CN110567998A - Sample preparation method for rapidly obtaining silicon carbide ceramic crystal grain information and analysis and determination method thereof - Google Patents
Sample preparation method for rapidly obtaining silicon carbide ceramic crystal grain information and analysis and determination method thereof Download PDFInfo
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Abstract
the invention provides a sample preparation method for rapidly obtaining crystal grain information of silicon carbide ceramics, and an analysis and determination method thereof, in particular to a method for preparing a silicon carbide ceramic cross section sample observed by a scanning electron microscope by utilizing an ion beam cross section polishing technology, which comprises the following steps: performing ion beam cross section polishing on the silicon carbide ceramic to obtain a silicon carbide ceramic cross section sample; the parameters of the ion beam cross section polishing comprise: the acceleration voltage of the ion beam is 5-8 kV; the sample polishing time is 120-300 minutes; the current is 1.5-3 mA.
Description
Technical Field
The invention relates to a sample preparation method for rapidly obtaining silicon carbide ceramic crystal grain information and an analysis and determination method thereof, in particular to a method for preparing silicon carbide ceramic crystal grains observed by a scanning electron microscope by using an ion beam cross section polishing technology, and a method for rapidly analyzing and measuring the sizes, the holes, the distribution and the components of a second phase and the like of the silicon carbide ceramic crystal grains by using the scanning electron microscope and an energy spectrometer, belonging to the field of microstructure test and analysis of ceramic materials.
Background
The silicon carbide ceramic has a plurality of excellent performances such as high melting point, high strength, high hardness, corrosion resistance, wear resistance, oxidation resistance, small thermal expansion coefficient, high thermal conductivity and the like, can bear a severe working environment which is hard to be met by metal or high polymer materials, and has great application value and potential application prospect in a plurality of industrial fields. However, silicon carbide itself is a strongly covalent bond compound, and the self-diffusion rate of Si and C atoms is very low even at high temperatures, so that sintering is very difficult. In order to promote the sintering densification of SiC ceramics, it is often necessary to add a sintering aid. The sintering of SiC ceramics can be divided into solid phase sintering and liquid phase sintering, depending on whether the additive forms a liquid phase during the sintering process. The two sintering modes have obvious difference in sintering temperature and densification mechanism, so that the mechanical property and the microstructure are different. The solid phase sintering temperature is higher, so that SiC crystal grains are coarse, and the bending strength and the fracture toughness are lower. The liquid phase sintering can obviously reduce the sintering temperature, the SiC ceramic with a fine crystal structure is obtained, and the bending strength and the fracture toughness are obviously improved. The second phase formed by the air holes and the sintering aid can also greatly influence the mechanical, thermal and electrical properties of the SiC ceramic. Therefore, observing the microstructure characteristics such as grain size, grain size distribution, second phase distribution, pores and the like in the ceramic by a scanning electron microscope is an effective way for understanding the structure-activity relationship of the material, thereby optimizing the material performance.
The current sample preparation method for obtaining information about grains, pores and second phases (usually various sintering aids) in silicon carbide ceramics by using a scanning electron microscope comprises the following steps: natural section method, observation after mechanical polishing and thermal etching, and Electron Back Scattering Diffraction (EBSD). The natural section method is the most commonly used method for researching the internal microstructure or mechanical fracture mode of SiC ceramics at present, and is very simple, practical and intuitive for SiC ceramics fractured along the crystal, but has very limited information for SiC ceramics fractured through the crystal. The polished surface can present rich information such as the morphology, the size, the pores, the distribution of the second phase, the crack propagation path and the like of grains. In the past, before observing the polished surface, the sample is usually placed in a molten NaOH solution for corrosion so as to enable the grain boundary outline to be clearer. However, because the chemical stability of the SiC ceramic is still extremely high in strong corrosive environments such as strong alkali, the search for corrosion conditions (corrosion temperature, time) is difficult, under-corrosion or over-corrosion is easily caused when the corrosion conditions are not good, SiC ceramic grains cannot be observed under the under-corrosion condition, and the artifact is generated when the corrosion is excessive, it is difficult to observe the microstructure such as grains, a second phase and the like of the polished SiC ceramic through hot corrosion; in addition, when mechanical polishing is performed, due to the difference in hardness of different phases, a grain extraction phenomenon is easily generated, so that it is difficult to obtain real microstructure information. The electron backscatter diffraction (EBSD) method calibrates crystal orientation by collecting backscatter diffraction signals, i.e., chrysanthemum cell patterns, and can accurately determine the crystal orientation, but has a severe requirement on sample pretreatment, and firstly, the sample surface needs to be flat, stress-free and clean, which requires vibration polishing or ion beam polishing after sample cutting and mechanical polishing, and simultaneously requires that the sample has good conductivity; after the sample is qualified, a complete data can be acquired for several hours according to the acquisition area and the grain size; and finally, carrying out noise reduction post-processing such as noise reduction and small crystal grain removal on the acquired data. The whole process is complex, the influencing factors are various, and the time consumption is long.
disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a method for preparing a silicon carbide ceramic cross section sample suitable for being observed by a scanning electron microscope by using an ion beam cross section polishing technology, and a novel method for observing the shape and the size of crystal grains in the silicon carbide ceramic cross section sample, and the distribution and the components of holes and second phases in the silicon carbide ceramic by using the scanning electron microscope and an energy spectrometer.
On one hand, the invention provides a method for preparing a silicon carbide ceramic cross-section sample observed by a scanning electron microscope by using an ion beam cross-section polishing technology, wherein the silicon carbide ceramic is subjected to ion beam cross-section polishing to obtain the silicon carbide ceramic cross-section sample; the parameters of the ion beam cross section polishing comprise: the acceleration voltage of the ion beam is 5-8 kV; the sample polishing time is 120-300 minutes; the current is 1.5-3 mA.
Preferably, before the ion beam cross section polishing, an automatic internal circle cutting machine is used, a diamond blade is selected, the cutting speed is set, and the silicon carbide ceramic is cut into a proper size.
