CN106908436B - The analysis ranking method of manganese sulfide type impurity in steel based on calibration curve - Google Patents
The analysis ranking method of manganese sulfide type impurity in steel based on calibration curve Download PDFInfo
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- CADICXFYUNYKGD-UHFFFAOYSA-N sulfanylidenemanganese Chemical compound [Mn]=S CADICXFYUNYKGD-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 238000011088 calibration curve Methods 0.000 title claims abstract description 54
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 51
- 239000010959 steel Substances 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 41
- 238000004458 analytical method Methods 0.000 title claims abstract description 37
- 239000012535 impurity Substances 0.000 title abstract 4
- 239000000463 material Substances 0.000 claims abstract description 43
- 238000002679 ablation Methods 0.000 claims abstract description 39
- 239000011572 manganese Substances 0.000 claims description 47
- 229910052717 sulfur Inorganic materials 0.000 claims description 29
- 229910052748 manganese Inorganic materials 0.000 claims description 28
- 238000002536 laser-induced breakdown spectroscopy Methods 0.000 claims description 25
- 230000005284 excitation Effects 0.000 claims description 19
- 238000009826 distribution Methods 0.000 claims description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 238000004364 calculation method Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000005259 measurement Methods 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 3
- 239000006104 solid solution Substances 0.000 claims description 3
- 230000015556 catabolic process Effects 0.000 abstract description 4
- 238000002203 pretreatment Methods 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 36
- 230000002159 abnormal effect Effects 0.000 description 4
- 238000007689 inspection Methods 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- 244000137852 Petrea volubilis Species 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 229910000915 Free machining steel Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000001636 atomic emission spectroscopy Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
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- 230000000052 comparative effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
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- 238000009776 industrial production Methods 0.000 description 1
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- 238000005070 sampling Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 238000007655 standard test method Methods 0.000 description 1
- 238000007619 statistical method Methods 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
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Abstract
The invention belongs to the surface micro-region analysis technique fields in materials science field, in particular to a kind of to use laser induced breakdown spectrograph, the analysis ranking method of manganese sulfide type impurity in the steel based on calibration curve.This method comprises the following steps: (a) obtaining calibration curve；(b) scanning analysis sample；(c) ablation spot is measured；(d) interpretation of result.What the present invention acquired is the signal strength of manganese sulfide type impurity component, and the length or area of manganese sulfide type impurity are obtained by using calibration curve inverting；Sample pre-treatments are simple, analysis speed is fast, scan area range is big.
Description
Technical Field
The invention belongs to the technical field of surface micro-area analysis in the field of material science, and particularly relates to an analysis and rating method for manganese sulfide inclusions in steel based on a calibration curve by using a laser-induced breakdown spectrometer.
Background
The modern industry has higher and higher requirements on the processing performance of steel products, a certain amount of sulfur is required to be contained in steel, the cutting performance is improved by utilizing the generated sulfide, and simultaneously, the content and the form of the sulfide are required to be controlled in order to ensure the comprehensive mechanical property. The method can be used for analyzing the content and distribution of the manganese sulfide inclusions in the material, and the method is mainly used in material research and industrial production in a metallographic microscope, a scanning electron microscope/energy spectrometer (SEM/EDS), an Electron Probe (EPMA) and the like, and forms standard inspection methods such as GB/T10561, ISO 4967, ASTM E45, DIN50602, EN10247 and the like. The method has the defects that the pretreatment of the steel material sample is very complicated, the analysis speed is slow, the observed area is very small, and the rapid full-automatic analysis in a large-size range is difficult to realize.
Laser Induced Breakdown Spectroscopy (LIBS) is an atomic emission spectroscopy analysis method which develops rapidly in the last thirty years, has the advantages of simple sample preparation, high analysis speed, small sample ablation amount, easy realization of on-line and remote analysis and the like, and has wide application prospect in the field of metallurgy. In the process of researching nonmetallic inclusions in steel by using laser-induced breakdown spectroscopy, the length and area of the inclusions, the signal intensity and the content of characteristic elements have a good linear relationship, and based on the characteristics of the rules, the invention provides an analysis method for determining the content of manganese sulfide inclusions by using the laser-induced breakdown spectroscopy.
