CN113899763A - Method for detecting and analyzing small-size nonmetallic inclusions in steel by using scanning electron microscope - Google Patents
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- 238000005498 polishing Methods 0.000 claims abstract description 35
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 21
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
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Abstract
The invention discloses a method for detecting and analyzing small-size nonmetallic inclusions in steel by using a scanning electron microscope, which mainly solves the technical problems of low quantitative analysis precision and poor stability of the small-size nonmetallic inclusions in the steel in the prior art. The technical scheme is that the method for detecting and analyzing small-size nonmetallic inclusions in steel by using a scanning electron microscope comprises the following steps: 1) preparing a metallographic sample, and inlaying the surface of the sample to be detected by using a hot inlaying machine; polishing, polishing and cleaning the inlaid sample; attaching aluminum foil paper to an area, which is not to be analyzed, of the edge of the sample to obtain a metallographic sample; 2) regulating and controlling the detection parameters of a scanning electron microscope and an energy spectrum; 3) detecting inclusions; 4) analyzing the inclusions, setting inclusion classification standards, and analyzing the detection result by using a computer inclusion analysis program to obtain the information of the number, size, shape and composition of the inclusions. The method has the advantages of simple and convenient operation, high efficiency and high precision of qualitative and quantitative analysis of small-size nonmetallic inclusions in the steel.
Description
Technical Field
The invention relates to an analysis method of nonmetallic inclusions in steel materials, in particular to a method for detecting and analyzing small-size nonmetallic inclusions in steel by using a scanning electron microscope, and belongs to the technical field of analysis and detection of steel materials.
Background
With the development of the modern refining technology, the cleanliness of steel is greatly improved, and the understanding of non-metallic inclusions in the steel also begins to be changed into the understanding that the non-metallic inclusions in the steel are used as the hazardous substances which can reduce the plasticity, toughness and fatigue property of the steel and lead the cold and hot processing performance of the steel to influence the performance of steel products by controlling the non-metallic inclusions in the steel. Therefore, the research on the information such as the number, the shape, the size, the distribution condition and the like of the non-metallic inclusions in the steel and the development of corresponding detection have very important significance for the analysis, the reasonable use and the like of the product performance of the steel and iron.
At present, in the detection technologies for measuring nonmetallic inclusions in steel materials at home and abroad, the most common methods are the conventional methods such as a metallographic method, an electrolytic method, an in-situ analysis method and the like, but the methods have certain limitations, cannot meet the total analysis of small-size inclusions in steel samples, cannot meet the requirements on detection accuracy and detection efficiency, and seriously influences the development of scientific research such as new product development, process improvement and the like.
The back scattering electrons mainly reflect the composition characteristics of the surface of the sample, namely, the parts with larger atomic number of the sample generate stronger back scattering electron signals, and form brighter regions on the fluorescent screen; while the lower average atomic number region produces less backscattered electrons and creates a darker area on the screen, thus creating an atomic number contrast. The scanning electron microscope backscattered electron morphology image can effectively identify inclusions, and the X-ray energy spectrum analysis can analyze components of corresponding inclusions, but when the scanning electron microscope method is used for analyzing inclusions generally, the analysis is limited to the targeted analysis of one or some specified inclusions, and cannot meet the requirements of the overall analysis of the size, shape, type and the like of the inclusions in steel, particularly the accurate analysis of small-size inclusions.
Chinese patent application publication No. CN108593649A discloses a method for qualitative and quantitative testing and analysis of inclusions in steel, which comprises observing a sample to be tested in a metallographic phase, determining the size range of the inclusions, adjusting the test parameters of a scanning electron microscope according to the size range to perform scanning electron microscope testing and EDS energy spectrum analysis on the sample to be tested, and obtaining the size, shape and composition data of the inclusions in steel. According to the method, different sizes of inclusions are observed according to a metallographic phase, different testing parameters and scanning areas of a scanning electron microscope are correspondingly adjusted, the working distance of the scanning electron microscope is 15-20mm, the operation process needs to be switched continuously, the working voltage and the working distance range change greatly, and the accuracy and the reproducibility of results are greatly influenced.
