CN106908436B - The analysis ranking method of manganese sulfide type impurity in steel based on calibration curve - Google Patents
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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
It is the invention belongs to the surface micro-region analysis technique field in materials science field, in particular to a kind of to be lured with laser
Breakdown spectrograph is led, the analysis ranking method of manganese sulfide type impurity in the steel based on calibration curve.
Background technique
Requirement of the modern industry to steel products processing performance is higher and higher, needs to utilize in steel containing a certain amount of sulphur
The sulfide of generation improves cutting ability, while in order to guarantee comprehensive mechanical property, and needs to control the content and shape of sulfide
State.It is many to can be used for manganese sulfide type impurity content and the instrument and method of distribution in analysis of material, in investigation of materials and industry
Mainly there are metallographic microscope, scanning electron microscope/energy disperse spectroscopy (SEM/EDS), electron probe (EPMA) using relatively more extensive in production
Deng foring the standard test methods such as GB/T 10561, ISO 4967, ASTM E45,50602 DIN, EN10247.Above-mentioned side
Method is disadvantageous in that steel material sample pre-treatments are very cumbersome, and analysis speed is slow, the region very little of observation, it is difficult to realize
The quick automatical analysis of large scale range.
Laser induced breakdown spectroscopy (LIBS) is a kind of Atomic Emission Spectral Analysis method that have developed rapidly for nearly 30 years, tool
Have the advantages that sample preparation is simple, analysis speed is fast, sample ablation amount is small, is easily achieved online, remote analysis, is led in metallurgy
Domain has broad application prospects.It is found during application laser induced breakdown spectroscopy research nonmetallic inclusionsin steel,
There are relatively good linear relationships between field trash length, area and signal strength and characteristic element, are based on above-mentioned rule
Characteristic is restrained, the invention proposes the analysis methods with laser induced breakdown spectroscopy measurement manganese sulfide type impurity content.
Summary of the invention
The object of the present invention is to provide a kind of using laser induced breakdown spectrograph based on vulcanizing in the steel of calibration curve
The analysis ranking method of manganese type impurity, for the content of manganese sulfide type impurity in steel material and the statistical of distribution
Analysis.
To achieve the goals above, the present invention provides the following technical scheme that
The present invention provides a kind of analysis ranking method of manganese sulfide type impurity in the steel based on calibration curve, this method
Include the following steps:
A. calibration curve is obtained:
Metallographic microscope or scanning electron microscope is used in combination by laser induced breakdown spectrograph device, obtains sulphur in steel material
Change manganese type impurity length-signal strength relation curve as calibration curve, or obtains manganese sulfide class in steel material and be mingled with
Object plane product-signal strength relation curve is as calibration curve；
Or concentration of element-signal strength relation curve is obtained as calibration by using serial steel material standard sample
Curve；
B. scanning analysis sample:
Sample surfaces are polished, under protective atmosphere environment, with laser induced breakdown spectrograph device to steel material to be analyzed
Expect that sample carries out two-dimensional scanning analysis, obtains the Two dimensional Distribution of S and Mn elemental signals intensity；
C. ablation spot is measured:
Step b steel material sample is calculated by directly measuring or being aided with geometry under metallographic microscope or scanning electron microscope
Lasing region size, area and the scanning step of ablation spot after product scanning analysis, and determine that grading visual field is big according to scanning step
It is small, that is, determine ablation amount of speckle in grading visual field；
D. interpretation of result:
Using the step a calibration curve obtained and step c the ablation spot measurement obtained as a result, in conjunction with step b scanning point
The Two dimensional Distribution data of obtained S and Mn elemental signals intensity are analysed, manganese sulfide type impurity length or face in grading visual field are calculated
Product, then, converts manganese sulfide type impurity length or area, finally, long according to the manganese sulfide type impurity after conversion
Degree or area are graded.