Preferably, the sample stage loaded with the silicon carbide ceramic is placed in an argon ion beam polishing instrument, and the silicon carbide ceramic is tightly attached to the baffle plate, so that the ion beam polishes the silicon carbide ceramic. At the moment, an inner circle cutting machine is used for cutting the silicon carbide ceramic into a proper size, and the silicon carbide ceramic is fixed on a sample table of an ion beam polishing machine, wherein the size of the silicon carbide ceramic is controlled within the limit range of the ion beam polishing machine.
In another aspect, the present invention further provides a method for rapidly analyzing and measuring the grain size, pores, second phase distribution and second phase composition in the silicon carbide ceramic cross-section sample, including:
Carrying out scanning electron microscope test on the silicon carbide ceramic cross section sample to obtain an electron channel contrast image and a secondary electron image of the silicon carbide ceramic cross section sample;
Carrying out energy spectrum instrument test on the silicon carbide ceramic cross section sample to obtain the energy spectrum surface distribution result of the silicon carbide ceramic cross section sample;
and judging the grain size, the pores, the second phase distribution and the second phase component of the silicon carbide ceramic according to the obtained electronic channel contrast image, the secondary electron image and the energy spectrum surface distribution result.
In the disclosure, the silicon carbide ceramic cross-section sample prepared by the above method is subjected to a scanning electron microscope test and an energy spectrometer test, and an electron channel contrast image, a secondary electron image and an energy spectrometer surface distribution result of the silicon carbide ceramic cross-section sample are obtained. And qualitatively determining the shape and size of the silicon carbide ceramic crystal grains and the distribution and composition information of the holes and the second phases in the silicon carbide ceramic according to the electron channel contrast image, the secondary electron image and the energy spectrometer surface distribution result of the obtained silicon carbide ceramic cross section sample.
Preferably, when obtaining the contrast image or the secondary electron image of the electron channel, the testing parameters of the scanning electron microscope testing are as follows: the voltage is 2-20 kV, the current is 0.2-6.4 nA, and the working distance is as follows: 4-6 mm, and the specific selection of voltage and current can obtain clear electronic channel contrast images or secondary electronic images with strong signal quantity and no charge phenomenon; when the energy spectrum surface distribution result is obtained, the testing parameters of the scanning electron microscope are as follows: the voltage is 10-20 kV, the current is 0.2-13 nA, the working distance needs to be the optimal working distance set during the energy spectrum correction, the voltage and the current are specifically selected according to the characteristic X-ray capable of exciting the contained elements, the peak count intensity is greater than 10000, and the preferred dead time is less than 10%; testing parameters of the spectrometer: the resolution of the scanning electron microscope image was set to 512 or 1024, and the dwell time was set to: 5-20 mus, starting the image drift correction function, setting the surface distribution resolution as 512, setting the pixel retention time as 20-100 mus, and stopping the acquisition time manually.
Preferably, the grain size, porosity, second phase distribution and second phase composition of the silicon carbide ceramic are qualitatively determined.
Further, preferably, when the contrast image of the electron channel has a difference in gray scale contrast, the crystal grain is determined to be a crystal grain of the silicon carbide ceramic; preferably, the size of the grains is measured.
Preferably, when a black area appears in the electronic channel contrast image, comparing the corresponding area in the secondary electronic image, and if the corresponding area in the secondary electronic image is a black area and the edge is bright, determining that the hole is formed.
Preferably, when a black area appears in the electron channel contrast image, the corresponding area in the secondary electron image is compared, if the corresponding area in the secondary electron image is the black area and the edge of the corresponding area presents gray scale, the secondary electron image is determined as a second phase, and the component of the second phase is determined by combining the energy spectrometer surface distribution result.
Also, preferably, when a white region appears in the electron channel contrast image, the composition of the second phase is determined in combination with the energy spectrum plane distribution result.
Has the advantages that:
The invention obtains the silicon carbide ceramic section which is suitable for the test of a scanning electron microscope and has no shearing stress, no abrasive pollution and no crystal grain extraction by using an ion beam section polishing method, thereby carrying out scanning electron microscope analysis on the shapes, the sizes, the distribution and the quantity of the crystal grains, the holes and the second phase, and carrying out qualitative analysis on the silicon carbide ceramic crystal grains, the second phase and the holes. Compared with a natural section method, the silicon carbide ceramic section can be prepared more smoothly by an ion beam polishing method, and the test of a scanning electron microscope on silicon carbide ceramic grains is more visual and controllable compared with a randomly fractured section; compared with a mechanical polishing corrosion method, the ion beam polishing method is simpler and easier, has high polishing parameter tolerance, does not need to search for complicated corrosion conditions, does not have under-corrosion or over-corrosion phenomena, and can quickly and qualitatively obtain the information of silicon carbide ceramic grains and the like. And when the ion beam polishing method is used, the operation is simple and convenient, and no personnel is needed to take care of after the instrument parameters are set in the polishing process.
The invention uses the electron channel contrast image of the silicon carbide ceramic section obtained by a scanning electron microscope, the electron channel contrast image is a method for reflecting the crystal orientation contrast, the atomic number contrast and the partial morphology contrast of the material surface by using the electron channel effect, and in the scanning electron microscope, the scattering probability of incident electrons by the crystal is closely related to the incidence angle of the incident electrons relative to a certain crystal plane (hkl). For the same crystal plane, the probability of scattering electrons is greater in some incident directions (relative to forbidden channels) and smaller in other incident directions (corresponding to channels), which is called electron channel effect. The crystal grains with different orientations present the difference of gray contrast in the electronic channel contrast image, so the crystal grains with different orientations can be rapidly judged through the difference of gray contrast, and the crystal grain information can be qualitatively obtained. The grain size of the silicon carbide ceramic can be directly measured using a length measuring tool carried by a scanning electron microscope and periodically verified. The electron channel contrast image can also reflect atomic number contrast (component contrast), that is, the larger the average atomic number is, the brighter contrast is presented in the electron channel contrast image, the smaller the average atomic number is, the darker contrast is presented in the electron channel contrast image, and when strong bright-dark contrast is presented, the secondary electron image and the energy spectrometer surface distribution result are combined to judge whether the image is a hole or a second phase.