Disclosure of Invention
The invention aims to provide an analysis and rating method for manganese sulfide inclusions in steel based on a calibration curve by adopting a laser-induced breakdown spectrometer, which is used for statistical analysis of the content and distribution of the manganese sulfide inclusions in steel materials.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides a method for analyzing and grading manganese sulfide inclusions in steel based on a calibration curve, which comprises the following steps:
a. obtaining a calibration curve:
obtaining a relation curve of length-signal intensity of the manganese sulfide inclusion in the steel material as a calibration curve or obtaining a relation curve of area-signal intensity of the manganese sulfide inclusion in the steel material as a calibration curve by combining a laser-induced breakdown spectroscopy instrument with a metallographic microscope or a scanning electron microscope;
or obtaining an element concentration-signal intensity relation curve as a calibration curve by using a series of steel material standard samples;
b. scanning analysis of the sample:
grinding the surface of a sample to be analyzed, and performing two-dimensional scanning analysis on the steel material sample to be analyzed by using a laser-induced breakdown spectroscopy instrument under a protective atmosphere environment to obtain two-dimensional distribution of signal intensity of S and Mn elements;
c. measurement of ablation spots:
b, under a metallographic microscope or a scanning electron microscope, directly measuring or assisting with geometric calculation to obtain the size, the area and the scanning step length of the excitation area of the ablation spots after the steel material sample in the step b is scanned and analyzed, and determining the size of the rating field of view according to the scanning step length, namely determining the number of the ablation spots in the rating field of view;
d. and (4) analyzing results:
and (c) calculating the length or the area of the manganese sulfide inclusion in the rating field of view by using the calibration curve obtained in the step (a) and the ablation spot measurement result obtained in the step (c) and combining the two-dimensional distribution data of the signal intensity of the S and Mn elements obtained by scanning and analyzing in the step (b), then converting the length or the area of the manganese sulfide inclusion, and finally rating according to the converted length or the converted area of the manganese sulfide inclusion.
In the step a, when a manganese sulfide inclusion length-signal intensity relation curve or a manganese sulfide inclusion area-signal intensity relation curve is used as a calibration curve, signals of S or Mn elements are used independently or signals of S and Mn elements are used simultaneously; selecting a material which is the same as or similar to a steel material sample to be analyzed, firstly obtaining a distribution map of the manganese sulfide inclusion on a steel material sample inspection surface by using a metallographic microscope or a scanning electron microscope, then scanning the steel material sample by using a laser-induced breakdown spectrum, extracting length or area information of the manganese sulfide inclusion in an excitation region of an ablation spot where an abnormal signal is located, and obtaining a relation curve between the length or area of the manganese sulfide inclusion in the steel material and S and/or Mn element signal intensity by counting the abnormal signals.
In the step a, when the element concentration-signal intensity relation curve is used as a calibration curve, signals of S or Mn elements are used independently, or signals of S and Mn elements are used simultaneously; selecting a series of standard samples of the steel materials which are similar to the steel material samples to be analyzed and have different S and/or Mn contents; and (3) statistically obtaining a relation curve of S and/or Mn element concentration-signal intensity by exciting a series of steel material standard samples.
The working parameters of the laser-induced breakdown spectroscopy instrument are set as follows:
the pulse energy adjustment range is 0 mJ-900 mJ;
the distance from the lens to the surface of the sample is 17 mm-28 mm;
filling high-purity argon into the sample chamber, wherein the purity is 99.999 percent, and the air pressure is 1000-10000 Pa;
the delay time of the S element is 1 mu S;
the delay time of Mn element was 1.5. mu.s.
Preferably, the operating parameters of the laser induced breakdown spectroscopy instrument are set as follows:
the pulse energy of the laser-induced breakdown spectroscopy instrument is 300 mJ;
the distance from the lens to the surface of the sample is 23 mm;
introducing high-purity argon into the sample chamber, wherein the purity is 99.999 percent, and the air pressure is 4000 Pa;
the delay time of the S element is 1 mu S;
the delay time of Mn element was 1.5. mu.s.
In the step c, the shape of the rating field is square, and the size of the rating field is 0.5 +/-0.1 mm specified in the metallographic examination standard2Square standard field of view.
In the step d, when a manganese sulfide inclusion length-signal intensity relation curve or a manganese sulfide inclusion area-signal intensity relation curve is used as a calibration curve, the calibration curve is directly used to obtain the length or the area of the manganese sulfide inclusion in the excitation area; the process is as follows:
firstly, a linear equation of a calibration curve is obtained by adopting a linear fitting mode, and then the signal intensity values of different analysis positions are substituted into the linear equation to calculate the length or the area of the manganese sulfide inclusions.