In the step a, using manganese sulfide type impurity length-signal strength relation curve or manganese sulfide type impurity face
When product-signal strength relation curve is as calibration curve, the signal of S or Mn element is used alone, or uses S and Mn two simultaneously
The signal of kind element；The material same or similar with steel material sample to be analyzed should be chosen, metallographic microscope or scanning are first used
Electronic Speculum obtains the distribution map of manganese sulfide type impurity on steel material sample survey face, is then scanned with laser induced breakdown spectroscopy
Steel material sample, the length of manganese sulfide type impurity or area are believed in the lasing region of ablation spot where extracting abnormal signal
Breath obtains manganese sulfide type impurity length or area and S and/or Mn in steel material by the statistics to these abnormal signals
Relation curve between elemental signals intensity.
In the step a, when using concentration of element-signal strength relation curve as calibration curve, S or Mn is used alone
The signal of element, or the signal of two kinds of elements of S and Mn is used simultaneously；It should select close with steel material sample to be analyzed and have
The serial steel material standard sample of different S and/or Mn contents；Pass through the excitation to serial steel material standard sample, statistics
Obtain S and/or Mn concentration of element-signal strength relation curve.
The running parameter of laser induced breakdown spectrograph device is provided that
Pulse energy adjusting range is 0mJ~900mJ；
Lens to sample surfaces distance is 17mm~28mm；
Sample room is filled with high-purity argon gas, purity 99.999%, and air pressure is 1000Pa~10000Pa；
The delay time of S element is 1 μ s；
The delay time of Mn element is 1.5 μ s.
Preferably, the running parameter of laser induced breakdown spectrograph device is provided that
Laser induced breakdown spectrograph device pulse energy is 300mJ；
Lens to sample surfaces distance is 23mm；
Sample room is filled with high-purity argon gas, purity 99.999%, air pressure 4000Pa；
The delay time of S element is 1 μ s；
The delay time of Mn element is 1.5 μ s.
In the step c, the shape of visual field of grading be it is rectangular, the size for visual field of grading is specified in metal lographic examination standard
0.5±0.1mm2Rectangular standard field of view.
In the step d, using manganese sulfide type impurity length-signal strength relation curve or manganese sulfide type impurity face
When product-signal strength relation curve is as calibration curve, directly it is mingled with using the manganese sulfide class that calibration curve obtains excitation area
Object length or area；Process is as follows:
The linear equation of calibration curve is obtained by the way of linear fit first, then by the signal of different analysis positions
Intensity value substitutes into linear equation and calculates manganese sulfide type impurity length or area.
In the step d, when using concentration of element-signal strength as calibration curve, the side of linear fit is used first
Formula obtains the linear equation of calibration curve, the Two dimensional Distribution data for the elemental signals intensity for then obtaining step b scanning analysis
The linear equation for bringing calibration curve into calculates the concentration of element of different analysis positions, calculates each analysis position further according to concentration of element
Ablation excitation area manganese sulfide type impurity area, calculation formula are as follows:
In formula,
CSAnd CMnThe concentration of respectively S and Mn, S the and Mn elemental signals intensity obtained by step b scanning analysis bring school into
The linear equation of directrix curve is calculated, and is known quantity；
CS0And CMn0The solid solution concentration of respectively S and Mn is known quantity；
StThe area of ablation excitation area is indicated, for the known quantity measured in step c；
SMnSIndicate the area of ablation lasing region MnS field trash.
In the step d, since ablation spot is covered in the single visual field of laser induced breakdown spectrograph device analysis
Area is not exactly equal to 0.5mm2, be calculated after MnS field trash length or area using calibration curve also need multiplied by
One conversion factor k, to be converted to 0.5mm2The total length or the gross area of MnS field trash in equivalent area, this conversion factor k
It is calculated and is obtained by following formula:
In formula,
ntFor ablation spot number in grading visual field；
SiFor the lasing region area of single ablation spot.
