CN106908436A - 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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Abstract
The invention belongs to the surface micro-region analysis technique field in material science, more particularly to one kind uses laser induced breakdown spectrograph, the analysis ranking method of manganese sulfide type impurity in the steel based on calibration curve.The method comprises the following steps：A () obtains calibration curve；(b) scanning analysis sample；C () measures ablation spot；(d) interpretation of result.What the present invention was gathered is the signal intensity 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, analyze speed is fast, scan area scope is big.
Description
Technical field
The invention belongs to the surface micro-region analysis technique field in material science, more particularly to one kind is lured with laser
Breakdown spectrograph is led, the analysis ranking method of manganese sulfide type impurity in the steel based on calibration curve.
Background technology
Requirement more and more higher of the modern industry to steel products processing characteristics is, it is necessary to containing a certain amount of sulphur in steel, utilize
The sulfide of generation improves cutting ability, while in order to ensure comprehensive mechanical property, need to control the content and shape of sulfide again
State.Can be used for manganese sulfide type impurity content and the instrument and method of distribution in analysis of material a lot, in investigation of materials and industry
Being applied in production relatively widely mainly has metallographic microscope, ESEM/energy disperse spectroscopy (SEM/EDS), electron probe (EPMA)
Deng foring the standard test methods such as GB/T 10561, ISO 4967, ASTM E45, DIN 50602, EN10247.Above-mentioned side
Method is disadvantageous in that ferrous materials sample pre-treatments are very cumbersome, and analyze speed is slow, the region very little of observation, it is difficult to realize
The quick automatical analysis of large scale scope.
LIBS (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, analyze speed is fast, sample ablation amount is small, be easily achieved online, remote analysis, led in metallurgy
Domain has broad application prospects.Found during application LIBS research nonmetallic inclusionsin steel,
Field trash length, there is relatively good linear relationship between area and signal intensity and characteristic element, based on above-mentioned rule
Rule characteristic, the present invention proposes the analysis method that manganese sulfide type impurity content is determined with LIBS.
The content of the invention
It is an object of the invention to provide vulcanization in the steel that a kind of use laser induced breakdown spectrograph is based on calibration curve
The analysis ranking method of manganese type impurity, for the content of manganese sulfide type impurity in ferrous materials and the statistical of distribution
Analysis.
To achieve these goals, the invention provides following technical scheme：
The present invention provides a kind of analysis ranking method of manganese sulfide type impurity in steel based on calibration curve, the method
Comprise the following steps：
A. calibration curve is obtained：
Metallographic microscope or ESEM are used in combination by laser induced breakdown spectrograph device, sulphur in ferrous materials is obtained
Change manganese type impurity length-signal intensity relation curve to be mingled with as manganese sulfide class in calibration curve, or acquisition ferrous materials
Object plane product-signal intensity relation curve is used as calibration curve；
Or concentration of element-signal intensity relation curve is obtained as calibration by using serial ferrous materials 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
Material sample carries out two-dimensional scan analysis, obtains the Two dimensional Distribution of S and Mn elemental signals intensity；
C. ablation spot is measured：
By direct measurement or it is aided with geometry and is calculated step b ferrous materials samples under metallographic microscope or ESEM
The lasing region size of ablation spot, area and scanning step 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：
The ablation spot measurement result that the calibration curve and step c obtained using step a are obtained, with reference to step b scannings point
The Two dimensional Distribution data of the S and Mn elemental signals intensity that analysis is obtained, calculate manganese sulfide type impurity length or face in grading visual field
Product, then, converts to 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 intensity relation curve or manganese sulfide type impurity face
When product-signal intensity relation curve is as calibration curve, the signal of S or Mn elements is used alone, or uses S and Mn two simultaneously
Plant the signal of element；The material same or like with ferrous materials sample to be analyzed should be chosen, first with metallographic microscope or scanning
Electronic Speculum obtains the distribution map of manganese sulfide type impurity on ferrous materials sample survey face, is then scanned with LIBS
Ferrous materials sample, extracts length or the area letter of manganese sulfide type impurity in the lasing region of ablation spot where abnormal signal
Breath, by the statistics to these abnormal signals, obtains manganese sulfide type impurity length or area and S and/or Mn in ferrous materials
Relation curve between elemental signals intensity.
