situ characterization system for the microstructure of ceramic materials, comprising:

[0047] The sample cutting module is used to sample and cut ceramic materials to generate sample materials;

[0048] The sample preprocessing module is used to preprocess sample materials;

[0049] The data acquisition module is used to perform high-throughput and high-precision acquisition of the surface three-dimensional height information of the pre-processed ceramic and ceramic-based sample materials across the entire field of view, and to obtain the three-dimensional surface height information of each constituent phase of the sample material.

[0050] The two-dimensional microstructure characterization module is used to characterize the two-dimensional microstructure of the same region corresponding to the three-dimensional surface height information based on the differences in three-dimensional surface height information.

[0051] The display module is used to display three-dimensional surface height information and two-dimensional microstructure.

[0052] This invention provides a full-field, high-throughput, multi-scale, in-situ characterization method for the microstructure of ceramic materials. It involves mechanically grinding and polishing ceramics and ceramic matrix composites to obtain a mirror-smooth polished surface. Combined with a white-light interferometric 3D profilometer, it acquires full-field, high-throughput, and high-precision three-dimensional surface height information of the polished ceramic sample. Using commercial data processing software, through filtering and other data analysis methods, it obtains a full-field, high-throughput characterization of the ceramic sample surface's three-dimensional information. The differences in three-dimensional height information of the wear surfaces of the constituent phases reflect the corresponding microstructure (three-dimensional wear surface information → two-dimensional microstructure information projection), achieving full-field, high-throughput characterization of the ceramic material's microstructure. This method breaks through the traditional imaging principle of optical microscopy by utilizing the differences in three-dimensional height information due to different wear properties of the constituent phases for processing and analysis, obtaining an approximate projection of a two-dimensional microstructure image. It is convenient, fast, efficient, and non-destructive. Simultaneously, the data processing software allows for rapid quantitative analysis of large amounts of acquired data, providing a new full-field, high-throughput, multi-scale, in-situ characterization technique for the comprehensive analysis of the microstructure of large-size samples.

[0053] like Figure 1 The diagram shows the implementation flowchart of a full-field, high-throughput, multi-scale in-situ characterization method for the microstructure of ceramic materials according to the present invention. In this embodiment, a directionally solidified B4C-TiB2 binary eutectic ceramic self-generated composite material is used as the ceramic matrix composite material test object. Through sampling and cutting of the ceramic sample, mechanical grinding and surface polishing, full-field, high-throughput, high-precision acquisition of surface three-dimensional morphology height information, and full-field surface three-dimensional morphology height information filtering analysis, the method achieves the acquisition of three-dimensional morphology height information of the worn surface of the ceramic and ceramic matrix composite materials and the approximate projection of the two-dimensional microstructure. This enables full-field, high-throughput, multi-scale in-situ analysis and characterization of the two-dimensional microstructure of the ceramic matrix composite material in the same region. The specific implementation includes the following steps:

[0054] Step 1: To characterize the microstructure of the directionally solidified B4C-TiB2 binary eutectic ceramic self-generated composite material, the rod-shaped directionally solidified B4C-TiB2 binary eutectic ceramic self-generated composite material prepared by the optical suspension zone melting method was selected, and the ceramic material was cut along its cross-sectional direction using a wire cutting device to obtain the cross-section of the ceramic sample.

[0055] Step two: For the cut B4C-TiB2 eutectic ceramic self-generated composite material sample, select appropriate sandpaper type and grade, polishing paste / slurry type, and abrasive particle size. In this experiment, silicon carbide sandpaper was selected, with sandpaper grades of 100#, 200#, 400#, 800#, 1200#, 1500#, and 2000#. The polishing slurry was selected as silica or diamond suspension, with abrasive particle sizes of 2.0 μm, 1.5 μm, and 0.5 μm, respectively. The polishing process was set to achieve a mirror-like reflective gloss on the sample surface, with no obvious scratches observed under an optical microscope, meeting the characterization requirements of this method.