Compared with prior art, the beneficial effects of the present invention are:
1, the existing manganese sulfide type impurity method of inspection, such as GB/T 10561, ISO 4967, ASTM E45, DIN
50602, EN10247 etc. is on the metallographic specimen prepared with the vulcanization in microscope direct observing and measurement standard visual field
Manganese type impurity is graded according to manganese sulfide type impurity length or area.The invention belongs to a kind of indirect method, acquisition
It is the signal strength of manganese sulfide type impurity component, the length of manganese sulfide type impurity is obtained by using calibration curve inverting
Degree or area.
2, existing metallographic test method need to be by sample preparation at the very high mirror surface of finish, the requirement of surface cleanness
Very high, any surface adhesion all can generate interference to examining, and influence of the sample preparation to inspection result is bigger.Sample of the invention
The process of product preparation is fairly simple, and sample surfaces need to only be polished with sand paper or grinding wheel, and surface is allowed there are a small amount of pollutant,
Pollutant can be removed by the method for pre-ablation.
3, the sample that existing standard test method uses can be used in the present invention, samples and principle, the method for sample preparation are close,
The Comparative result analysis of several different detection methods can be conveniently realized.
4, compared with existing method, the present invention is the advantage of manganese sulfide type impurity content analysis in steel material
Sample pre-treatments are simple, analysis speed is fast, scan area range is big.
Detailed description of the invention
Fig. 1 is that the present invention is based on the flow charts of the analysis ranking method of manganese sulfide type impurity in the steel of calibration curve；
Fig. 2 is the ablation spot pattern after the analysis of steel material of embodiment of the present invention Sample Scan；
Fig. 3 is manganese sulfide inclusion of embodiment of the present invention object plane product-S elemental signals intensity calibration curve；
Fig. 4 is Mn of embodiment of the present invention concentration of element-signal strength calibrated curve；
Fig. 5 is manganese sulfide inclusion of embodiment of the present invention object plane product-Mn concentration of element calculated curve.
Specific embodiment
Invention is further explained with reference to the accompanying drawings and examples.
The present invention is the method for carrying out analysis grading to manganese sulfide type impurity in steel based on calibration curve, analysis grading
Process is as shown in Figure 1, include the following steps:
(a) calibration curve is obtained:
Metallographic microscope or scanning electron microscope is used in combination by laser induced breakdown spectroscopy (LIBS) instrument, obtains steel material
Manganese sulfide type impurity length-signal strength relation curve is as calibration curve in material, or obtains manganese sulfide in steel material
Type impurity area-signal strength relation curve is (as shown in Figure 3) to be used as calibration curve；
Or concentration of element-signal strength relation curve is obtained (such as Fig. 4 institute by using serial steel material standard sample
Show) as calibration curve.
Wherein,
Using manganese sulfide type impurity length-signal strength relation curve or manganese sulfide type impurity area-signal strength
When relation curve is as calibration curve, the signal of S or Mn element can be used alone, also can be used simultaneously two kinds of elements of S and Mn
Signal.The material same or similar with steel material sample to be analyzed should be chosen, is first obtained with metallographic microscope or scanning electron microscope
The distribution map of manganese sulfide type impurity on steel material sample survey face is taken, is then scanned with laser induced breakdown spectroscopy (LIBS)
Steel material sample, the length of manganese sulfide type impurity or area are believed in the lasing region of ablation spot where extracting abnormal signal
Breath obtains manganese sulfide type impurity length or area and S and/or Mn in steel material by the statistics to these abnormal signals
Relation curve between elemental signals intensity.
When using concentration of element-signal strength relation curve as calibration curve, the letter of S or Mn element can be used alone
Number, it also can be used simultaneously the signal of two kinds of elements of S and Mn.Should select it is close from steel material sample to be analyzed and have different S and/
Or the serial steel material standard sample of Mn content.By the excitation to serial steel material standard sample, statistics obtain S and/
Or Mn concentration of element-signal strength relation curve.