In the step d, when the element concentration-signal intensity is used as a calibration curve, firstly, a linear equation of the calibration curve is obtained in a linear fitting mode, then, the two-dimensional distribution data of the element signal intensity obtained by scanning and analyzing in the step b is substituted into the linear equation of the calibration curve to calculate the element concentration of different analysis positions, and then, the area of the manganese sulfide inclusion in the ablation excitation area of each analysis position is calculated according to the element concentration, wherein the calculation formula is as follows:
in the formula,
CSand CMnThe concentrations of S and Mn are respectively calculated by a linear equation of the S and Mn element signal intensities obtained by scanning analysis in the step b and taken into a calibration curve, and the concentrations are known quantities;
CS0and CMn0The solid solution concentrations of S and Mn, respectively, are known amounts;
Strepresenting the area of the ablation excitation area as a known quantity measured in step c;
SMnSthe area of MnS inclusions in the ablation excitation area is shown.
In step d, the area covered by the ablation spot in a single field of view analyzed by the laser-induced breakdown spectroscopy instrument is not strictly equal to 0.5mm2After the length or area of the MnS inclusion is calculated by using the calibration curve, the length or area of the MnS inclusion is multiplied by a conversion coefficient k to be converted into 0.5mm2The total length or total area of MnS inclusions in the equivalent area, and the conversion coefficient k is calculated by the following formula:
in the formula,
ntrating the number of ablation spots in the field of view;
Sithe area of the excitation zone of a single ablation spot.
Compared with the prior art, the invention has the beneficial effects that:
1. the existing inspection method for the manganese sulfide inclusion, such as GB/T10561, ISO 4967, ASTM E45, DIN50602, EN10247 and the like, directly observes and measures the manganese sulfide inclusion in a standard visual field on a prepared metallographic specimen by using a microscope, and grades the manganese sulfide inclusion according to the length or the area of the manganese sulfide inclusion. The invention belongs to an indirect method, which acquires the signal intensity of the constituent elements of the manganese sulfide inclusion and obtains the length or the area of the manganese sulfide inclusion by using a calibration curve for inversion.
2. The existing metallographic examination method needs to prepare a sample into a mirror surface with high finish degree, the requirement on surface cleanliness is high, any surface adhesion can interfere with the examination, and the influence of the sample preparation on the examination result is large. The sample preparation process is simple, the surface of the sample is only ground by using sand paper or a grinding wheel, a small amount of pollutants are allowed to exist on the surface, and the pollutants can be removed by a pre-ablation method.
3. The invention can use the sample used by the existing standard test method, and the principles and methods of sampling and sample preparation are similar, thereby conveniently realizing the result comparative analysis of several different detection methods.
4. Compared with the existing method, the method for analyzing the content of the manganese sulfide inclusion in the steel material has the advantages of simple sample pretreatment, high analysis speed and large scanning area range.
Drawings
FIG. 1 is a flow chart of a method for analyzing and grading manganese sulfide inclusions in steel based on a calibration curve according to the invention;
FIG. 2 is a graph showing the morphology of the ablation spots after scanning analysis of the steel material sample according to the embodiment of the present invention;
FIG. 3 is a calibration curve of the area of a manganese sulfide inclusion versus the signal intensity of the S element in the embodiment of the present invention;
FIG. 4 is a calibration curve of Mn element concentration versus signal intensity according to an embodiment of the present invention;
FIG. 5 is a calculated curve of the area of a manganese sulfide inclusion-the concentration of Mn element in the example of the present invention.
Detailed Description
The invention is further illustrated with reference to the following figures and examples.
The invention relates to a method for analyzing and grading manganese sulfide inclusions in steel based on a calibration curve, wherein the analyzing and grading process is shown in figure 1 and comprises the following steps:
(a) obtaining a calibration curve:
obtaining a relation curve of length-signal intensity of the manganese sulfide inclusion in the steel material as a calibration curve or obtaining a relation curve of area-signal intensity of the manganese sulfide inclusion in the steel material (as shown in figure 3) as a calibration curve by combining a Laser Induced Breakdown Spectroscopy (LIBS) instrument with a metallographic microscope or a scanning electron microscope;
or an element concentration-signal intensity relation curve (as shown in fig. 4) is obtained as a calibration curve by using a series of standard samples of steel materials.