In the step a, during using concentration of element-signal intensity relation curve as calibration curve, S or Mn is used alone
The signal of element, or two kinds of signals of element of S and Mn are used simultaneously；Should select close with ferrous materials sample to be analyzed and have
The serial ferrous materials standard sample of different S and/or Mn contents；Excited by serial ferrous materials standard sample, counted
Obtain the relation curve of S and/or Mn concentration of element-signal intensity.
The running parameter of laser induced breakdown spectrograph device sets as follows：
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 elements is 1 μ s；
The delay time of Mn elements is 1.5 μ s.
Preferably, the running parameter of laser induced breakdown spectrograph device sets as follows：
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, and purity 99.999%, air pressure is 4000Pa；
The delay time of S elements is 1 μ s；
The delay time of Mn elements is 1.5 μ s.
In the step c, being shaped as grading visual field is square, and the size of visual field of grading is specified in metal lographic examination standard
0.5±0.1mm2Square standard field of view.
In the step d, using manganese sulfide type impurity length-signal intensity relation curve or manganese sulfide type impurity face
When product-signal intensity relation curve is as calibration curve, the manganese sulfide class for directly obtaining excitation area using calibration curve is mingled with
Thing 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 level substitutes into linear equation and calculates manganese sulfide type impurity length or area.
In the step d, during using concentration of element-signal intensity as calibration curve, first using the side of linear fit
Formula obtains the linear equation of calibration curve, the Two dimensional Distribution data of 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, and each analysis position is calculated further according to concentration of element
Ablation excitation area manganese sulfide type impurity area, computing 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 brings 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 represented, is the known quantity measured in step c；
SMnSRepresent the area of ablation lasing region MnS field trashes.
In the step d, covered by ablation spot in the single visual field of laser induced breakdown spectrograph device analysis
Area is not exactly equal to 0.5mm2, it is calculated after MnS field trashes length or area using calibration curve and also needs to be multiplied by
One conversion factor k, to be converted to 0.5mm2The total length or the gross area of MnS field trashes in equivalent area, this conversion factor k
Calculated by following formula and obtained：
In formula,
ntIt is ablation spot number in grading visual field；
SiIt is the lasing region area of single ablation spot.
Compared with prior art, the beneficial effects of the present invention are：
1st, the existing manganese sulfide type impurity method of inspection, such as GB/T 10561, ISO 4967, ASTM E45, DIN
50602nd, EN10247 etc., is with the vulcanization in microscope direct observing and measurement standard visual field on the metallographic specimen for preparing
Manganese type impurity, is graded according to manganese sulfide type impurity length or area.The invention belongs to a kind of indirect method, collection
It is the signal intensity of manganese sulfide type impurity component, the length of manganese sulfide type impurity is obtained by using calibration curve inverting
Degree or area.
2nd, existing metallographic test method need to be by sample preparation into finish minute surface very high, the requirement of surface cleanness
Very high, any surface adhesion all can produce interference to inspection, and influence of the sample preparation to assay is than larger.Sample of the invention
Process prepared by product is fairly simple, and sample surfaces need to only be polished with sand paper or emery wheel, and surface allows there is a small amount of pollutant,
Pollutant can be removed by the method for pre-ablation.
The principle of the 3rd, sample that the present invention can be used using existing standard test method, sampling and sample preparation, method are close,
The Comparative result analysis of several different detection methods can be conveniently realized.
4 compare with existing method, and the present invention is to the advantage of manganese sulfide type impurity content analysis in ferrous materials
Sample pre-treatments are simple, analyze speed is fast, scan area scope is big.
Brief description of the drawings
Fig. 1 is the flow chart of the analysis ranking method of manganese sulfide type impurity in steel of the present invention based on calibration curve；
Fig. 2 is the ablation spot pattern after the analysis of embodiment of the present invention ferrous materials Sample Scan；
Fig. 3 is that embodiment of the present invention manganese sulfide inclusion object plane accumulates-S elemental signals intensity calibration curves；
Fig. 4 is embodiment of the present invention Mn concentration of element-signal strength calibrated curve；
Fig. 5 is that embodiment of the present invention manganese sulfide inclusion object plane accumulates-Mn concentration of element calculated curves.
