CN103439301A - Spot quick analysis method of pearlite nodularization grade of number-20 steel - Google Patents

Spot quick analysis method of pearlite nodularization grade of number-20 steel Download PDF

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CN103439301A
CN103439301A CN201310338134XA CN201310338134A CN103439301A CN 103439301 A CN103439301 A CN 103439301A CN 201310338134X A CN201310338134X A CN 201310338134XA CN 201310338134 A CN201310338134 A CN 201310338134A CN 103439301 A CN103439301 A CN 103439301A
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steel
matrix
analysis
pipeline
pearlite
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CN103439301B (en
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戴沅
陆继东
林介东
姚顺春
李文胜
李军
王敏
董璇
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South China University of Technology SCUT
Electric Power Research Institute of Guangdong Power Grid Co Ltd
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South China University of Technology SCUT
Electric Power Research Institute of Guangdong Power Grid Co Ltd
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Abstract

The invention discloses a spot quick analysis method of a pearlite nodularization grade of number-20 steel. The method overcomes the defects of destructiveness of traditional pipe cutting or complex film metallographic analysis and the like, a tedious working procedure and high requirements on a knowledge level and the experience of an operator. The method comprises the steps that the surface of a power station boiler heating surface pipeline is not required to be mechanically cleaned, ground or polished before analysis; a pulse laser is used for directly acting on the surface of the pipeline; plasma spectrum data is collected; characteristic spectrum data characterizing a pipeline matrix is extracted; a spectrum database comprising samples with different pearlite nodularization grades is utilized; a category is distinguished by combining a principal component analysis method; and the nodularization grade of the detected number-20 steel pipeline is obtained. According to the method, the whole data analysis process is automatically accomplished by a computer program; the total detection time is less than 2min; and the method has the advantages that the method is close to nondestructiveness, is simple in detection procedure and high in checking efficiency, and has low requirements on the specialized knowledge level and the experience of the operator.