Wherein,
when the relation curve of the length of the manganese sulfide inclusion and the signal intensity or the relation curve of the area of the manganese sulfide inclusion and the signal intensity is used as a calibration curve, the signal of the S or Mn element can be used independently, and the signal of the S and Mn elements can also be used simultaneously. Selecting a material which is the same as or similar to a steel material sample to be analyzed, firstly obtaining a distribution map of the manganese sulfide inclusion on a steel material sample inspection surface by using a metallographic microscope or a scanning electron microscope, then scanning the steel material sample by using a Laser Induced Breakdown Spectroscopy (LIBS), extracting length or area information of the manganese sulfide inclusion in an excitation area of an ablation spot where an abnormal signal is located, and obtaining a relation curve between the length or area of the manganese sulfide inclusion in the steel material and S and/or Mn element signal intensity by counting the abnormal signals.
When the element concentration-signal intensity relation curve is used as the calibration curve, the signal of the S or Mn element can be used independently, and the signal of the S and Mn elements can also be used simultaneously. A series of standard samples of ferrous material similar to the sample of ferrous material to be analyzed and having different contents of S and/or Mn should be selected. And (3) statistically obtaining a relation curve of S and/or Mn element concentration-signal intensity by exciting a series of steel material standard samples.
(b) Scanning analysis of the sample:
and (3) grinding the surface of the sample by using sand paper or a grinding wheel, and performing two-dimensional scanning analysis on the steel material sample to be analyzed by using a Laser Induced Breakdown Spectroscopy (LIBS) instrument under a protective atmosphere environment to obtain the two-dimensional distribution of the signal intensity of S and Mn elements.
The morphology of the ablation spots after the scanning analysis of the steel material sample is shown in fig. 2.
The step (a) of establishing the calibration curve and the step (b) of scanning and analyzing the sample, the working parameter setting of the Laser Induced Breakdown Spectroscopy (LIBS) instrument should be identical.
Before analysis, the working parameters of a Laser Induced Breakdown Spectroscopy (LIBS) instrument are usually optimized to make the instrument in an optimal working state. Parameters such as pulse energy output by a Laser Induced Breakdown Spectroscopy (LIBS) instrument, the distance from a lens to the surface of a steel material sample to be analyzed, the type of gas, the gas pressure of the gas, signal delay acquisition time and the like have obvious influence on the analysis performance.
The pulse energy of the equipment used by the invention can be adjusted between 0 and 900mJ, and the optimal pulse energy is 300 mJ; the distance between the lens and the surface of the sample can be adjusted between 17mm and 28mm, and the optimal distance is 23 mm; the sample chamber is filled with high-purity argon with the purity of 99.999 percent, the air pressure can be adjusted between 1000Pa and 10000Pa, the optimal time delay of 4000Pa, the optimal time delay of S is 1 mu S, and the optimal time delay of Mn is 1.5 mu S.
(c) Measurement of ablation spots:
and (c) under a metallographic microscope or a scanning electron microscope, directly measuring or assisting with geometric calculation to obtain the size, the area and the scanning step length of the excitation area of the ablation spots after the steel material sample in the step (b) is scanned and analyzed, and determining the size of the grading field of view according to the scanning step length, namely determining the number of the ablation spots in the grading field of view.
The shape of the rating field is square as much as possible, and the size of the rating field is as close to 0.5mm specified in the metallographic examination standard as possible2Square standard field of view.
Typically, due to the large size of the ablation spot of Laser Induced Breakdown Spectroscopy (LIBS) instruments, a rating field size cannot be determined with as accurate a 0.5mm rating as in metallographic examination2The standard field of view. To improve the accuracy of the LIBS results, the rated field of view is typically determined to be slightly larger than the standard field of view, e.g., when the scan step size is 0.3mm, the LIBS rated field of view can be set to a square area covered by 3 × 3 ablation spots.
(d) And (4) analyzing results:
and (c) calculating the length or the area of the manganese sulfide inclusion in a rating view by using the calibration curve obtained in the step (a) and the ablation spot measurement result obtained in the step (c) and combining the two-dimensional distribution data of the signal intensity of the S and Mn elements obtained by scanning and analyzing in the step (b), then converting the length or the area of the manganese sulfide inclusion, and finally rating according to the converted length or the converted area of the manganese sulfide inclusion.