Specific embodiment
The present invention is further described with reference to the accompanying drawings and examples.
The present invention is the method for being analyzed grading to manganese sulfide type impurity in steel based on calibration curve, analysis grading
Flow is as shown in figure 1, comprise the following steps：
A () obtains calibration curve：
Metallographic microscope or ESEM are used in combination by LIBS (LIBS) instrument, steel material is obtained
Manganese sulfide type impurity length-signal intensity relation curve is used as calibration curve in material, or obtains manganese sulfide in ferrous materials
Type impurity area-signal intensity relation curve (as shown in Figure 3) is used as calibration curve；
Or concentration of element-signal intensity relation curve is obtained (such as Fig. 4 institutes by using serial ferrous materials standard sample
Show) as calibration curve.
Wherein,
Using manganese sulfide type impurity length-signal intensity relation curve or manganese sulfide type impurity area-signal intensity
When relation curve is as calibration curve, the signal of S or Mn elements is can be used alone, also can simultaneously use two kinds of elements of S and Mn
Signal.The material same or like with ferrous materials sample to be analyzed should be chosen, is first obtained with metallographic microscope or ESEM
The distribution map of manganese sulfide type impurity on ferrous materials sample survey face is taken, is then scanned with LIBS (LIBS)
Ferrous materials sample, extracts length or the area letter of manganese sulfide type impurity in the lasing region of ablation spot where abnormal signal
Breath, by the statistics to these abnormal signals, obtains manganese sulfide type impurity length or area and S and/or Mn in ferrous materials
Relation curve between elemental signals intensity.
During using concentration of element-signal intensity relation curve as calibration curve, the letter of S or Mn elements is can be used alone
Number, also can simultaneously use two kinds of signals of element of S and Mn.Should select it is close from ferrous materials sample to be analyzed and with different S and/
Or the serial ferrous materials standard sample of Mn contents.Excited by serial ferrous materials standard sample, statistics obtain S and/
Or the relation curve of Mn concentration of element-signal intensity.
(b) scanning analysis sample：
Sample surfaces are polished with sand paper or emery wheel, under protective atmosphere environment, with LIBS (LIBS)
Instrument carries out two-dimensional scan analysis to ferrous materials sample to be analyzed, obtains the Two dimensional Distribution of S and Mn elemental signals intensity.
Ablation spot pattern after the analysis of ferrous materials Sample Scan, as shown in Figure 2.
The step (a) is set up in calibration curve and step (b) scanning analysis sample, LIBS (LIBS)
The running parameter of instrument is set should be identical.
Generally first LIBS (LIBS) Instrument working parameter is optimized before analysis, be in instrument
Optimum Working.Pulse energy, the lens to ferrous materials sample to be analyzed of LIBS (LIBS) instrument output
The parameter such as product surface distance, gaseous species and its air pressure, signal lag acquisition time has significant impact to analytical performance.
Device therefor pulse energy of the present invention can be adjusted 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
Adjusted between~10000Pa, optimum delay time of most preferably 4000Pa, S is 1.5 μ s for the optimum delay time of 1 μ s, Mn.
C () measures ablation spot：
By direct measurement or it is aided with geometry and is calculated step (b) ferrous materials under metallographic microscope or ESEM
The lasing region size of ablation spot, area and scanning step after Sample Scan analysis, and grading visual field is determined according to scanning step
Size, that is, determine ablation amount of speckle in grading visual field.
The shape of visual field of grading is tried one's best as square, and the size of visual field of grading is tried one's best close to specified in metal lographic examination standard
0.5mm2Square standard field of view.
Under normal circumstances because the ablation spot size of LIBS (LIBS) instrument is larger, it is determined that grading
Without accurately delimiting 0.5mm like that in the image of Buddha metal lographic examination during size of visual field2Standard field of view.To improve the accurate of LIBS results
Degree, the grading visual field for generally determining should be slightly bigger than standard field of view, such as when scanning step is for 0.3mm, LIBS can grade visual field
It is arranged to 3 × 3 square regions of ablation spot covering.