Description

A kind of on-the-spot rapid analysis of No. 20 steel pearlite nodulizing grades
Technical field
The present invention relates to a kind of analytical approach of pearlitic spheroidization grade, particularly the on-the-spot rapid analysis of a kind of pearlitic spheroidization grade of No. 20 steel.
Background technology
No. 20 steel are a kind of Fine Steel Casting irons, as the main of station boiler vitals, with material, for wall temperature, are no more than heating surface tubes in boilers jet chimney and the header of 450 ℃.Under high-temperature and high-pressure conditions, in long-term use procedure, nodularization can occur in the pearlite in its tissue, and the cementite in pearlite (carbonide) form is transformed into spherically gradually by initial lamellar, causes also decline thereupon of mechanical property.Therefore the pearlitic spheroidization degree in No. 20 structure of steel often is widely used as one of evaluation criterion of its dependability for a long time.According to People's Republic of China's power industry standard--" DL/T674-1999, No. 20 steel pearlitic spheroidization grading standards for thermal power plant ", it is 5 grades that No. 20 steel are divided into to complete nodularization from virgin state, be respectively 1 grade (not nodularization, former primary state), 2 grades (tendentiousness nodularization), 3 grades (slight nodularizations), 4 grades (moderate nodularization) and 5 grades (nodularization fully).
Traditional pearlitic spheroidization analytical sample preparation is divided into sampling metallographic specimen in kind and on-the-spot multiple film metallographic specimen.The former need to carry out pipe cutting and prepare sample on pipeline, and roughly grinds successively and then refine or grind with the metallographic refiner with 01,02 and No. 03 abrasive paper for metallograph with 180,320,400,500 and No. 600 waterproof abrasive papers after emery wheel is smooth.Carry out again the first etch of 5-10s with 3%～5% nital, then adopt mechanical polishing method remove to grind cut and distortion layer, finally adopt 3%-5% nital etch 10s left and right and clean after drying up and organize demonstration.Multiple film metallographic directly adopts mechanical means to remove surface oxide layer and the decarburized layer of tested heating surface piping fully, then with milling tools, ground, and employing and the same grinding order of sampling in kind, follow according to actual conditions and field condition and select mechanical buffing chemical polishing or electropolishing to carry out polishing and etch to pipe surface.Finally adopting thickness is that 80 μ m-100 μ m cellulose acetates (AC paper) or other similar material are as multiple diaphragm, to answer between diaphragm and metallographic flour milling and fill with acetone class organic solvent, and to multiple diaphragm a little pressure make between multiple diaphragm and metal surface without the laminating of bubble gapless closely and obtain multiple membrane sample, carefully taking off that multiple membrane sample is fixed on glass plate or cardboard after dry on self-check face is observable.First method need to be carried out destructive pipe cutting to tested heating surface piping, complex procedures, length consuming time.Although second method without carrying out destructive pipe cutting, detects also more complicated of operation, and two kinds of methods are all higher to operator's professional standing and experience requirement.
Summary of the invention
Technical matters to be solved by this invention, just be to provide a kind of on-the-spot rapid analysis of No. 20 steel pearlite nodulizing grades, the method is utilized portable laser spectrum quick analysis system, utilize pulse laser to directly act on pipe surface, gather the plasma spectrometry data that characterize the heating surface piping matrix, according to set up pearlitic spheroidization grade sample spectral data storehouse, carry out class discrimination by principal component analytical method, obtain the pearlitic spheroidization grade of tested heating surface piping.The present invention both need not carry out destructive pipe cutting to tested heating surface piping, and the operation simple and fast, and required not high to operator's professional standing and experience.
Solve the problems of the technologies described above, the technical solution used in the present invention is:
A kind of on-the-spot rapid analysis of No. 20 steel pearlite nodulizing grades, is characterized in that comprising the steps:
The first step: No. 20 steel samples of the 1-5 level pearlitic spheroidization of selection standard at first, utilize the laser spectral analysis system to obtain respectively the plasma spectrometry of different pearlitic spheroidization samples; The sample of each nodulizing grade obtains n group spectroscopic data, and every group of spectroscopic data comprises m pixel intensity, and 1-5 level nodularization sample obtains 5n group spectroscopic data altogether, is expressed as the spectroscopic data matrix of 5n * m dimension, that is:
X = x 11 x 12 . . . x 1 m x 21 x 22 . . . x 2 m . . . . . . . . . . . . x 5 n 1 x 5 n 2 . . . x 5 nm = [ x 1 x 2 . . . x m ] - - - ( 1 )
Wherein, x i=[x 1i, x 2i..., x 5ni] tbe i pixel intensive variable;
Second step: utilize the plasma spectrometry data of the 1-5 level pearlitic spheroidization sample obtained in the first step, by principal component analysis (PCA), set up the spectra database that different nodulizing grades are sorted out.By principal component analysis (PCA), by linear transformation, obtain fully reflecting raw information and separate new variables, to retain the main information in X.