Drawings
Fig. 1 shows an electron channel contrast image with a cross-sectional magnification of 3000 times of the solid phase sintered silicon carbide ceramic prepared in example 1, wherein different gray levels in the image can be qualitatively judged as different crystal grains, such as A, B, C in the image, for the presence of four black regions, such as D, E, F and G (indicated by arrows in the image), the judgment is further made by combining the secondary electron image and the energy spectrum surface distribution result;
FIG. 2 is a secondary electron image of the same region of solid phase sintered silicon carbide ceramic produced in example 1, wherein the edge of the H region (corresponding to the E region) is bright and the region is judged to be a hole; the edge of the I area (corresponding to the F area) presents gray scale, and the area can be judged as a second phase; the edge part of the G area (corresponding to the D area) presents gray scale, the part is bright, and the area can be judged to contain a second phase and holes, namely the holes are present near the second phase; the edge of the K region (corresponding to the G region) presents gray scale, and the region can be judged as a second phase.
FIG. 3 shows a magnification of a cross section of the solid-phase sintered silicon carbide ceramic prepared in example 1The number of the energy spectrum surface distribution results (Si, C and B elements) in the same area is 3000 times, the I area of the second phase can be judged through the electronic channel contrast image and the secondary electronic image, the Si element is deficient, the C element is enriched, and the second phase can be preliminarily judged to be C; the second phase B can be preliminarily judged by judging that the second phase is a B region in the K region, the Si element is deficient and the C, B element is enriched through the electronic channel contrast image and the secondary electron image4C。
fig. 4 shows an electron channel contrast image with 10000 times magnification of a local section of the liquid phase sintered silicon carbide ceramic prepared in example 2, wherein different gray levels in the image can be qualitatively judged as different crystal grains, such as L, M and N in the image can be qualitatively judged as three crystal grains, and for the occurrence of strong white areas and black areas, such as O and P (indicated by arrows in the image), the judgment is further made by combining the secondary electron image and the energy spectrum surface distribution result;
FIG. 5 is a diagram showing a secondary electron image of the same region of a liquid phase sintered silicon carbide ceramic prepared in example 2, wherein the edge of the R black region (corresponding to the P region) is bright and the region can be judged to be a hole, at a local magnification of 10000 times in the cross section; the Q area in the secondary electron image is still a white area;
FIG. 6 shows the distribution results (Al, Y, O and Si elements) of the surface of the spectrometer in the same region with the cross-sectional magnification of 100000 times of the liquid phase sintered silicon carbide ceramic prepared in example 2, wherein Al, Y and O are enriched, Si is deficient, and the region can be judged as second phase YAG;
FIG. 7 shows a backscattering image of a solid phase sintered silicon carbide ceramic prepared in comparative example 1 with a natural fracture magnification of 3000 times;
FIG. 8 shows a back-scattered image of a solid phase sintered silicon carbide ceramic prepared in comparative example 2 with a 3000-fold magnification of the cut surface;
FIG. 9 shows a backscattering image of a solid phase sintered silicon carbide ceramic prepared in comparative example 3 with a mechanical polished surface magnification of 3000 times;
Fig. 10 shows a back-scattering image of natural fracture magnification of 10000 times for the liquid phase sintered silicon carbide ceramic prepared in comparative example 4;
Fig. 11 shows a back-scattered image of a cut surface of the liquid phase sintered silicon carbide ceramic prepared in comparative example 5 at a magnification of 10000 times;
Fig. 12 shows a back-scattered image of a mechanically polished surface of the liquid phase sintered silicon carbide ceramic prepared in comparative example 6 at a magnification of 10000 times.
Detailed Description
The present invention is further illustrated by the following examples, which are to be understood as merely illustrative and not restrictive.
In the disclosure, a silicon carbide ceramic cross section suitable for a scanning electron microscope test is obtained by an ion beam polishing method, and the distribution and the components of crystal grains, holes and a second phase of the silicon carbide ceramic are rapidly observed and measured by the scanning electron microscope and an energy spectrometer. In particular to the preparation of a silicon carbide ceramic cross section sample by using proper steps, how to adjust and obtain the contrast image of an electronic channel and the clearest image of a secondary electron image of the silicon carbide ceramic cross section sample, and the content of obtaining the surface distribution result of an energy spectrometer and the like. The following is an exemplary description of the method for preparing silicon carbide ceramic observed by a scanning electron microscope using the ion beam polishing technique provided by the present invention.
Cutting the silicon carbide ceramic into proper size by an inner circle cutting machine, and fixing the cut silicon carbide ceramic on a sample table of an ion beam polishing machine. In the disclosure, silicon carbide ceramic is selected as sintered and crystallized dense ceramic, when the contrast image of an electronic channel of the cross section of the silicon carbide ceramic has gray contrast difference, the crystal grain of the silicon carbide ceramic can be judged, and when a strong black area appears, the secondary electron image of the area is compared to judge whether the area is a hole. And if the edge of the black area in the secondary electronic image is bright, determining that the hole is formed. If the edge of the black area in the secondary electronic image presents gray, whether the secondary electronic image is a second phase or not needs to be judged by combining the surface distribution result of the energy spectrometer. When an intense white area appears, whether the area is a second phase or not needs to be judged by combining the energy spectrum surface distribution result.
And (3) carrying out ion beam polishing on the cut sample to obtain the silicon carbide ceramic section to be tested, which is polished by the ion beam and has a smooth silicon carbide ceramic section without shear stress and crystal grain extraction. In alternative embodiments, the parameters of the ion beam polishing process may be: the acceleration voltage of the ion beam is 5-8 kV; the sample polishing time can be 120-300 minutes; the current is 1.5-3 mA. Specifically, when the silicon carbide ceramic is placed into an ion beam polishing machine, firstly, the cut silicon carbide ceramic is adhered to a special sample table for section polishing by means of a sample mounting centering table; and then the sample stage adhered with the silicon carbide ceramic is placed into an argon ion beam polishing instrument, and the silicon carbide ceramic is tightly attached to the baffle plate, so that the ion beam polishes the silicon carbide ceramic.