(d) interpretation of result：
The ablation spot measurement result that the calibration curve and step (c) obtained using step (a) are obtained, with reference to step (b)
The Two dimensional Distribution data of the S and Mn elemental signals intensity that scanning analysis are obtained, calculate manganese sulfide type impurity in grading visual field long
Degree or area, then, convert to manganese sulfide type impurity length or area, finally, according to the manganese sulfide class folder after conversion
Debris length or area are graded.
Relation between manganese sulfide type impurity length or area and rank referring to metal lographic examination standard GB/T 10561,
ISO 4967, ASTM E45, DIN 50602, EN10247 etc..
In the step (d),
Using manganese sulfide type impurity length-signal intensity relation curve or manganese sulfide type impurity area-signal intensity
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 level substitutes into linear equation and calculates manganese sulfide type impurity length or area.
During using S or Mn concentration of element-signal intensity 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 of 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, and calculating each analysis position further according to concentration of element burns
Erosion excitation area manganese sulfide type impurity area, computing 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 is 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 represented, is the known quantity measured in step (c)；
SMnSRepresent the area of ablation lasing region MnS field trashes.
Fig. 5 is the Mn concentration of element-inclusion area curve map drawn with above-mentioned formula.If desired, it is also possible to
Draw S concentration of element-inclusion area curve map.
Such as need to calculate MnS field trash length, can be obtained divided by MnS field trashes mean breadth with MnS inclusion areas, MnS
Field trash mean breadth can be used metallographic microscope or ESEM to measure.
By the area that ablation spot in the single visual field of LIBS analyses is covered is not exactly equal to 0.5mm2, use school
Directrix curve also needs to be multiplied by a conversion factor k after being calculated MnS field trashes length or area, to be converted to 0.5mm2Deng
The total length or the gross area of MnS field trashes in effect region, this conversion factor k are calculated by following formula and obtained：
In formula,
ntIt is ablation spot number in grading visual field；
SiIt is the lasing region area of single ablation spot.
The evaluation of manganese sulfide type impurity rank, manganese sulfide are carried out according to the manganese sulfide type impurity length or area after conversion
Relation and Assessment principle between type impurity length or area and rank are performed according to the regulation in related metal lographic examination standard.
Embodiment
Using the M methods in the method for the invention and DIN50602 respectively to 12 regions in an automatic steel material
Graded respectively, comparing result is shown in Table 1.Here the relation 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 level, is chosen as n grades.
The rating result contrast of the inventive method of table 1 and metallographic method
The result that analysis method of the invention is obtained can be relatively good with the existing standard method of comparative example coincide, can use
Checked in the grading of manganese sulfide type impurity.
Claims (9)
1. in a kind of steel based on calibration curve manganese sulfide type impurity analysis ranking method, it is characterised in that：The method
Comprise the following steps：
A. calibration curve is obtained：
Metallographic microscope or ESEM are used in combination by laser induced breakdown spectrograph device, manganese sulfide in ferrous materials is obtained
Type impurity length-signal intensity relation curve is used as calibration curve, or obtains manganese sulfide type impurity face in ferrous materials
Product-signal intensity relation curve is used as calibration curve；
Or concentration of element-signal intensity relation curve is obtained as calibration song by using serial ferrous materials standard sample
Line；
B. scanning analysis sample：
Sample surfaces are polished, under protective atmosphere environment, with laser induced breakdown spectrograph device to ferrous materials sample to be analyzed
Product carry out two-dimensional scan analysis, obtain the Two dimensional Distribution of S and Mn elemental signals intensity；
C. ablation spot is measured：
By direct measurement or it is aided with geometry and is calculated step b ferrous materials samples and sweep under metallographic microscope or ESEM
The lasing region size of ablation spot, area and scanning step after analyzing are retouched, and grading visual field size is determined according to scanning step, i.e.,
It is determined that ablation amount of speckle in grading visual field；
D. interpretation of result：
The ablation spot measurement result that the calibration curve and step c obtained using step a are obtained, obtains with reference to step b scanning analysis
The Two dimensional Distribution data of the S and Mn elemental signals intensity for arriving, 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 the manganese sulfide type impurity length after conversion or face
Product is graded.