The relationship between the length or area of the manganese sulfide-based inclusions and the grade is described in the metallographic examination standards GB/T10561, ISO 4967, ASTM E45, DIN50602, EN10247 and the like.
In the step (d), the step (c),
when a manganese sulfide inclusion length-signal intensity relation curve or a manganese sulfide inclusion area-signal intensity relation curve is used as a calibration curve, the calibration curve is directly used for inversion to obtain the length or the area of the manganese sulfide inclusions in the excitation area. The specific inversion process is as follows:
firstly, a linear equation of a calibration curve is obtained by adopting a linear fitting mode, and then the signal intensity values of different analysis positions are substituted into the linear equation to calculate the length or the area of the manganese sulfide inclusions.
When S or Mn element concentration-signal intensity is used as a calibration curve, firstly, a linear equation of the calibration curve is obtained in a linear fitting mode, then, the two-dimensional distribution data of the S and Mn element signal intensity obtained by scanning and analyzing in the step (b) are substituted into the linear equation of the calibration curve to calculate the element concentration of different analysis positions, and then, the area of the manganese sulfide inclusion in the ablation excitation area of each analysis position is calculated according to the element concentration, wherein the calculation formula is as follows:
in the formula,
CSand CMnRespectively obtaining the concentrations of S and Mn, and calculating the concentrations of S and Mn by a linear equation obtained by substituting the signal intensities of the S and Mn elements obtained by scanning and analyzing in the step (b) into a calibration curve, wherein the concentrations are known quantities;
CS0and CMn0The solid solution concentrations of S and Mn, respectively, are known amounts;
Strepresenting the area of the ablation excitation area as a known quantity measured in step (c);
SMnSthe area of MnS inclusions in the ablation excitation area is shown.
FIG. 5 is a graph of Mn element concentration-inclusion area plotted by the above formula. The S element concentration-inclusion area graph can also be plotted, if desired.
If the length of the MnS inclusion needs to be calculated, the length can be obtained by dividing the area of the MnS inclusion by the average width of the MnS inclusion, and the average width of the MnS inclusion can be measured by using a metallographic microscope or a scanning electron microscope.
The area covered by the ablation spot within a single field of view due to LIBS analysis is not exactly equal to 0.5mm2After the length or area of the MnS inclusion is calculated by using the calibration curve, the length or area of the MnS inclusion is multiplied by a conversion coefficient k to be converted into 0.5mm2Total length or total area of MnS inclusion in the equivalent region, the conversion coefficient k is defined byAnd (3) calculating the formula:
in the formula,
ntrating the number of ablation spots in the field of view;
Sithe area of the excitation zone of a single ablation spot.
And (4) carrying out grade evaluation on the manganese sulfide inclusion according to the converted length or area of the manganese sulfide inclusion, wherein the evaluation principle and the relation between the length or area of the manganese sulfide inclusion and the grade are executed according to the regulations in the relevant metallographic examination standard.
Examples
The results of a comparison of 12 regions in a piece of free-cutting steel material, which were rated separately by the method according to the invention and by the M method in DIN50602, are shown in Table 1. Here, the relationship between the area of the inclusions of manganese sulfide type and the grade is A ═ 2nWherein A is the area of the manganese sulfide inclusion, and n is the number of grades. And in the evaluation process, if the area of the manganese sulfide inclusion is measured to be between n and n +1 grades, rounding downwards, and evaluating as n grades.
TABLE 1 comparison of the rating results of the inventive method and the metallographic method
The result obtained by the analysis method of the invention can be well matched with the existing standard method of the comparative example, and can be used for the rating test of the manganese sulfide inclusion.