The method is used for analyzing and measuring the shapes, sizes and distributions of the crystal grains, the holes and the second phase of the silicon carbide ceramic section by using a scanning electron microscope and an energy spectrometer. Specifically, a scanning electron microscope test is carried out on the silicon carbide ceramic section (silicon carbide ceramic section sample) to be tested which is polished by the ion beam, and the shapes, sizes and distributions of the crystal grains, the holes and the second phase are judged according to the silicon carbide ceramic electronic channel contrast image, the secondary electron image and the energy spectrometer surface distribution result obtained by the test. In an alternative embodiment, when obtaining the contrast image and the secondary electron image of the electron channel, the test parameters of the sem test may be: selecting a back scattering detector and a secondary electron detector, wherein the selection voltage is 2-20 kV, the current is 0.2-6.4 nA, and the working distance is as follows: 4-6 mm; when obtaining the energy spectrometer surface distribution result, the test parameters of the scanning electron microscope test can be as follows: the voltage is 10-20 kV, the current is 0.2-13 nA, the working distance needs to be the optimal working distance set during the energy spectrum correction, the voltage and the current are specifically selected according to the characteristic X-ray capable of exciting the contained elements, the peak count intensity is greater than 10000, and the preferred dead time is less than 10%; testing parameters of the spectrometer: the resolution of the scanning electron microscope image was set to 512 or 1024, and the dwell time was set to: 5-20 mus, starting the image drift correction function, setting the area distribution resolution as 512, setting the pixel retention time as 20-100 mus (preferably 30-70 mus, more preferably 40-60 mus), and manually stopping the acquisition time.
Reagents required for the experiment:
Silicon carbide ceramic adhesive material: the conductive adhesive tape comprises a carbon-based conductive adhesive tape, an aluminum-based conductive adhesive tape, a copper-based conductive adhesive tape, an isopropanol-based Pelco Colloidal Graphite liquid carbon conductive adhesive and DAG-T-502 liquid carbon conductive adhesive.
The silicon carbide ceramic is cut into proper sizes (the sizes of length, width and thickness are less than 25 multiplied by 20 multiplied by 5mm) by using an inner circle cutting machine, selecting a diamond blade and setting the cutting speed. Since silicon carbide ceramics are second only to diamond, the slower cutting speed can be set as: 1-2 mm/min, rotation speed: 3000 r/min. And then ultrasonically cleaning the cut silicon carbide ceramic.
putting the sample into an argon ion beam polishing instrument, installing a centering table by using a cross-section sample, adhering the silicon carbide ceramic on a special sample table for cross-section polishing by using a liquid or conductive adhesive tape, and if a liquid carbon conductive adhesive material is adopted, ensuring that the liquid carbon conductive adhesive material is cured and then carrying out the next operation;
Placing the sample stage adhered with the silicon carbide ceramic into an argon ion beam polishing instrument, wherein the silicon carbide ceramic is tightly attached to the baffle, and the baffle and the silicon carbide ceramic are ensured to have no gap under an optical microscope of 9.6 times;
Adjusting the position of the sample stage to enable the polished area to be in the central position of the optical microscope visual field;
under an optical microscope with the power of 76.8 times, the position of the sample stage is adjusted to ensure that the silicon carbide ceramic protrudes out of the upper edge of the baffle plate by about 17-50 mu m.
Finishing argon ion beam polishing treatment and vacuumizing, and setting polishing parameters:
The acceleration voltage of the ion beam is 5-8 kV, such as 7 kV;
The sample polishing time is 120-300 minutes, such as 240 minutes;
And when the current of the three ion guns is stabilized to be 1.5-3 mA, such as 2mA, the argon ion beam polishing instrument starts to work normally.
Obtaining an electron channel contrast image and a secondary electron image and analyzing data:
a) Acquiring a contrast image and a secondary electron image of an electron channel, wherein the parameters of the scanning electron microscope are set as follows:
The voltage is 2-20 kV, such as 5 kV;
The current is 0.2 to 6.4nA, such as 3.2 nA;
b) The main steps of acquiring the electronic channel contrast image and the secondary electronic image are as follows:
Opening the voltage and current of a scanning electron microscope, adjusting to a reasonable working distance of 4-6 mm, inserting a back scattering detector, obtaining a clear image through focusing and stigmation operations, finding out the silicon carbide ceramic polished by the ion beam, and obtaining a clear electron channel contrast image of the section; and simultaneously acquiring a secondary electron image of the region by using a secondary electron detector.
c) The main steps of the analysis of the electron channel contrast image and the secondary electron image are as follows:
Observing the contrast difference of the gray scale in the electronic channel contrast images, the crystal grains of the silicon carbide ceramic can be judged (for example, see the attached figure 1); when a strong black area appears, firstly, judging whether the area is a hole by comparing the secondary electron image of the area, if the edge of the black area in the secondary electron image is bright, judging the area is a hole (for example, see fig. 2 and 5), and if the edge of the black area in the secondary electron image presents gray scale, judging whether the area is a second phase by combining an energy spectrometer surface distribution result (for example, see fig. 3); when the strong white area appears, the result of the energy spectrum surface distribution (for example, see fig. 6) is combined to judge whether the phase is the second phase.
d) Acquiring the surface distribution result of the energy spectrometer, and setting the parameters of the scanning electron microscope as follows:
The voltage is 10-20 kV;
The current is 0.2 to 13nA, such as 0.8 nA;
e) The main steps for obtaining the surface distribution result of the energy spectrometer are as follows:
opening the voltage and current of the scanning electron microscope, adjusting the working distance to the optimal working distance set during the energy spectrum correction, inserting the energy spectrum, obtaining a clear image through focusing and stigmation operations, finding the area for obtaining the contrast image and the secondary electron image of the electron channel, setting the resolution ratio 512 or 1024 for collecting the image of the scanning electron microscope, and setting the retention time as follows: and 5-20 mus, starting an image drift correction function, setting the surface distribution resolution ratio 512, setting the pixel retention time to be 20-100 mus, collecting the micro-area surface distribution of the area, and stopping manually after the distribution image of each element surface is clear. And judging whether the region is a second phase or not by combining the energy spectrometer surface distribution result.
