CN113899763B - Method for detecting and analyzing small-size nonmetallic inclusion in steel by using scanning electron microscope - Google Patents
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- 238000001514 detection method Methods 0.000 claims abstract description 51
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- 239000010937 tungsten Substances 0.000 claims description 8
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
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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 proposal is that the method for detecting and analyzing the small-size nonmetallic inclusion in the steel by using the 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 thermal inlaying machine; polishing, polishing and cleaning the inlaid sample; attaching aluminum foil paper to the area where the edge of the sample is not analyzed to obtain a metallographic sample; 2) Regulating and controlling scanning electron microscope and energy spectrum detection parameters; 3) Detecting inclusions; 4) And 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, the size, the shape and the components of the inclusions. The method has the advantages of simple operation, high efficiency and high accuracy for qualitatively and quantitatively analyzing the nonmetallic inclusions with small size in the steel.
Description
Technical Field
The invention relates to a method for analyzing nonmetallic inclusion in steel materials, in particular to a method for detecting and analyzing small-size nonmetallic inclusion in steel by using a scanning electron microscope, belonging to the technical field of steel material analysis and detection.
Background
With the development of modern refining technology, the cleanliness of steel is greatly improved, and the understanding of nonmetallic inclusion in steel is also started to be used as a harmful substance which can reduce the plasticity, toughness and fatigue performance of steel, so that the cold and hot workability of steel is changed into the control of nonmetallic inclusion in steel to influence the performance of steel products. Therefore, the method for detecting the nonmetallic inclusion in the steel by the non-metallic inclusion detection has very important significance for researching the information such as the quantity, the shape, the size, the distribution condition and the like of nonmetallic inclusions in the steel and developing corresponding detection on the performance analysis, the reasonable use and the like of steel products.
At present, in the detection technology for determining nonmetallic inclusion in steel materials at home and abroad, the most common conventional methods such as metallographic method, electrolytic method and in-situ analysis method are adopted, but the methods have certain limitations, cannot meet the requirement of all analysis of small-size inclusion in steel samples, cannot meet the requirements of detection accuracy and detection efficiency, and seriously influence development of scientific research and research such as new product development, process improvement and the like.
The back scattering electrons mainly reflect the component characteristics of the sample surface, namely, the parts with larger atomic numbers of the sample generate stronger back scattering electron signals, and a brighter area is formed on the fluorescent screen; and the lower average atomic number sites produce less backscattered electrons, forming darker areas on the screen, thus resulting in atomic number contrast. The scanning electron microscope back scattering electron morphology image can effectively identify the inclusions, the X-ray energy spectrum analysis can analyze the components of the corresponding inclusions, but the analysis of the inclusions by the scanning electron microscope method is generally limited to the targeted analysis of one or more specified inclusions, and can not meet the total analysis of the sizes, shapes, types and the like of the inclusions in the steel, especially the accurate analysis of the small-size inclusions.
The Chinese patent application with the application publication number of CN108593649A discloses a qualitative and quantitative method for testing and analyzing inclusions in steel, wherein the size range of the inclusions is determined by observing a sample to be tested in a metallographic phase, and the test parameters of a scanning electron microscope are adjusted according to the range to perform scanning electron microscope testing and EDS energy spectrum analysis on the sample to be tested to obtain the size, shape and composition data of the inclusions in the steel. According to the method, different test parameters and scanning areas of the scanning electron microscope are correspondingly adjusted according to different inclusion sizes of metallographic observation, the working distance of the scanning electron microscope is 15-20mm, the operation process is continuously switched, the working voltage and the working distance range are greatly changed, and the influence on the accuracy and reproducibility of results is great.