Claims (6)
1. A method for analyzing and rating manganese sulfide inclusions in steel based on a calibration curve is characterized by comprising the following steps: the method comprises the following steps:
a. obtaining a calibration curve:
a metallographic microscope or a scanning electron microscope is used in combination with a laser-induced breakdown spectroscopy instrument, and a series of steel material standard samples are used to obtain an element concentration-signal intensity relation curve as a calibration curve;
b. scanning analysis of the sample:
grinding the surface of a sample to be analyzed, and performing two-dimensional scanning analysis on the steel material sample to be analyzed by using a laser-induced breakdown spectroscopy instrument under a protective atmosphere environment to obtain two-dimensional distribution of signal intensity of S and Mn elements;
c. measurement of ablation spots:
b, under a metallographic microscope or a scanning electron microscope, directly measuring or assisting with geometric calculation to obtain the size, the area and the scanning step length of the excitation area of the ablation spots after the steel material sample in the step b is scanned and analyzed, and determining the size of the rating field of view according to the scanning step length, namely determining the number of the ablation spots in the rating field of view;
d. and (4) analyzing results:
b, calculating the length or the area of the manganese sulfide inclusion in a rating field of view by using the calibration curve obtained in the step a and the ablation spot measurement result obtained in the step c and combining the two-dimensional distribution data of the signal intensity of the S and Mn elements obtained by scanning and analyzing in the step b, then converting the length or the area of the manganese sulfide inclusion, and finally rating according to the converted length or the converted area of the manganese sulfide inclusion;
in the step d, when the element concentration-signal intensity is used as a calibration curve, firstly, a linear equation of the calibration curve is obtained in a linear fitting mode, then, the two-dimensional distribution data of the element signal intensity obtained by scanning and analyzing in the step b is substituted into the linear equation of the calibration curve to calculate the element concentration of different analysis positions, and then, the area of the manganese sulfide inclusion in the ablation excitation area of each analysis position is calculated according to the element concentration, wherein the calculation formula is as follows:
in the formula,
CSand CMnThe concentrations of S and Mn are respectively calculated by a linear equation of the S and Mn element signal intensities obtained by scanning analysis in the step b and taken into a calibration curve, and the concentrations are known quantities;
CS0and CMn0The solid solution concentrations of S and Mn, respectively, are known amounts;
Strepresenting the area of the ablation excitation area as measured in step c for a given valueAn amount;
SMnSthe area of MnS inclusions in the ablation excitation area is shown.
2. The method for analyzing and grading manganese sulfide inclusions in steel according to claim 1, wherein the method comprises the following steps:
in the step a, when the element concentration-signal intensity relation curve is used as a calibration curve, signals of S or Mn elements are used independently, or signals of S and Mn elements are used simultaneously; selecting a series of standard samples of the steel materials which are similar to the steel material samples to be analyzed and have different S and/or Mn contents; and (3) statistically obtaining a relation curve of S and/or Mn element concentration-signal intensity by exciting a series of steel material standard samples.
3. The method for analyzing and grading manganese sulfide inclusions in steel according to claim 1, wherein the method comprises the following steps:
the working parameters of the laser-induced breakdown spectroscopy instrument are set as follows:
the pulse energy adjustment range is 0 mJ-900 mJ;
the distance from the lens to the surface of the sample is 17 mm-28 mm;
filling high-purity argon into the sample chamber, wherein the purity is 99.999 percent, and the air pressure is 1000-10000 Pa;
the delay time of the S element is 1 mu S;
the delay time of Mn element was 1.5. mu.s.
4. The method for analyzing and grading manganese sulfide inclusions in steel according to claim 3, wherein the method comprises the following steps:
the working parameters of the laser-induced breakdown spectroscopy instrument are set as follows:
the pulse energy of the laser-induced breakdown spectroscopy instrument is 300 mJ;
the distance from the lens to the surface of the sample is 23 mm;
introducing high-purity argon into the sample chamber, wherein the purity is 99.999 percent, and the air pressure is 4000 Pa;
the delay time of the S element is 1 mu S;
the delay time of Mn element was 1.5. mu.s.
5. The method for analyzing and grading manganese sulfide inclusions in steel according to claim 1, wherein the method comprises the following steps:
in the step c, the shape of the rating field is square, and the size of the rating field is 0.5 +/-0.1 mm specified in the metallographic examination standard2Square standard field of view.
6. The method for analyzing and grading manganese sulfide inclusions in steel according to claim 1, wherein the method comprises the following steps:
in step d, the area covered by the ablation spot in a single field of view analyzed by the laser-induced breakdown spectroscopy instrument is not strictly equal to 0.5mm2After the length or area of the MnS inclusion is calculated by using the calibration curve, the length or area of the MnS inclusion is multiplied by a conversion coefficient k to be converted into 0.5mm2The total length or total area of MnS inclusions in the equivalent area, and the conversion coefficient k is calculated by the following formula:
in the formula,
ntrating the number of ablation spots in the field of view;
Sithe area of the excitation zone of a single ablation spot.
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