in the method, a scanning electron microscope and an energy spectrometer are used for obtaining a testing method combining an electron channel contrast image and a secondary electron image, the shapes, the sizes and the distributions of crystal grains, holes and a second phase of a silicon carbide ceramic section sample are observed and analyzed, the crystal grains and the holes are effectively measured, data can be provided for the relation between the microstructure of the silicon carbide ceramic and the preparation process and the performance, and the method has important significance for the development, production and quality control of the materials. Compared with the prior art, the method has the advantages that the silicon carbide ceramic ion beam polishing method suitable for the scanning electron microscope is determined, the shapes, sizes and distributions of the crystal grains, the holes and the second phase can be judged, and the method is more accurate and convenient compared with the prior method.
the present invention will be described in detail by way of examples. It is also to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that certain insubstantial modifications and adaptations of the invention by those skilled in the art may be made in light of the above teachings. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below. The experimental articles and instruments referred to in the following examples and comparative examples include: silicon carbide ceramic adhesive material: the conductive adhesive tape comprises a carbon-based conductive adhesive tape, an aluminum-based conductive adhesive tape, a copper-based conductive adhesive tape, an isopropanol-based Pelco Colloidal Graphite liquid carbon conductive adhesive and a DAG-T-502 liquid carbon conductive adhesive; silicon carbide ceramics: see examples 1 and 2; scanning electron microscope (company: Thermo Fisher Scientific, model: Verios G4 UC); energy spectrometer (company: EDAX, model: 70 mm)2SiN window).
example 1
Preparing solid-phase sintered silicon carbide ceramic: silicon carbide powder is taken as raw material, and 0.6 wt% of B is added4c and 1.5 wt% of C as sintering aids. The method comprises the steps of sequentially carrying out wet ball milling, drying and sieving to obtain a powder raw material, preparing a ceramic biscuit by dry pressing and cold isostatic pressing forming processes, and then carrying out heat preservation at 2200 ℃ for 1h and high-temperature sintering in a carbon tube furnace under the atmosphere of argon to obtain the normal-pressure solid-phase sintered silicon carbide ceramic material.
example 2
Preparing liquid phase sintered silicon carbide ceramic: silicon carbide powder is taken as raw material, and 3.12 wt% of Al is added2O3and 3.88 wt% Y2O3the sintering aid is put into a ball milling tank, ball milling, drying and sieving are sequentially carried out to obtain a powder raw material, a ceramic biscuit is prepared by dry pressing and cold isostatic pressing forming processes, then debonding is carried out in a debonding furnace, and the ceramic biscuit is put into a graphite crucible and sintered in a vacuum carbon tube furnace after debonding. And (3) carrying out high-temperature sintering at 1700 ℃ for 1h under the argon atmosphere in a carbon tube furnace to prepare the liquid-phase sintered silicon carbide ceramic.
Example 3
firstly, cutting the solid-phase sintered silicon carbide ceramic into proper sizes (the sizes of length, width and thickness are less than 25 multiplied by 20 multiplied by 5mm) by using an inner circle cutting machine, loading the cut samples into an argon ion beam polisher by using a cross-section sample mounting centering table, and polishing the cut surfaces of the samples by using ion beams. Wherein the parameters of the ion beam polishing comprise: acceleration voltage: 7kV, current: 2mA, polishing time: and 4h, adhering the polished section sample on a sample stage of a scanning electron microscope. Secondly, observing the solid-phase sintered silicon carbide ceramic cross section sample after ion beam polishing by using a scanning electron microscope, and selecting a magnification factor of 3000 times and a voltage: 5kV, current: 3.2nA, the working distance is 4.5mm, clear electronic channel contrast images are obtained, different gray levels of the cross section of the solid phase sintered silicon carbide ceramic are observed as shown in figure 1, the silicon carbide ceramic can be judged to be different crystal grains, and A, B and C in figure 1 can be qualitatively judged to be three crystal grains. The arrows in FIG. 1 indicate D, E, F and G four black areas, which are first based on the secondary electron image of the same area, see FIG. 2, the H area (and E area)Corresponding to the domain) has bright edges, and the domain can be judged to be a hole; the edge of an I area (corresponding to an F area) in the secondary electronic image presents gray scale, and the area can be judged as a second phase; the edge part of the J area (corresponding to the D area) presents gray scale, the part is bright, and the area can be judged to contain a second phase and holes, namely the holes are present near the second phase; the edge of the K region (corresponding to the G region) presents gray scale, and the region can be judged as a second phase. Then, for the judged region of the second phase, utilizing an energy spectrum semi-quantitative result (when an energy spectrum surface distribution result is obtained, the test parameters of a scanning electron microscope test are that the voltage is 10kV, the current is 6.4nA, the working distance needs to select the optimal working distance set during energy spectrum correction, the test parameters of the energy spectrum test are that the resolution of an image of the scanning electron microscope is set to be 512 or 1024, the retention time is set to be 5-20 mus, the image drift correction function is started, the surface distribution resolution is set to be 512, the pixel retention time is 50 mus, and the acquisition time is manually stopped) to deeply analyze the second phase component, as shown in figure 3, the energy spectrum surface distribution result (Si, C and B elements) of the same region is judged to be an F region of the second phase after analyzing an electron channel contrast image and a secondary electron image, the Si element is deficient, the C element is enriched, the second phase can be preliminarily judged to be C; the second phase is judged to be B in the G region, Si is deficient and C, B is enriched4C. The solid phase sintered silicon carbide ceramic grains, pores, second phase distribution and components are judged according to the method.