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, 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 of the invention is that the method for detecting and analyzing small-size nonmetallic inclusion 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 thermal inlaying machine; polishing, polishing and cleaning the inlaid sample; attaching aluminum foil paper to the area where the edge of the sample is not analyzed to obtain a metallographic sample;
2) Regulating and controlling scanning electron microscope and energy spectrum detection parameters, and placing the prepared metallographic sample in a scanning electron microscope sample chamber; setting scanning electron microscope and X-ray energy spectrum analysis parameters to ensure that the energy spectrum analysis dead time of the aluminum foil substrate is 38-42% and the inclusion analysis count is above 4500;
3) Detecting the inclusion, detecting a metallographic sample to be detected by using a scanning electron microscope, setting inclusion detection parameters, inclusion size parameters, calibration parameters, threshold parameters and inclusion detection areas, and detecting the inclusion;
4) And 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, the size, the shape and the components of the inclusions.
Further, step 1) of polishing, polishing and cleaning the sample comprises:
1.1 Polishing the embedded sample, wherein the granularity of sand paper is selected from 180 meshes to 1200 meshes in sequence in the polishing process on a polishing machine, and the polishing time of each granularity is 2-3min; the polishing solution sequentially selects diamond suspension liquid with the thickness of 2.5 mu m and diamond suspension liquid with the thickness of 0.05 mu m during polishing, and the polishing time is 2-3min;
1.2 Placing the polished metallographic sample into alcohol for ultrasonic cleaning for 10-15min.
Further, the setting of the scanning electron microscope and the X-ray energy spectrum analysis parameters in the step 2) includes:
2.1 The inclusion is detected by a tungsten filament scanning electron microscope or a field emission scanning electron microscope, and when the inclusion is detected by the tungsten filament scanning electron microscope, the saturation current value of the filament is set to be 2.5-2.7A; when the field emission scanning electron microscope detects the inclusion, the inclusion test is started after the high pressure is applied for 20-30 min;
2.2 Setting the working distance of the scanning electron microscope to be 8.5-10mm in the optimal working distance of the energy spectrum;
2.3 Setting the electron microscope voltage to 15-20KV, adjusting the processing time, adjusting the scanning electron microscope diaphragm and the current mode, and setting the activation time so that the energy spectrum analysis dead time of the aluminum foil substrate is 38-42% and the inclusion analysis count is above 4500.
Further, the setting of the inclusion detection parameter, the inclusion size parameter, the calibration parameter, the threshold parameter, and the inclusion detection region in step 3) includes:
3.1 Inclusion detection parameters set, field of view is 2048×1536; the signal is back scattered electrons; the time to first pass the image is 8 milliseconds;
3.2 Setting inclusion size parameters, and limiting the size and corresponding magnification of the minimum inclusion to be detected in the detection characteristics;
3.3 The calibration parameters are set, the steel matrix and the aluminum foil are ensured to be simultaneously arranged in the view field, and the contrast and the brightness of the scanning electron microscope are adjusted to ensure that the gray value of the steel matrix is 200 and the gray value of the aluminum foil is 40;
3.4 A threshold parameter is set, a threshold lower limit is set to 0, and a threshold upper limit is set to 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 actual condition;
3.5 The inclusion detection area is set, and the inclusion detection area is determined by a diagonal method or a four-point method.
The method of the invention is based on the following studies by the applicant:
in order to ensure that the inclusion sample is clean and the polished surface of the sample is free from artificial pits, foreign matters (such as polishing powder), scratches or blurs, the polishing solution is diamond polishing solution, and the polished metallographic sample is put into alcohol for ultrasonic cleaning for 10-15min.
Detecting impurities by using a tungsten filament scanning electron microscope or a field emission scanning electron microscope, and adjusting filament current of the tungsten filament scanning electron microscope to set a filament saturation current value to be 2.5-2.7A in order to obtain stable beam current; when the field emission scanning electron microscope detects the inclusion, the inclusion test is started after the high pressure is applied for 20-30 min.
The method can rapidly and automatically count the inclusions, saves time and labor, has statistical significance and reliable result, and can pay attention to finer small-size inclusions and easily acquire the components, types, shapes, sizes and distribution of the inclusions.