[0056] Step 3: Based on the sample size, shape, hardness, and marking requirements, use a microhardness tester to select an appropriate load and holding time to mark the test area on the sample surface. Since this sample has many characteristic areas (cracks, etc.) that are easy to identify, no positioning marking is required.

[0057] Step 4: Using a white light interferometer (Bruker ContourGT-K), set appropriate acquisition parameters according to the size of the acquisition area and the typical size of the microstructure, and perform high-throughput and high-precision acquisition of the surface three-dimensional morphology height information of the sample area to be tested across the entire field of view.

[0058] Step 5: Use commercial 3D surface morphology information data software (Vision64) to perform filtering and other analysis on the collected 3D surface morphology height information of the ceramic sample.

[0059] Step 6: Based on the filtering analysis results and referring to the statistical distribution law of three-dimensional height, the full-field high-throughput cross-scale in-situ characterization of the two-dimensional microstructure of the corresponding region of the directional solidified B4C-TiB2 eutectic ceramic is obtained by setting the display parameters and analyzing the three-dimensional morphology height information of the ceramic material surface.

[0060] like Figure 2 The image shown is a contour map obtained by high-throughput and high-precision acquisition of the three-dimensional morphology height information of the surface of the directionally solidified B4C-TiB2 eutectic ceramic self-generated composite material using a white light interferometer. Since the results include macroscopic contour height information of the sample, it is not possible to directly achieve differentiated display of different phases by uniformly setting the Z-axis height. In order to achieve unified processing of wear height information corresponding to microstructure, it is necessary to separate the wear height information of the microstructure constituent phases from the macroscopic shape information of the sample and filter the macroscopic contour information of the sample.

[0061] like Figure 3 As shown Figure 2The height information along the cross section in the contour map changes (after leveling, the cross section length L is approximately 4.1 mm). It can be seen that due to the arc-shaped contour of the sample with a high center and low edges after grinding and polishing, the sample as a whole has a certain height difference Δh. It can be seen that Δh can reach about 11 μm in this sample. This size is much larger than the wear height difference of the eutectic phase. Therefore, when the Z-axis is set to a uniform height, the contour information has a significant impact on the three-dimensional height information difference of different phases. In order to achieve full-field high-throughput cross-scale observation and in-situ characterization, this contour information is removed.

[0062] like Figure 4 The image shows the filtering and analysis of the surface three-dimensional information acquisition results. The macroscopic contour information of the ceramic sample is filtered out, and the two-dimensional microstructure of each component phase in the approximate projection area is reflected by the difference in the three-dimensional height information of the wear of each component phase. The Z-axis display height is adjusted to obtain the full field high-throughput characterization of the microstructure of the self-generated composite material of directional solidified B4C-TiB2 eutectic ceramic.

[0063] like Figure 5 The image shows the full-field three-dimensional height information filtering analysis of the directionally solidified B4C-TiB2 eutectic ceramic self-generated composite material. Figure 4 The magnified results of a local micro-area show that the microscopic structural features can be clearly displayed through selected area magnification.

[0064] like Figure 6 As shown Figure 5 The height information changes along the cut-off line within the region. The results show that after filtering analysis, the arc-shaped contour features (low-frequency information) of the sample have been filtered out, while the wear height difference information of the constituent phases (high-frequency information) has been preserved.

[0065] like Figure 7 The image shows the phase composition of a local micro-region as characterized by full-field high-throughput characterization of the microstructure of directionally solidified B4C-TiB2 eutectic ceramics.

[0066] like Figure 8 As shown Figure 5 The grayscale image of the light intensity in the same region was obtained by acquiring data using a white light interferometer 3D profilometer (Vision64). The results show that... Figure 2 ~Figure 7 shows that the two-dimensional microstructure morphology obtained by the three-dimensional morphology information analysis is in good agreement with the microstructure morphology observed by optical observation in the corresponding area, indicating that the method of the present invention can be used for full-field high-throughput cross-scale in-situ characterization of the microstructure of ceramics and ceramic matrix composites.