example 4
firstly, an inner circle cutting machine cuts liquid phase sintering silicon carbide ceramics into proper size (the size of length, width and thickness is less than 25 multiplied by 20 multiplied by 5mm), and a cross section sample mounting centering table is used for loading the cut sample into an argon ion beam polishing instrument, and the ion beam is used for polishing the cut surface of the sample. Wherein the parameters of the ion beam polishing comprise: acceleration voltage: 7kV, current: 2mA, polishing time: and 4h, adhering the polished section sample on a sample stage of a scanning electron microscope. Secondly, observing the liquid phase sintered silicon carbide ceramic cross section sample after ion beam polishing by using a scanning electron microscope, and selecting 10000 times of magnification, voltage: 5kV, current: 3.2nA, working distance: 4.5mm, obtaining clear contrast image of the electronic channel, and observing different gray scales of the cross section of the liquid phase sintered silicon carbide ceramic shown in figure 4, judging the cross section to be different crystal grains of the silicon carbide ceramic, wherein L, M and N in figure 4 can be qualitatively judged to be three crystal grains. In fig. 4, the P black area indicated by the arrow is a hole according to the secondary electron image of the same area, see fig. 5, and the edge of the R black area (corresponding to the P area) in the secondary electron image is bright; in the arrow in fig. 4, the strong white O area is determined to be second-phase YAG by enriching three elements of Al, Y, and O and lacking Si element according to the secondary electron image (see Q area in fig. 5) and the energy spectrum surface distribution result (Al, Y, O, and Si elements, see fig. 6) in the same area; the distribution and the components of crystal grains, pores and a second phase of the liquid phase sintered silicon carbide ceramic are judged according to the method. When the energy spectrum surface distribution result is obtained, the testing parameters of the scanning electron microscope test are as follows: the voltage is 10kV, the current is 6.4nA, and the working distance needs to select the optimal working distance set during the energy spectrum correction; the test parameters of the energy spectrometer test are as follows: the resolution of the scanning electron microscope image was set to 512 or 1024, and the dwell time was set to: and 5-20 mus, starting an image drift correction function, setting the surface distribution resolution as 512, setting the pixel retention time as 50 mus, and manually stopping the acquisition time.
Comparative example 1
Firstly, a solid-phase sintered silicon carbide ceramic natural fracture is obtained by an external force applying method such as knocking by a tool (a hammer and the like), and the fracture is upwards adhered to a scanning electron microscope sample stage. Secondly, observing a solid-phase sintered silicon carbide ceramic natural fracture sample by using a scanning electron microscope, wherein the voltage is as follows: 5kV, current: 3.2nA, working distance: 4.4mm, obtaining a backscattering image with the magnification of 3000 times, as shown in the attached figure 7, wherein black in the image is a second phase, and gray is silicon carbide crystal grains, compared with the embodiment 3, under the same scanning electron microscope test conditions, in a natural fracture of the solid-phase sintered silicon carbide ceramic, the grain boundary of the silicon carbide crystal grains is difficult to determine, and the size cannot be preliminarily measured. It is difficult to judge the solid phase sintered silicon carbide ceramic crystal grains according to the above method.
comparative example 2
firstly, an inner circle cutting machine is adopted to cut to obtain a solid-phase sintered silicon carbide ceramic cutting surface, and the cutting surface is upwards adhered to a sample table of a scanning electron microscope. Secondly, observing the cut solid-phase sintered silicon carbide ceramic cutting surface by using a scanning electron microscope, wherein the voltage is as follows: 5kV, current: 3.2nA, working distance: 4.5mm, a clear backscatter image at 3000 times magnification was obtained, see fig. 8, where the black area in the image is the second phase, and in addition to this, there were numerous mechanical cuts causing pits and scratches in the grey scale area, and compared to example 3, it was completely impossible to identify silicon carbide grains.
comparative example 3
firstly, a mechanical polishing method (firstly, an inner circle cutting machine is adopted for cutting, and then, a polishing machine is adopted for mechanically polishing the cutting surface) is adopted for obtaining a mechanical polishing surface of the solid-phase sintered silicon carbide ceramic, and the mechanical polishing surface is upwards adhered on a sample stage of a scanning electron microscope. Secondly, observing the mechanically polished surface of the solid-phase sintered silicon carbide ceramic after mechanical polishing by using a scanning electron microscope, wherein the voltage is as follows: 5kV, current: 3.2nA, working distance: 4.7mm, a clear backscatter image with a magnification of 3000 times is obtained, as shown in fig. 9, wherein the black area in the image is a hole or a second phase, and the other gray scales are silicon carbide grains, and the shape and the size of the silicon carbide grains are difficult to identify according to the image.
Comparative example 4
firstly, a liquid phase sintered silicon carbide ceramic natural fracture is obtained by an external force applying method such as knocking by a tool (a hammer and the like), and the fracture is upwards adhered to a scanning electron microscope sample stage. Secondly, observing a liquid phase sintered silicon carbide ceramic natural fracture sample by using a scanning electron microscope, wherein the voltage is as follows: 5kV, current: 3.2nA, working distance: 4.5mm, obtaining a backscattering image with a magnification of 10000 times, as shown in figure 10, wherein white in the image is a second phase, gray is silicon carbide crystal grains, and a black area is a hole, compared with example 4, under the same test conditions of a scanning electron microscope, in a natural fracture of the phase-sintered silicon carbide ceramic, a crystal boundary of the silicon carbide crystal grains can be observed, but holes with larger sizes (as shown by arrows in the figure) exist in the figure, and the figure cannot judge whether the holes are caused by the extraction of crystal grains during the fracture or the defects of the silicon carbide ceramic such as the holes and the like.
Comparative example 5
Firstly, an inner circle cutting machine is adopted to cut to obtain a liquid phase sintered silicon carbide ceramic cutting surface, and the cutting surface is upwards adhered to a sample stage of a scanning electron microscope. Secondly, observing the cut liquid phase sintered silicon carbide ceramic cutting surface by using a scanning electron microscope, wherein the voltage is as follows: 5kV, current: 3.2nA, working distance: 4.5mm, a clear back-scattered image was obtained at a magnification of 10000 times, as shown in fig. 11, in which the white region was the second phase and the gray region was partially recognized in the shape of the crystal grains (as indicated by arrows in the figure), but in addition, a large number of pits and scratches were present due to mechanical cutting, and the grain boundary of the silicon carbide crystal grains was hardly determined as compared with example 4.