Compared with the prior art, the invention has the following positive effects: 1. the method can obtain the information of the small-size and large-size inclusions at the same time under a certain fixed optimal working distance and magnification, and has the advantages of simple operation and high detection efficiency. 2. The method can rapidly and automatically count the inclusions, saves time and labor, has statistical significance, and has reliable results and high reproducibility. The method can accurately, qualitatively and quantitatively analyze the attribute of the inclusion in the steel, has accurate and comprehensive analysis and test, small artificial influence factors and specific, accurate and visual evaluation results. 3. The method can obtain the components, types, shapes, sizes and distribution stereology information of the inclusions, and has large analysis area, enough collected particle numbers and obvious statistical significance.
Detailed Description
The invention is further illustrated below with reference to specific examples, as shown in tables 1, 2.
Example 1, inclusions of a continuous casting slab having a grade B500CL with a thickness of 200mm were detected and analyzed.
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 thermal inlaying machine; polishing, polishing and cleaning the inlaid sample; attaching aluminum foil paper to the area where the edge of the sample is not analyzed to obtain a metallographic sample; the embedding, buffing, polishing and cleaning of the test specimen includes,
1.1 Selecting a representative position of a continuous casting blank, cutting a sample 15mm multiplied by 15mm, and inlaying the surface by a thermal inlaying machine through a thermal inlaying method; polishing the inlaid sample, wherein the granularity of sand paper is selected from 180 meshes to 1200 meshes in sequence in the polishing process on a polishing machine, and the polishing time of each granularity is 3min; the polishing solution sequentially selects diamond suspension liquid with the thickness of 2.5 mu m and diamond suspension liquid with the thickness of 0.05 mu m during polishing, and the polishing time is 3min;
1.2 In order to ensure that the inclusion samples are clean, placing the polished metallographic samples into alcohol for ultrasonic cleaning for 10min;
2) Regulating and controlling scanning electron microscope and energy spectrum detection parameters, and placing the prepared metallographic sample in a scanning electron microscope sample chamber; setting scanning electron microscope and X-ray energy spectrum analysis parameters to ensure that the energy spectrum analysis dead time of the aluminum foil substrate is 38-42% and the inclusion analysis count is above 4500; the setting of the scanning electron microscope and the X-ray energy spectrum analysis parameters comprises,
2.1 Detecting the inclusion by using a field emission scanning electron microscope, and starting the inclusion test after the vacuum is up and the pressure is increased for 20 min;
2.2 Setting the working distance of the scanning electron microscope to be 8.5mm from the optimal working distance of the energy spectrum;
2.3 Setting the voltage of a field emission scanning electron microscope to 15KV, and using a probe (Signal): asB, setting the treatment time to be 5, and the living time to be 0.1, so as to ensure that the energy spectrum analysis dead time of the aluminum foil matrix reaches 40%, and the inclusion analysis count is more than 4500;
3) Detecting the inclusion, detecting a metallographic sample to be detected by using a scanning electron microscope, setting inclusion detection parameters, inclusion size parameters, calibration parameters, threshold parameters and inclusion detection areas, and detecting the inclusion; the setting of the inclusion detection parameter, the inclusion size parameter, the calibration parameter, the threshold parameter and the inclusion detection area comprises,
3.1 Inclusion detection parameters set, field of view is 2048×1536; the signal is back scattered electrons; the time to first pass the image is 8 milliseconds;
3.2 Setting inclusion size parameters, inputting the size of the minimum inclusion to be detected to be 2 mu m in the detection characteristics, and automatically giving the magnification of 58×;
3.3 The calibration parameters are set, the steel matrix and the aluminum foil are ensured to be simultaneously arranged in the view field, and the contrast and the brightness of the scanning electron microscope are adjusted to ensure that the gray value of the steel matrix is 200 and the gray value of the aluminum foil is 40;
3.4 A) threshold parameter setting, a threshold lower limit is set to 0, and a threshold upper limit is set to 160;
3.5 Setting an inclusion detection area, and determining the inclusion detection area by a diagonal method;
4) The inclusions were analyzed, inclusion classification criteria were set, and the detection results were analyzed by a computer inclusion analysis program to obtain the information on the number, size, shape and composition of inclusions, as shown in table 1.