In the prior art, the analysis and detection precision of small-size nonmetallic inclusions in steel is low, and the detection requirement of clean steel production cannot be met.
Disclosure of Invention
The invention aims to provide a method for detecting and analyzing small-size nonmetallic inclusions in steel by using a scanning electron microscope, and mainly solves the technical problems of low quantitative analysis precision and poor stability of the small-size nonmetallic inclusions in the steel in the prior art.
The invention has the technical scheme that the method for detecting and analyzing small-size nonmetallic inclusions in steel by using a scanning electron microscope comprises the following steps:
1) preparing a metallographic sample, and inlaying the surface of the sample to be detected by using a hot inlaying machine; polishing, polishing and cleaning the inlaid sample; attaching aluminum foil paper to an area, which is not to be analyzed, of the edge of the sample to obtain a metallographic sample;
2) regulating and controlling a scanning electron microscope and energy spectrum detection parameters, and placing the prepared metallographic sample in a scanning electron microscope sample chamber; setting analysis parameters of a scanning electron microscope and an X-ray energy spectrum, ensuring that the dead time of the energy spectrum analysis of the aluminum foil matrix is 38-42 percent, and the impurity analysis count is above 4500 percent;
3) detecting inclusions, namely detecting a metallographic sample to be detected by using a scanning electron microscope, and setting inclusion detection parameters, inclusion size parameters, calibration parameters, threshold parameters and an inclusion detection area to detect the inclusions;
4) analyzing the inclusions, setting inclusion classification standards, and analyzing the detection result by using a computer inclusion analysis program to obtain the information of the number, size, shape and composition of the inclusions.
Further, the step 1) of grinding, polishing and cleaning the sample comprises the following steps:
1.1) grinding and polishing the embedded sample, wherein the granularity of sand paper selected in the grinding and polishing process on a grinding and polishing machine is sequentially from 180 meshes to 1200 meshes, and the grinding time of each granularity is 2-3 min; during polishing, the polishing solution sequentially selects diamond suspensions with the particle size of 2.5 micrometers and diamond suspensions with the particle size of 0.05 micrometers, and the polishing time is 2-3 min;
1.2) putting the polished metallographic sample into alcohol for ultrasonic cleaning for 10-15 min.
Further, the step 2) of setting analysis parameters of the scanning electron microscope and the X-ray energy spectrum comprises the following steps:
2.1) detecting the impurities by using a tungsten filament scanning electron microscope or a field emission scanning electron microscope, wherein the saturation current value of the filament is set to be 2.5-2.7A when the tungsten filament scanning electron microscope detects the impurities; when detecting the inclusions by a field emission scanning electron microscope, starting inclusion testing after applying high pressure for 20-30 min;
2.2) setting the working distance of the scanning electron microscope to be 8.5-10mm until the optimal working distance of the energy spectrum;
2.3) setting the voltage of an electron microscope at 15-20KV, adjusting the treatment time, adjusting the diaphragm and current mode of the scanning electron microscope, and setting the activation time, so that the dead time of the energy spectrum analysis of the aluminum foil substrate is 38-42%, and the impurity analysis count is 4500 or above.
Further, the setting of the inclusion detection parameter, the inclusion size parameter, the calibration parameter, the threshold parameter and the inclusion detection area in the step 3) includes:
3.1) setting the detection parameters of the inclusions, wherein the field of view is 2048 multiplied by 1536; the signal is backscattered electrons; the time for the first pass through the image is 8 milliseconds;
3.2) setting size parameters of the inclusions, and limiting the size of the minimum inclusions needing to be detected and the corresponding magnification in the detection characteristics;
3.3) setting calibration parameters, ensuring that a steel matrix and an aluminum foil exist in a view field at the same time, and adjusting the contrast and the brightness of a scanning electron microscope to ensure that the gray value of the steel matrix is 200 and the gray value of the aluminum foil is 40;
3.4) setting threshold parameters, setting the lower limit of the threshold to be 0 and setting the upper limit of the threshold to be 145-160, so that the number of detected inclusions and the coverage condition of the area detected by a single inclusion are matched with the real condition;
3.5) setting an inclusion detection area, and determining the inclusion detection area by using a diagonal line method or a four-point method.