Comparative example 6
Firstly, obtaining a mechanical polishing surface of liquid-phase sintered silicon carbide ceramic by adopting a mechanical polishing method, and adhering the mechanical polishing surface to a scanning electron microscope sample stage upwards. Secondly, observing the mechanically polished surface of the mechanically polished liquid phase sintered silicon carbide ceramic by using a scanning electron microscope, wherein the voltage is as follows: 5kV, current: 3.2nA, working distance: 4.6mm, a clear back scattering image with the magnification of 10000 times is obtained, and the image is shown in figure 12, wherein the black area in the image is a hole, the white area is a second phase, and other gray scales are silicon carbide crystal grains, the shape and the size of the silicon carbide crystal grains in the local area can be identified according to the image, compared with the embodiment 4, the silicon carbide crystal grains can be only partially judged, and a large number of scratches exist, which affect the image quality.
in the present invention, the ion beam polishing apparatus used was Leica EM TIC3X, scanning electron microscope (company: Thermo Fisher Scientific, model: Verios G4 UC); energy spectrometer (company: EDAX, model: 70 mm)2SiN window).
Claims (10)
1. A method for preparing a silicon carbide ceramic cross-section sample observed by a scanning electron microscope by using an ion beam cross-section polishing technology is characterized in that the silicon carbide ceramic cross-section sample is obtained by performing ion beam cross-section polishing on the silicon carbide ceramic; the parameters of the ion beam cross section polishing comprise: the acceleration voltage of the ion beam is 5-8 kV; the sample polishing time is 120-300 minutes; the current is 1.5-3 mA.
2. the method of claim 1, wherein the silicon carbide ceramic is cut to size using an automatic internal circular cutting machine with diamond blades selected and cutting speed set prior to ion beam cross-sectional polishing.
3. The method according to claim 1 or 2, wherein the sample stage loaded with the silicon carbide ceramic is loaded into an argon ion beam polisher and the silicon carbide ceramic is brought into close contact with a baffle plate so that the ion beam polishes the silicon carbide ceramic.
4. a method for rapid analysis and measurement of grain size, porosity, second phase distribution, and second phase composition in a silicon carbide ceramic cross-sectional sample according to any one of claims 1 to 3, comprising:
Carrying out scanning electron microscope test on the silicon carbide ceramic cross section sample to obtain an electron channel contrast image and a secondary electron image of the silicon carbide ceramic cross section sample;
Carrying out energy spectrum instrument test on the silicon carbide ceramic cross section sample to obtain the energy spectrum surface distribution result of the silicon carbide ceramic cross section sample;
and judging the grain size, the pores, the second phase distribution and the second phase component of the silicon carbide ceramic according to the obtained electronic channel contrast image, the secondary electron image and the energy spectrum surface distribution result.
5. The method of claim 4, wherein the scanning electron microscope test parameters for obtaining the electron channel contrast image or the secondary electron image are: the voltage is 2-20 kV, the current is 0.2-6.4 nA, and the working distance is as follows: 4-6 mm; when the energy spectrum surface distribution result is obtained, the testing parameters of the scanning electron microscope test are as follows: the voltage is 10-20 kV, the current is 0.2-13 nA, and the working distance needs to be the optimal working distance set during energy spectrum correction; the test parameters of the energy spectrometer test are as follows: the resolution of the scanning electron microscope image was set to 512 or 1024, and the dwell time was set to: and 5-20 mus, starting the image drift correction function, setting the surface distribution resolution as 512, setting the pixel retention time as 20-100 mus, and manually stopping the acquisition time.
6. The method according to claim 4 or 5, wherein the crystal grain, pore, second phase distribution, and second phase composition of the silicon carbide ceramic are qualitatively judged.
7. The method according to claim 6, wherein when a difference in gray scale contrast occurs in the electron channel contrast image, it is judged as a crystal grain of the silicon carbide ceramic; preferably, the size of the grains is measured.
8. The method of claim 6, wherein when a black area appears in the electron channel contrast image, comparing the corresponding area in the secondary electron image, and if the corresponding area in the secondary electron image is a black area and the edge is bright, determining that the hole is formed.
9. the method of claim 6, wherein when a black area appears in the electron channel contrast image, comparing the corresponding areas in the secondary electron image, if the corresponding areas in the secondary electron image are black areas and the edges present gray levels, determining the corresponding areas as the second phase, and determining the components of the second phase by combining the energy spectrometer surface distribution result.