(b) scanning analysis sample:
Sample surfaces are polished with sand paper or grinding wheel, under protective atmosphere environment, with laser induced breakdown spectroscopy (LIBS)
Instrument carries out two-dimensional scanning analysis to steel material sample to be analyzed, obtains the Two dimensional Distribution of S and Mn elemental signals intensity.
Ablation spot pattern after the analysis of steel material Sample Scan, as shown in Figure 2.
The step (a) is established in calibration curve and step (b) scanning analysis sample, laser induced breakdown spectroscopy (LIBS)
The running parameter setting of instrument is answered identical.
Usually first laser induced breakdown spectroscopy (LIBS) Instrument working parameter is optimized before analysis, be in instrument
Optimum Working.The pulse energy of laser induced breakdown spectroscopy (LIBS) instrument output, lens to steel material sample to be analyzed
The parameters such as product surface distance, gaseous species and its air pressure, signal delay acquisition time have significant impact to analysis performance.
Device therefor pulse energy of the present invention can adjust between 0~900mJ, most preferably 300mJ；Lens to sample surfaces away from
From can be adjusted between 17~28mm, most preferably 23mm；Sample room is filled with high-purity argon gas, and purity 99.999%, air pressure can be 1000
It is adjusted between~10000Pa, most preferably 4000Pa, the optimum delay time that the optimum delay time of S is 1 μ s, Mn is 1.5 μ s.
(c) ablation spot is measured:
Step (b) steel material is calculated by directly measuring or being aided with geometry under metallographic microscope or scanning electron microscope
Lasing region size, area and the scanning step of ablation spot after Sample Scan analysis, and grading visual field is determined according to scanning step
Size determines ablation amount of speckle in grading visual field.
Grading visual field shape be as far as possible it is rectangular, the size for visual field of grading is as far as possible close to specified in metal lographic examination standard
0.5mm2Rectangular standard field of view.
Under normal conditions since the ablation spot size of laser induced breakdown spectroscopy (LIBS) instrument is larger, grade determining
0.5mm accurately delimited without such in the image of Buddha metal lographic examination when visual field size2Standard field of view.To improve the accurate of LIBS result
Degree, usually determining grading visual field should be slightly bigger than standard field of view, and such as when scanning step is 0.3mm, can grade LIBS visual field
It is arranged to the square region of 3 × 3 ablation spots covering.
(d) interpretation of result:
The ablation spot measurement that the calibration curve and step (c) obtained using step (a) is obtained is as a result, in conjunction with step (b)
It is long to calculate manganese sulfide type impurity in grading visual field for the Two dimensional Distribution data for the S and Mn elemental signals intensity that scanning analysis obtains
Then degree or area are converted manganese sulfide type impurity length or area, finally, being pressed from both sides according to the manganese sulfide class after conversion
Sundries length or area are graded.
Relationship between manganese sulfide type impurity length or area and rank referring to metal lographic examination standard GB/T 10561,
ISO 4967, ASTM E45,50602 DIN, EN10247 etc..
In the step (d),
Using manganese sulfide type impurity length-signal strength relation curve or manganese sulfide type impurity area-signal strength
When relation curve is as calibration curve, directly using calibration curve inverting obtain excitation area manganese sulfide type impurity length or
Area.Specific refutation process is as follows:
The linear equation of calibration curve is obtained by the way of linear fit first, then by the signal of different analysis positions
Intensity value substitutes into linear equation and calculates manganese sulfide type impurity length or area.