2. in the steel based on calibration curve according to claim 1 manganese sulfide type impurity analysis ranking method, its
It is characterised by：
In the step a, using manganese sulfide type impurity length-signal intensity relation curve or manganese sulfide type impurity area-
When signal intensity relation curve is as calibration curve, the signal of S or Mn elements is used alone, or uses S and two kinds of Mn simultaneously
The signal of element；The material same or like with ferrous materials sample to be analyzed should be chosen, first with metallographic microscope or scanning electricity
Mirror obtains the distribution map of manganese sulfide type impurity on ferrous materials sample survey face, then scans steel with LIBS
Iron material sample, extracts the length or area information of manganese sulfide type impurity in the lasing region of ablation spot where abnormal signal,
By the statistics to these abnormal signals, manganese sulfide type impurity length or area and S and/or Mn elements in ferrous materials are obtained
Relation curve between signal intensity.
3. in the steel based on calibration curve according to claim 1 manganese sulfide type impurity analysis ranking method, its
It is characterised by：
In the step a, during using concentration of element-signal intensity relation curve as calibration curve, S or Mn elements are used alone
Signal, or simultaneously use two kinds of signals of element of S and Mn；Should select close with ferrous materials sample to be analyzed and with difference
The serial ferrous materials standard sample of S and/or Mn contents；Excited by serial ferrous materials standard sample, statistics obtains S
And/or the relation curve of Mn concentration of element-signal intensity.
4. in the steel based on calibration curve according to claim 1 manganese sulfide type impurity analysis ranking method, its
It is characterised by：
The running parameter of laser induced breakdown spectrograph device sets as follows：
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 elements is 1 μ s；
The delay time of Mn elements is 1.5 μ s.
5. in the steel based on calibration curve according to claim 4 manganese sulfide type impurity analysis ranking method, its
It is characterised by：
The running parameter of laser induced breakdown spectrograph device sets as follows：
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, and purity 99.999%, air pressure is 4000Pa；
The delay time of S elements is 1 μ s；
The delay time of Mn elements is 1.5 μ s.
6. in the steel based on calibration curve according to claim 1 manganese sulfide type impurity analysis ranking method, its
It is characterised by：
In the step c, being shaped as grading visual field is square, and the size of visual field of grading is 0.5 specified in metal lographic examination standard
±0.1mm2Square standard field of view.
7. in the steel based on calibration curve according to claim 1 manganese sulfide type impurity analysis ranking method, its
It is characterised by：
In the step d, using manganese sulfide type impurity length-signal intensity relation curve or manganese sulfide type impurity area-
When signal intensity relation curve is as calibration curve, the manganese sulfide type impurity for directly obtaining excitation area using calibration curve is long
Degree 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 intensity of different analysis positions
Value substitutes into linear equation and calculates manganese sulfide type impurity length or area.
8. in the steel based on calibration curve according to claim 1 manganese sulfide type impurity analysis ranking method, its
It is characterised by：
In the step d, during using concentration of element-signal intensity as calibration curve, obtained by the way of linear fit first
The linear equation of calibration curve is taken, the Two dimensional Distribution data of the elemental signals intensity for then obtaining step b scanning analysis are brought into
The linear equation of calibration curve calculates the concentration of element of different analysis positions, and each analysis position ablation is calculated further according to concentration of element
Excitation area manganese sulfide type impurity area, computing formula is 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 represented, is the known quantity measured in step c；
SMnSRepresent the area of ablation lasing region MnS field trashes.
9. in the steel based on calibration curve according to claim 1 manganese sulfide type impurity analysis ranking method, its
It is characterised by：
In the step d, by the area that ablation spot in the single visual field of laser induced breakdown spectrograph device analysis is covered
It is not exactly equal to 0.5mm2, it is calculated after MnS field trashes length or area using calibration curve and also needs to be multiplied by one
Conversion factor k, to be converted to 0.5mm2The total length or the gross area of MnS field trashes in equivalent area, k is under for this conversion factor
Formula is calculated and obtained：
In formula,
ntIt is ablation spot number in grading visual field；
SiIt is the lasing region area of single ablation spot.
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| CN113447512A (en) * | 2021-03-16 | 2021-09-28 | 首钢集团有限公司 | Quantitative evaluation method for hypoeutectoid steel strip-shaped structure |
| 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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