[0067] like Figure 9 The image shown is obtained using a high-throughput scanning electron microscope. Figure 5 , Figure 7Backscattered electron images of microstructures in micro-regions show that the microstructures obtained by this method are in good agreement with the results of scanning electron microscopy, indicating that the method of this invention can be used for high-throughput, multi-scale in-situ characterization of the microstructures of ceramics and ceramic matrix composites across the entire field of view.

[0068] It should be noted that similar labels and letters in the following figures indicate similar items. Therefore, once an item is defined in one figure, it does not need to be further defined and explained in subsequent figures. In addition, the terms "first", "second", "third", etc. are used only to distinguish descriptions and should not be construed as indicating or implying relative importance.

[0069] Finally, it should be noted that the above-described embodiments are merely specific implementations of the present invention, used to illustrate the technical solutions of the present invention, and not to limit it. The scope of protection of the present invention is not limited thereto. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that any person skilled in the art can still modify or easily conceive of changes to the technical solutions described in the foregoing embodiments within the technical scope disclosed in the present invention, or make equivalent substitutions for some of the technical features; and these modifications, changes, or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention. All should be covered within the scope of protection of the present invention. Therefore, the scope of protection of the present invention should be determined by the scope of the claims.

Claims

1. A method for microstructure full-field high-throughput cross-scale in-situ characterization of ceramic materials, characterized in that, The method comprises the following steps: sampling and cutting the ceramic material to generate sample material; the ceramic material is a directional solidification B4C-TiB2 eutectic ceramic autogenous composite material; after pretreating the sample material, using a white light interference three-dimensional profiler to collect high-precision surface three-dimensional height information of the sample material in a full field of view; during the pretreatment of the sample material, the cross section of the sample material is ground using sandpaper, polishing liquid, and setting the size of the grinding particles to achieve mirror reflection and no obvious scratches under an optical microscope, meeting the characterization requirements; after pretreating the sample material, the surface of the sample material is marked using a microhardness tester and a nanoindenter, and when the surface feature area of the sample material is large and easy to identify, no marking is performed; the full field of view three-dimensional surface height information is obtained according to the sample material after marking; while obtaining the three-dimensional surface height information, the microstructure composition phase abrasion local height information of the sample material is segmented with the sample macro shape information, the sample macro profile information is filtered, and the three-dimensional surface height information is generated; according to the difference of the three-dimensional surface height information, the two-dimensional microstructure structure of the same region corresponding to the three-dimensional surface height information is characterized; during the characterization of the two-dimensional microstructure structure, the three-dimensional surface height information is analyzed and processed by filtering, the two-dimensional microstructure structure characteristics of each composition phase in the projection area are obtained through the difference of the abrasion three-dimensional height information of each composition phase, and the microstructure structure full field of view high throughput characterization of the sample material is obtained by adjusting the display height of the Z axis, which is used to characterize the two-dimensional microstructure structure of the sample material.

2. The ceramic material microstructure full field of view high throughput cross-scale in-situ characterization method according to claim 1, characterized in that: according to the shape, hardness, wear resistance, electrical conductivity, sampling site or direction requirements of the ceramic material, a sampling rule is formulated, a sample cutting method is selected, and processing parameters are set to sample and cut the ceramic material.

3. The ceramic material microstructure full field of view high throughput cross-scale in-situ characterization method according to claim 2, characterized in that: during the generation of the sample material, the ceramic material is cut using a wire cutting device to obtain the sample material.

4. The ceramic material microstructure full field of view high throughput cross-scale in-situ characterization method according to claim 1, characterized in that: a characterization system for realizing the ceramic material microstructure full field of view high throughput cross-scale in-situ characterization method comprises: a sample cutting module for sampling and cutting the ceramic material to generate sample material; a sample pretreatment module for pretreating the sample material; a data acquisition module for collecting high-precision surface three-dimensional height information of the pretreated sample material in a full field of view, obtaining three-dimensional surface height information of each composition phase of the sample material; A two-dimensional microstructure characterization module is configured to characterize a two-dimensional microstructure of a same region corresponding to the three-dimensional surface height information according to a difference of the three-dimensional surface height information. A display module is configured to display the three-dimensional surface height information and the two-dimensional microstructure.

Images