The method of the invention is based on the following studies of the applicant:
in order to ensure the cleanness of the inclusion sample and ensure that the polished surface of the sample is not scratched or blurred due to artificial pits, foreign matters (such as polishing powder), diamond polishing solution is selected as the polishing solution, and the polished metallographic sample is put into alcohol for ultrasonic cleaning for 10-15 min.
Detecting impurities by using a tungsten filament scanning electron microscope or a field emission scanning electron microscope, adjusting filament current for the tungsten filament scanning electron microscope in order to obtain stable beam current, and setting the filament saturation current value to be 2.5-2.7A; when the inclusion is detected by a field emission scanning electron microscope, the inclusion test is started after high pressure is applied for 20-30 min.
The method can rapidly and automatically count the inclusions, is time-saving and labor-saving, has statistical significance and reliable results, and can focus on finer small-size inclusions and easily acquire the composition, type, shape, size and distribution stereological information of the inclusions.
Compared with the prior art, the invention has the following positive effects: 1. the method can simultaneously obtain the information of the inclusions with small size and large size under a certain fixed optimal working distance and amplification factor, and has the advantages of simple and convenient operation and high detection efficiency. 2. The method can rapidly and automatically count the impurities, saves time and labor, and has statistical significance, reliable result and high reproducibility. The method can carry out accurate qualitative and quantitative analysis on the attributes of inclusions in the steel, and has the advantages of accurate and comprehensive analysis and test, small artificial influence factors, and specific, accurate and visual evaluation results. 3. The method can obtain the composition, type, shape, size and distribution stereology information of the inclusions, and has the advantages of large analysis area, enough collected particle number and obvious statistical significance.
Detailed Description
The present invention will be further described with reference to specific examples, which are shown in tables 1 and 2.
Example 1, a billet having a thickness of 200mm and a mark of B500CL was examined and analyzed for inclusions.
A method for detecting and analyzing small-size nonmetallic inclusions in steel by using a scanning electron microscope comprises the following steps:
1) preparing a metallographic sample, and inlaying the surface of the sample to be detected by using a hot inlaying machine; polishing, polishing and cleaning the inlaid sample; attaching aluminum foil paper to an area, which is not to be analyzed, of the edge of the sample to obtain a metallographic sample; the sample is inlaid, ground, polished and cleaned, comprising,
1.1) selecting a continuous casting billet representative position, cutting a sample with the thickness of 15mm multiplied by 15mm, and inlaying the surface by a hot inlaying method by using a hot inlaying machine; grinding and polishing the embedded sample, wherein the granularity of sand paper selected in the grinding and polishing process on a grinding and polishing machine is sequentially from 180 meshes to 1200 meshes, and the grinding time of each granularity is 3 min; during polishing, diamond suspensions of 2.5 microns and 0.05 microns are sequentially selected as polishing solution, and the polishing time is 3 min;
1.2) in order to ensure the cleanness of the inclusion sample, putting the polished metallographic sample into alcohol for ultrasonic cleaning for 10 min;
2) regulating and controlling a scanning electron microscope and energy spectrum detection parameters, and placing the prepared metallographic sample in a scanning electron microscope sample chamber; setting analysis parameters of a scanning electron microscope and an X-ray energy spectrum, ensuring that the dead time of the energy spectrum analysis of the aluminum foil matrix is 38-42 percent, and the impurity analysis count is above 4500 percent; the setting of the analysis parameters of the scanning electron microscope and the X-ray energy spectrum comprises,
2.1) detecting the inclusions by using a field emission scanning electron microscope, and starting inclusion testing after the vacuum is reached and the high pressure is applied for 20 min;
2.2) setting the working distance of the scanning electron microscope to be 8.5mm until the optimal working distance of the energy spectrum is reached;