Example 2, inclusions of a hot rolled plate having a grade B550CL having a thickness of 2.5mm were examined and analyzed.
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 thermal inlaying machine; polishing, polishing and cleaning the inlaid sample; attaching aluminum foil paper to the area where the edge of the sample is not analyzed to obtain a metallographic sample; the embedding, buffing, polishing and cleaning of the test specimen includes,
1.1 Selecting a representative position of a hot rolled plate, cutting a sample of 20mm multiplied by 20mm, taking four pieces of the sample with the longitudinal section of 2.5mm multiplied by 20mm, discharging the four pieces together, and inlaying the four pieces by a thermal inlaying method by using a thermal inlaying machine; polishing the inlaid sample, wherein the granularity of sand paper is selected from 180 meshes to 1200 meshes in sequence in the polishing process on a polishing machine, and the polishing time of each granularity is 2min; the polishing solution sequentially selects diamond suspension liquid with the thickness of 2.5 mu m and diamond suspension liquid with the thickness of 0.05 mu m during polishing, and the polishing time is 2min;
1.2 In order to ensure that the inclusion samples are clean, placing the polished metallographic samples into alcohol for ultrasonic cleaning for 15min;
2) Regulating and controlling scanning electron microscope and energy spectrum detection parameters, and placing the prepared metallographic sample in a scanning electron microscope sample chamber; setting scanning electron microscope and X-ray energy spectrum analysis parameters to ensure that the energy spectrum analysis dead time of the aluminum foil substrate is 38-42% and the inclusion analysis count is above 4500; the setting of the scanning electron microscope and the X-ray energy spectrum analysis parameters comprises,
2.1 Detecting impurities by using a tungsten filament scanning electron microscope, and adjusting filament current after 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 from the optimal working distance of the energy spectrum;
2.3 Setting the voltage of a tungsten filament scanning electron microscope to 15KV, and using a probe (Signal): HDBSD, setting a treatment time of 5 and a living time of 0.3, and ensuring that the energy spectrum analysis dead time of the aluminum foil substrate reaches 40% and the inclusion analysis count is more than 4500;
3) Detecting the inclusion, detecting a metallographic sample to be detected by using a scanning electron microscope, setting inclusion detection parameters, inclusion size parameters, calibration parameters, threshold parameters and inclusion detection areas, and detecting the inclusion; the setting of the inclusion detection parameter, the inclusion size parameter, the calibration parameter, the threshold parameter and the inclusion detection area comprises,
3.1 Inclusion detection parameters set, field of view is 2048×1536; the signal is back scattered electrons; the time to first pass the image is 8 milliseconds;
3.2 Setting inclusion size parameters, inputting the size of the minimum inclusion to be detected to be 1 mu m in the detection characteristics, and automatically giving the magnification of 116×;
3.3 The calibration parameters are set, the steel matrix and the aluminum foil are ensured to be simultaneously arranged in the view field, and the contrast and the brightness of the scanning electron microscope are adjusted to ensure that the gray value of the steel matrix is 200 and the gray value of the aluminum foil is 40;
3.4 A) threshold parameter setting, a threshold lower limit is set to 0, and a threshold upper limit setting is set to 150;
3.5 Setting an inclusion detection area, and determining the inclusion detection area by a four-point method;
4) The inclusions were analyzed, inclusion classification criteria were set, and the detection results were analyzed by a computer inclusion analysis program to obtain the information on the number, size, shape and composition of inclusions, as shown in table 2.