When using S or Mn concentration of element-signal strength as calibration curve, school is obtained by the way of linear fit first
The linear equation of directrix curve, the Two dimensional Distribution data band for the S and Mn elemental signals intensity for then obtaining step (b) scanning analysis
The linear equation for entering calibration curve calculates the concentration of element of different analysis positions, calculates each analysis position further according to concentration of element and burns
Excitation area manganese sulfide type impurity area is lost, calculation formula is as follows:
In formula,
CSAnd CMnThe concentration of respectively S and Mn, S the and Mn elemental signals intensity obtained by step (b) scanning analysis are brought into
The linear equation of calibration curve is calculated, and is known quantity；
CS0And CMn0The solid solution concentration of respectively S and Mn is known quantity；
StThe area of ablation excitation area is indicated, for the known quantity measured in step (c)；
SMnSIndicate the area of ablation lasing region MnS field trash.
Fig. 5 is the Mn concentration of element-inclusion area curve graph drawn with above-mentioned formula.If desired, can also be with
Draw S concentration of element-inclusion area curve graph.
If you need to calculate MnS field trash length, can be obtained with MnS inclusion area divided by MnS field trash mean breadth, MnS
Metallographic microscope or scanning electron microscope can be used to measure for field trash mean breadth.
Since the area that ablation spot is covered in the single visual field of LIBS analysis is not exactly equal to 0.5mm2, use school
Directrix curve also needs after MnS field trash length or area is calculated multiplied by a conversion factor k, to be converted to 0.5mm2Deng
The total length or the gross area of MnS field trash in region are imitated, this conversion factor k is calculated by following formula and obtained:
In formula,
ntFor ablation spot number in grading visual field；
SiFor the lasing region area of single ablation spot.
According to the manganese sulfide type impurity length or area progress manganese sulfide type impurity rank evaluation after conversion, manganese sulfide
Relationship and Assessment principle between type impurity length or area and rank are executed according to the regulation in related metal lographic examination standard.
Embodiment
Using the M method in the method for the invention and DIN50602 respectively to 12 regions in an automatic steel material
It grades respectively, comparing result is shown in Table 1.Here the relationship between manganese sulfide type impurity area and rank is A=2n, wherein
A is manganese sulfide type impurity area, and n is number of levels.If measuring manganese sulfide type impurity area during evaluation between n and n+1
Then downward rounding between grade, is chosen as n grades.
1 the method for the present invention of table and the comparison of the rating result of metallographic method
The result and the existing standard method of comparative example that analysis method of the invention obtains can be relatively good coincide, can use
It is examined in the grading of manganese sulfide type impurity.
Claims (6)
1. the analysis ranking method of manganese sulfide type impurity in a kind of steel based on calibration curve, it is characterised in that: this method
Include the following steps:
A. calibration curve is obtained:
Metallographic microscope or scanning electron microscope is used in combination by laser induced breakdown spectrograph device, by using serial steel material
Standard sample obtains concentration of element-signal strength relation curve as calibration curve；
B. scanning analysis sample:
Sample surfaces are polished, under protective atmosphere environment, with laser induced breakdown spectrograph device to steel material sample to be analyzed
Product carry out two-dimensional scanning analysis, obtain the Two dimensional Distribution of S and Mn elemental signals intensity；
C. ablation spot is measured:
It is swept under metallographic microscope or scanning electron microscope by directly measuring or being aided with geometry step b steel material sample is calculated
Lasing region size, area and the scanning step of ablation spot after analyzing are retouched, and grading visual field size is determined according to scanning step, i.e.,
Determine ablation amount of speckle in grading visual field；
D. interpretation of result:
The ablation spot measurement obtained using the step a calibration curve obtained and step c in conjunction with step b scanning analysis as a result, obtain
The Two dimensional Distribution data of the S and Mn elemental signals intensity arrived calculate manganese sulfide type impurity length or area in grading visual field, so
Afterwards, manganese sulfide type impurity length or area are converted, finally, according to after conversion manganese sulfide type impurity length or face
Product is graded；
In the step d, when using concentration of element-signal strength as calibration curve, obtained by the way of linear fit first
The linear equation of calibration curve is taken, then brings the Two dimensional Distribution data for the elemental signals intensity that step b scanning analysis obtains into
The linear equation of calibration curve calculates the concentration of element of different analysis positions, calculates each analysis position ablation further according to concentration of element
Excitation area manganese sulfide type impurity area, calculation formula are as follows:
In formula,
CSAnd CMnThe concentration of respectively S and Mn, it is bent that S the and Mn elemental signals intensity obtained by step b scanning analysis brings calibration into
The linear equation of line is calculated, and is known quantity；
CS0And CMn0The solid solution concentration of respectively S and Mn is known quantity；
StThe area of ablation excitation area is indicated, for the known quantity measured in step c；
SMnSIndicate the area of ablation lasing region MnS field trash.