2.3) set the voltage of the field emission scanning electron microscope to 15KV, and use a probe (Signal): AsB, setting the processing time to be 5 and the active time to be 0.1, ensuring that the dead time of the energy spectrum analysis of the aluminum foil matrix reaches 40 percent and the impurity analysis count is 4500 or above;
3) detecting inclusions, namely detecting a metallographic sample to be detected by using a scanning electron microscope, and setting inclusion detection parameters, inclusion size parameters, calibration parameters, threshold parameters and an inclusion detection area to detect the inclusions; the inclusion detection parameters, the inclusion size parameters, the calibration parameters, the threshold parameters and the inclusion detection area are set, including,
3.1) setting the detection parameters of the inclusions, wherein the field of view is 2048 multiplied by 1536; the signal is backscattered electrons; the time for the first pass through the image is 8 milliseconds;
3.2) setting size parameters of the inclusions, inputting the minimum inclusion size to be detected to be 2 mu m in detection characteristics, and automatically giving a magnification factor of 58 x by a system;
3.3) setting calibration parameters, ensuring that a steel matrix and an aluminum foil exist in a view field at the same time, and adjusting the contrast and the brightness of a scanning electron microscope to ensure that the gray value of the steel matrix is 200 and the gray value of the aluminum foil is 40;
3.4) setting a threshold parameter, setting a lower threshold to be 0 and setting an upper threshold to be 160;
3.5) setting an inclusion detection area, and determining the inclusion detection area by using a diagonal method;
4) analyzing the inclusions, setting inclusion classification standards, and analyzing the detection results by using a computer inclusion analysis program to obtain the information of the number, size, shape and composition of the inclusions, which is shown in table 1.
Example 2 hot rolled steel sheet having a thickness of 2.5mm and a mark number of B550CL was examined and analyzed for inclusions.
A method for detecting and analyzing small-size nonmetallic inclusions in steel by using a scanning electron microscope comprises the following steps:
1) preparing a metallographic sample, and inlaying the surface of the sample to be detected by using a hot inlaying machine; polishing, polishing and cleaning the inlaid sample; attaching aluminum foil paper to an area, which is not to be analyzed, of the edge of the sample to obtain a metallographic sample; the sample is inlaid, ground, polished and cleaned, comprising,
1.1) selecting a representative position of a hot rolled plate, cutting a sample with the size of 20mm multiplied by 20mm, taking four blocks with the longitudinal sections of 2.5mm multiplied by 20mm, arranging the four blocks in parallel, and inlaying the four blocks by a hot inlaying machine through a hot inlaying method; grinding and polishing the embedded sample, wherein the granularity of sand paper selected in the grinding and polishing process on a grinding and polishing machine is sequentially from 180 meshes to 1200 meshes, and the grinding time of each granularity is 2 min; during polishing, diamond suspensions of 2.5 microns and 0.05 microns are sequentially selected as polishing solution, and the polishing time is 2 min;
1.2) in order to ensure the cleanness of the inclusion sample, putting the polished metallographic sample into alcohol for ultrasonic cleaning for 15 min;
2) regulating and controlling a scanning electron microscope and energy spectrum detection parameters, and placing the prepared metallographic sample in a scanning electron microscope sample chamber; setting analysis parameters of a scanning electron microscope and an X-ray energy spectrum, ensuring that the dead time of the energy spectrum analysis of the aluminum foil matrix is 38-42 percent, and the impurity analysis count is above 4500 percent; the setting of the analysis parameters of the scanning electron microscope and the X-ray energy spectrum comprises,
2.1) detecting inclusions by using a tungsten filament scanning electron microscope, and adjusting filament current after the vacuum is achieved to ensure that the saturation point of the filament current is 2.65A;
2.2) setting the working distance of the scanning electron microscope to be 8.5mm until the optimal working distance of the energy spectrum is reached;
2.3) setting the voltage of a tungsten filament scanning electron microscope to be 15KV, and using a probe (Signal): HDBSD, setting the treatment time to be 5 and the activation time to be 0.3, ensuring that the dead time of the energy spectrum analysis of the aluminum foil matrix reaches 40 percent and the impurity analysis count is above 4500 percent;