TABLE 1 type, size and quantity of inclusions in continuous casting slab having a grade B500CL according to example 1 of the present invention
TABLE 2 type, size and quantity of inclusions in hot rolled plate having a grade B550CL according to example 2 of the invention
In addition to the embodiments described above, other embodiments of the invention are possible. All technical schemes formed by equivalent substitution or equivalent transformation fall within the protection scope of the invention.
Claims (3)
1. A method for detecting and analyzing small-size nonmetallic inclusions in steel by using a scanning electron microscope, which is characterized by comprising the following steps:
step 1) preparing a metallographic sample, and inlaying the surface of the sample to be tested by using a thermal inlaying machine; polishing, polishing and cleaning the inlaid sample; attaching aluminum foil paper to the area where the edge of the sample is not analyzed to obtain a metallographic sample;
step 2) regulating and controlling scanning electron microscope and energy spectrum detection parameters, and placing the prepared metallographic sample in a scanning electron microscope sample chamber; setting scanning electron microscope and X-ray energy spectrum analysis parameters to ensure that the energy spectrum analysis dead time of the aluminum foil substrate is 38-42% and the inclusion analysis count is above 4500;
and 3) detecting the inclusion, detecting a metallographic sample to be detected by using a scanning electron microscope, setting an inclusion detection parameter, an inclusion size parameter, a calibration parameter, a threshold parameter and an inclusion detection area, and detecting the inclusion, wherein the setting of the inclusion detection parameter, the inclusion size parameter, the calibration parameter, the threshold parameter and the inclusion detection area comprises the following steps:
3.1 Inclusion detection parameters set, field of view is 2048×1536; the signal is back scattered electrons; the time to first pass the image is 8 milliseconds;
3.2 Setting inclusion size parameters, and limiting the size and corresponding magnification of the minimum inclusion to be detected in the detection characteristics;
3.3 The calibration parameters are set, the steel matrix and the aluminum foil are ensured to be simultaneously arranged in the view field, and the contrast and the brightness of the scanning electron microscope are adjusted to ensure that the gray value of the steel matrix is 200 and the gray value of the aluminum foil is 40;
3.4 A) setting a threshold parameter, wherein the lower threshold limit is set to 0, and the upper threshold limit is set to 145-160;
3.5 Setting an inclusion detection area, and determining the inclusion detection area by a diagonal method or a four-point method;
and 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, the size, the shape and the components of the inclusions.
2. The method for analyzing small-sized nonmetallic inclusions in steel by scanning electron microscopy according to claim 1, wherein the step 1) of polishing, buffing, and cleaning the sample comprises:
1.1 Polishing the embedded sample, wherein the granularity of sand paper is selected from 180 meshes to 1200 meshes in sequence in the polishing process on a polishing machine, and the polishing time of each granularity is 2-3min; the polishing solution sequentially selects diamond suspension liquid with the thickness of 2.5 mu m and diamond suspension liquid with the thickness of 0.05 mu m during polishing, and the polishing time is 2-3min;
1.2 Placing the polished metallographic sample into alcohol for ultrasonic cleaning for 10-15min.
3. The method for detecting and analyzing small-sized nonmetallic inclusions in steel by using a scanning electron microscope as set forth in claim 1, wherein the setting of scanning electron microscope and X-ray energy spectrum analysis parameters in the step 2) includes:
2.1 The inclusion is detected by a tungsten filament scanning electron microscope or a field emission scanning electron microscope, and when the inclusion is detected by the tungsten filament scanning electron microscope, the saturation current value of the filament is set to be 2.5-2.7A; when the field emission scanning electron microscope detects the inclusion, the inclusion test is started after the high pressure is applied for 20-30 min;
2.2 Setting the electron microscope voltage to 15-20KV, adjusting the processing time, adjusting the scanning electron microscope diaphragm and the current mode, and setting the activation time so that the energy spectrum analysis dead time of the aluminum foil substrate is 38-42% and the inclusion analysis count is above 4500.
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