10. The method of claim 6, wherein the composition of the second phase is determined in combination with the energy dispersive surface distribution when white regions appear in the electron channel contrast image.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111795984A (en) * | 2020-06-22 | 2020-10-20 | 中国科学院上海硅酸盐研究所 | Sample preparation method for observing microstructure in ceramic by scanning electron microscope |
| CN112378941A (en) * | 2020-10-20 | 2021-02-19 | 西安富阎时代新能源有限公司 | Characterization method for cross-sectional morphology and components of lithium battery anode and cathode materials |
| CN112858362A (en) * | 2021-01-08 | 2021-05-28 | 重庆大学 | Preparation method of micron-sized spherical particle section for electron microscope observation |
| CN112946319A (en) * | 2021-02-05 | 2021-06-11 | 上海市计量测试技术研究院 | Preparation method of plane ion channel contrast sample |
| CN113390914A (en) * | 2020-03-13 | 2021-09-14 | 中国科学院上海硅酸盐研究所 | Method for representing three-dimensional microstructure of ceramic coating material based on focused ion beam |
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Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101458180A (en) * | 2007-12-13 | 2009-06-17 | 中芯国际集成电路制造(上海)有限公司 | Method for preprocessing TEM example and carrying out TEM test for example |
| CN105675364A (en) * | 2016-01-15 | 2016-06-15 | 中国地质科学院矿产资源研究所 | Preparation method of zircon mineral particle transmission sample |
| CN105973674A (en) * | 2016-07-01 | 2016-09-28 | 中国科学院地质与地球物理研究所 | Preparation method of transmission electron microscope sample with large area of thin region |
| CN106525532A (en) * | 2016-11-07 | 2017-03-22 | 上海达是能源技术有限公司 | Transmission electron microscope sample preparation method |
| CN206066090U (en) * | 2016-08-31 | 2017-04-05 | 北京埃德万斯离子束技术研究所股份有限公司 | A kind of Subnano-class ion beam polishing equipment |
| CN106596616A (en) * | 2016-12-26 | 2017-04-26 | 株洲硬质合金集团有限公司 | Analysis and detection method of two cobalt phases in WC-Co hard alloy |
| CN106840744A (en) * | 2017-03-02 | 2017-06-13 | 河钢股份有限公司 | A kind of preparation method of mild steel EBSD sample for analysis |
| CN107470991A (en) * | 2017-09-13 | 2017-12-15 | 成都睿坤科技有限公司 | A kind of high stability ion beam polishing device |
| CN109030530A (en) * | 2018-05-03 | 2018-12-18 | 中国科学院上海硅酸盐研究所 | A kind of preparation method and measuring method of the pearlescent pigment cross-sectional sample for scanning electron microscope measurement |
| CN109270105A (en) * | 2018-08-21 | 2019-01-25 | 中国科学院地质与地球物理研究所 | The method for quickly identifying and positioning target mineral particle in the big ken |
-
2019
- 2019-09-09 CN CN201910849849.9A patent/CN110567998A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101458180A (en) * | 2007-12-13 | 2009-06-17 | 中芯国际集成电路制造(上海)有限公司 | Method for preprocessing TEM example and carrying out TEM test for example |
| CN105675364A (en) * | 2016-01-15 | 2016-06-15 | 中国地质科学院矿产资源研究所 | Preparation method of zircon mineral particle transmission sample |
| CN105973674A (en) * | 2016-07-01 | 2016-09-28 | 中国科学院地质与地球物理研究所 | Preparation method of transmission electron microscope sample with large area of thin region |
| CN206066090U (en) * | 2016-08-31 | 2017-04-05 | 北京埃德万斯离子束技术研究所股份有限公司 | A kind of Subnano-class ion beam polishing equipment |
| CN106525532A (en) * | 2016-11-07 | 2017-03-22 | 上海达是能源技术有限公司 | Transmission electron microscope sample preparation method |
| CN106596616A (en) * | 2016-12-26 | 2017-04-26 | 株洲硬质合金集团有限公司 | Analysis and detection method of two cobalt phases in WC-Co hard alloy |
| CN106840744A (en) * | 2017-03-02 | 2017-06-13 | 河钢股份有限公司 | A kind of preparation method of mild steel EBSD sample for analysis |
| CN107470991A (en) * | 2017-09-13 | 2017-12-15 | 成都睿坤科技有限公司 | A kind of high stability ion beam polishing device |
| CN109030530A (en) * | 2018-05-03 | 2018-12-18 | 中国科学院上海硅酸盐研究所 | A kind of preparation method and measuring method of the pearlescent pigment cross-sectional sample for scanning electron microscope measurement |
| CN109270105A (en) * | 2018-08-21 | 2019-01-25 | 中国科学院地质与地球物理研究所 | The method for quickly identifying and positioning target mineral particle in the big ken |
Non-Patent Citations (8)
| Title |
|---|
| 岳鹏: "《金属材料与热处理概论》", 30 June 2018 * |
| 张峰: "空间相机碳化硅反射镜表面硅改性层的组合式抛光", 《中国激光》 * |
| 曲远方: "《现代陶瓷材料及技术》", 31 May 2008 * |
| 李熹: "煤的氩离子抛光－ 扫描电镜分析样品制备研究", 《广州化工》 * |
| 武磊 等: "ZnS离子束抛光过程中的粗糙度演变", 《西安工业大学学报》 * |
| 王亮 等: "页岩的氩离子抛光制样研究", 《石油实验地质》 * |
| 陈威， 等: "稀土稳定四方多晶氧化锆陶瓷相变微结构的表征", 《硅酸盐学报》 * |
| 陈晨， 等: "不同岩相泥页岩数字岩心构建方法研究—以东营凹陷为例", 《现代地质》 * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN113390914B (en) * | 2020-03-13 | 2022-10-14 | 中国科学院上海硅酸盐研究所 | Method for representing three-dimensional microstructure of ceramic coating material based on focused ion beam |
| CN111795984A (en) * | 2020-06-22 | 2020-10-20 | 中国科学院上海硅酸盐研究所 | Sample preparation method for observing microstructure in ceramic by scanning electron microscope |
| CN111795984B (en) * | 2020-06-22 | 2022-05-10 | 中国科学院上海硅酸盐研究所 | Sample preparation method for observing microstructure inside ceramic by scanning electron microscope |
| CN112378941A (en) * | 2020-10-20 | 2021-02-19 | 西安富阎时代新能源有限公司 | Characterization method for cross-sectional morphology and components of lithium battery anode and cathode materials |
| CN112858362A (en) * | 2021-01-08 | 2021-05-28 | 重庆大学 | Preparation method of micron-sized spherical particle section for electron microscope observation |
| CN112946319A (en) * | 2021-02-05 | 2021-06-11 | 上海市计量测试技术研究院 | Preparation method of plane ion channel contrast sample |
| CN112946319B (en) * | 2021-02-05 | 2023-09-08 | 上海市计量测试技术研究院 | Preparation method of planar ion channel contrast sample |
| CN116242683A (en) * | 2023-03-31 | 2023-06-09 | 胜科纳米(苏州)股份有限公司 | Preparation method of plane transmission electron microscope sample and plane transmission electron microscope sample |
| CN116242683B (en) * | 2023-03-31 | 2024-06-11 | 胜科纳米(苏州)股份有限公司 | Preparation method of plane transmission electron microscope sample and plane transmission electron microscope sample |
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