3) detecting inclusions, namely detecting a metallographic sample to be detected by using a scanning electron microscope, and setting inclusion detection parameters, inclusion size parameters, calibration parameters, threshold parameters and an inclusion detection area to detect the inclusions; the inclusion detection parameters, the inclusion size parameters, the calibration parameters, the threshold parameters and the inclusion detection area are set, including,
3.1) setting the detection parameters of the inclusions, wherein the field of view is 2048 multiplied by 1536; the signal is backscattered electrons; the time for the first pass through the image is 8 milliseconds;
3.2) setting size parameters of the inclusions, inputting the minimum inclusion size to be detected to be 1 mu m in detection characteristics, and automatically giving a magnification factor of 116 x by a system;
3.3) setting calibration parameters, ensuring that a steel matrix and an aluminum foil exist in a view field at the same time, and adjusting the contrast and the brightness of a scanning electron microscope to ensure that the gray value of the steel matrix is 200 and the gray value of the aluminum foil is 40;
3.4) setting a threshold parameter, setting a lower threshold to be 0 and setting an upper threshold to be 150;
3.5) setting an inclusion detection area, and determining the inclusion detection area by using a four-point method;
4) analyzing the inclusions, setting inclusion classification standards, and analyzing the detection results by using a computer inclusion analysis program to obtain the information of the number, size, shape and composition of the inclusions, which is shown in table 2.
TABLE 1 type, size and amount of inclusions in slab of example 1 of the present invention having a B500CL brand
TABLE 2 type, size and amount of inclusions in hot rolled steel sheet of brand No. B550CL in example 2 of the present invention
In addition to the above embodiments, the present invention may have other embodiments. All technical solutions formed by adopting equivalent substitutions or equivalent transformations fall within the protection scope of the claims of the present invention.
Claims (4)
1. A method for detecting and analyzing small-size nonmetallic inclusions in steel by using a scanning electron microscope is characterized by comprising the following steps:
1) preparing a metallographic sample, and inlaying the surface of the sample to be detected by using a hot inlaying machine; polishing, polishing and cleaning the inlaid sample; attaching aluminum foil paper to an area, which is not to be analyzed, of the edge of the sample to obtain a metallographic sample;
2) regulating and controlling a scanning electron microscope and energy spectrum detection parameters, and placing the prepared metallographic sample in a scanning electron microscope sample chamber; setting analysis parameters of a scanning electron microscope and an X-ray energy spectrum, ensuring that the dead time of the energy spectrum analysis of the aluminum foil matrix is 38-42 percent, and the impurity analysis count is above 4500 percent;
3) detecting inclusions, namely detecting a metallographic sample to be detected by using a scanning electron microscope, and setting inclusion detection parameters, inclusion size parameters, calibration parameters, threshold parameters and an inclusion detection area to detect the inclusions;
4) analyzing the inclusions, setting inclusion classification standards, and analyzing the detection result by using a computer inclusion analysis program to obtain the information of the number, size, shape and composition of the inclusions.
2. The method for detecting and analyzing small-sized nonmetallic inclusions in steel by using a scanning electron microscope as claimed in claim 1, wherein the step 1) of grinding, polishing and cleaning the test sample comprises the following steps:
1.1) grinding and polishing the embedded sample, wherein the granularity of sand paper selected in the grinding and polishing process on a grinding and polishing machine is sequentially from 180 meshes to 1200 meshes, and the grinding time of each granularity is 2-3 min; during polishing, the polishing solution sequentially selects diamond suspensions with the particle size of 2.5 micrometers and diamond suspensions with the particle size of 0.05 micrometers, and the polishing time is 2-3 min;
1.2) putting the polished metallographic sample into alcohol for ultrasonic cleaning for 10-15 min.