2. the analysis ranking method of manganese sulfide type impurity in the steel according to claim 1 based on calibration curve,
It is characterized in that:
In the step a, when using concentration of element-signal strength relation curve as calibration curve, S or Mn element is used alone
Signal, or simultaneously use two kinds of elements of S and Mn signal；It should select close from steel material sample to be analyzed and have different
The serial steel material standard sample of S and/or Mn content；By the excitation to serial steel material standard sample, statistics obtains S
And/or Mn concentration of element-signal strength relation curve.
3. the analysis ranking method of manganese sulfide type impurity in the steel according to claim 1 based on calibration curve,
It is characterized in that:
The running parameter of laser induced breakdown spectrograph device is provided that
Pulse energy adjusting range is 0mJ~900mJ；
Lens to sample surfaces distance is 17mm~28mm；
Sample room is filled with high-purity argon gas, purity 99.999%, and air pressure is 1000Pa~10000Pa；
The delay time of S element is 1 μ s；
The delay time of Mn element is 1.5 μ s.
4. the analysis ranking method of manganese sulfide type impurity in the steel according to claim 3 based on calibration curve,
It is characterized in that:
The running parameter of laser induced breakdown spectrograph device is provided that
Laser induced breakdown spectrograph device pulse energy is 300mJ；
Lens to sample surfaces distance is 23mm；
Sample room is filled with high-purity argon gas, purity 99.999%, air pressure 4000Pa；
The delay time of S element is 1 μ s；
The delay time of Mn element is 1.5 μ s.
5. the analysis ranking method of manganese sulfide type impurity in the steel according to claim 1 based on calibration curve,
It is characterized in that:
In the step c, the shape of visual field of grading be it is rectangular, the size for visual field of grading is 0.5 specified in metal lographic examination standard
±0.1mm2Rectangular standard field of view.
6. the analysis ranking method of manganese sulfide type impurity in the steel according to claim 1 based on calibration curve,
It is characterized in that:
In the step d, by the area that ablation spot is covered in the single visual field of laser induced breakdown spectrograph device analysis
It is not exactly equal to 0.5mm2, it is calculated after MnS field trash length or area and is also needed multiplied by one using calibration curve
Conversion factor k, to be converted to 0.5mm2The total length or the gross area of MnS field trash in equivalent area, k is under for this conversion factor
Formula, which calculates, to be obtained:
In formula,
ntFor ablation spot number in grading visual field；
SiFor the lasing region area of single ablation spot.
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| CN109030462A (en) * | 2018-08-21 | 2018-12-18 | 钢研纳克检测技术股份有限公司 | Different type inclusion area and the quantitatively characterizing method of content in a kind of steel |
| DE102019106765B4 (en) * | 2019-03-18 | 2020-11-26 | Thyssenkrupp Ag | Method for the preparation and analysis of a sample of a metallic material |
| EP3726206B1 (en) * | 2019-03-26 | 2022-11-02 | FEI Company | Methods and systems for inclusion analysis |
| CN112285143B (en) * | 2020-11-17 | 2022-07-08 | 钢铁研究总院 | Method for evaluating inclusion of high-cleanliness gear steel |
| CN113447512B (en) * | 2021-03-16 | 2024-02-06 | 首钢集团有限公司 | Quantitative assessment method for hypoeutectoid steel strip-shaped structure |
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