3. The method for detecting and analyzing small-sized nonmetallic inclusions in steel by using a scanning electron microscope as claimed in claim 1, wherein the step 2) of setting the analysis parameters of the scanning electron microscope and the X-ray energy spectrum comprises the following steps:
2.1) detecting the impurities by using a tungsten filament scanning electron microscope or a field emission scanning electron microscope, wherein the saturation current value of the filament is set to be 2.5-2.7A when the tungsten filament scanning electron microscope detects the impurities; when detecting the inclusions by a field emission scanning electron microscope, starting inclusion testing after applying high pressure for 20-30 min;
2.2) setting the working distance of the scanning electron microscope to be 8.5-10mm until the optimal working distance of the energy spectrum;
2.3) setting the voltage of an electron microscope at 15-20KV, adjusting the treatment time, adjusting the diaphragm and current mode of the scanning electron microscope, and setting the activation time, so that the dead time of the energy spectrum analysis of the aluminum foil substrate is 38-42%, and the impurity analysis count is 4500 or above.
4. The method for detecting and analyzing small-sized nonmetallic inclusions in steel by using a scanning electron microscope as claimed in claim 1, wherein the setting of the inclusion detection parameters, the inclusion size parameters, the calibration parameters, the threshold parameters and the inclusion detection area in step 3) comprises:
3.1) setting the detection parameters of the inclusions, wherein the field of view is 2048 multiplied by 1536; the signal is backscattered electrons; the time for the first pass through the image is 8 milliseconds;
3.2) setting size parameters of the inclusions, and limiting the size of the minimum inclusions needing to be detected and the corresponding magnification in the detection characteristics;
3.3) setting calibration parameters, ensuring that a steel matrix and an aluminum foil exist in a view field at the same time, and adjusting the contrast and the brightness of a scanning electron microscope to ensure that the gray value of the steel matrix is 200 and the gray value of the aluminum foil is 40;
3.4) setting a threshold parameter, setting a lower threshold to be 0, and setting an upper threshold to be 145-160;
3.5) setting an inclusion detection area, and determining the inclusion detection area by using a diagonal line method or a four-point method.
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| CN202010568468.6A CN113899763B (en) | 2020-06-19 | 2020-06-19 | Method for detecting and analyzing small-size nonmetallic inclusion in steel by using scanning electron microscope |
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| CN114636802A (en) * | 2022-02-16 | 2022-06-17 | 大冶特殊钢有限公司 | Method for detecting purity of molten steel in smelting process |
| CN117147601A (en) * | 2023-10-31 | 2023-12-01 | 钢研纳克检测技术股份有限公司 | Quantitative statistical characterization method for rare earth elements in different states and distribution of rare earth elements in steel |
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|---|---|---|---|---|
| CN114441580A (en) * | 2022-01-28 | 2022-05-06 | 首钢集团有限公司 | Identification method of non-metal inclusion phase |
| CN114636802A (en) * | 2022-02-16 | 2022-06-17 | 大冶特殊钢有限公司 | Method for detecting purity of molten steel in smelting process |
| CN114636802B (en) * | 2022-02-16 | 2023-11-28 | 大冶特殊钢有限公司 | Method for detecting purity of molten steel in smelting process |
| CN117147601A (en) * | 2023-10-31 | 2023-12-01 | 钢研纳克检测技术股份有限公司 | Quantitative statistical characterization method for rare earth elements in different states and distribution of rare earth elements in steel |
| CN117147601B (en) * | 2023-10-31 | 2024-01-30 | 钢研纳克检测技术股份有限公司 | Quantitative statistical characterization method for rare earth elements in different states and distribution of rare earth elements in steel |
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