If [u i1u i2... u in] be the coefficient vector of linear combination, can obtain by y thus ithe new vector formed:
y i = u i 1 x 1 + u i 2 x 2 + . . . + u im x m = [ x 1 x 2 . . . x m ] u i 1 u i 2 . . . u i 5 n = Xu i - - - ( 2 )
Y in formula ibe i major component, u ifor calculating i the coefficient vector that major component is required.
Therefore, the matrix that all major components form can be expressed as:
Y=XU （3）
The original spectrum data matrix that in formula, X is a kind of acquisition of step, U is matrix of coefficients corresponding to each major component, Y is the major component matrix.
The original spectrum data message amount maximum known according to the definition of major component, that first principal component is expressed, Second principal component, takes second place, and the accumulation contribution rate of general the first two major component can reach 85%.Therefore, retain the first and second major components, set up the spectra database that 1-5 level pearlitic spheroidization is sorted out;
The 3rd step: for detected boiler heating surface pipeline, utilize the pulse laser in portable laser spectrum quick analysis system to impact continuously pipe surface, characteristic spectral line by No. 20 steel in the plasma spectrometry detected and oxide layer component changes simultaneously, judge whether laser has passed surface oxide layer and decarburized layer, and be applied to the pipeline matrix.
The 4th step: in step 3, laser impacts continuously until be applied to the pipeline matrix, start to obtain the plasma spectrometry data that characterize tested heating surface piping matrix, and principal component analysis (PCA) is carried out in its substitution formula (1)-(3), obtain its first and second major component, and and step 1 in the spectra database set up the classification of 1-5 level pearlitic spheroidization contrasted, thereby judge the pearlitic spheroidization grade of tested heating surface piping.
The present invention has following advantage:
The present invention, by the combination of laser spectral analysis and principal component analytical method, obtains the pearlitic spheroidization grade of tested No. 20 steel heating surface pipings at the scene fast, and main advantage applies exists: 1) approximate harmless to heating surface piping; 2) operational sequence is simple, can realize field quick detection; 3) full-automatic data are processed, and analysis efficiency is high; 4) to operating personnel's professional standing and experience, require low.
The accompanying drawing explanation
Fig. 1 is pearlitic spheroidization grade express-analysis process flow diagram of the present invention;
Fig. 2 is 260～290nm spectroscopic data exemplary plot of the present invention
Fig. 3 is 400～440nm spectroscopic data exemplary plot of the present invention;
Fig. 4 is that the spectrum of 1-5 level pearlitic spheroidization of the present invention is sorted out the database schematic diagram;
Fig. 5 is that Ca spectral line of the present invention excites the variation tendency of number of times with pulse laser;
Fig. 6 is that Fe spectral line of the present invention excites the variation tendency of number of times with pulse laser.
Embodiment
Known in conjunction with the process flow diagram shown in Fig. 1, the on-the-spot rapid analysis of a kind of No. 20 steel pearlite nodulizing grades that the present invention proposes has comprised following steps:
1) No. 20 steel samples of the 1-5 level pearlitic spheroidization of selection standard at first, utilize the laser spectral analysis system to obtain respectively the plasma spectrometry of different pearlitic spheroidization samples.The sample of each nodulizing grade obtains 10 groups of spectroscopic datas as shown in Figures 2 and 3, and every group of spectroscopic data comprises 2034 pixel intensity, and 1-5 level nodularization sample obtains the spectroscopic data matrix of 50 * 2034 dimensions altogether.
2) again 50 * 2034 spectroscopic data matrixes of tieing up are carried out to principal component analysis (PCA), can be set up by the first and second major components the spectrum classification database of the 1-5 level pearlitic spheroidization shown in Fig. 4.
3) utilize at the scene the pulse laser in portable laser spectrum quick analytic instrument to impact continuously pipe surface, simultaneously by the Fe in the plasma spectrometry detected and Ca characteristic spectral line, variation tendency according to the characteristic spectral line spectral intensity shown in Fig. 5 and Fig. 6, when Ca line strength is tending towards 0, and Fe line strength is while tending towards stability, can judge that laser has passed surface oxide layer and decarburized layer, and be applied to the pipeline matrix, start to gather the plasma spectrometry data that characterize tested heating surface piping matrix.
4) in step 3), 5 different parts on tested heating surface piping surface gather respectively 1 group of plasma spectrometry data, these 5 groups of spectroscopic datas are carried out to substitution step 2 after principal component analysis (PCA)) in the spectrum set up sort out database, distribute (as shown in Figure 4) according to the classification of tested heating surface piping spectroscopic data, can judge that tested heating surface piping is 5 grades of pearlitic spheroidizations.

Claims (5)

1. the on-the-spot rapid analysis of No. 20 steel pearlite nodulizing grades, is characterized in that comprising the steps:
The first step: No. 20 steel samples of the 1-5 level pearlitic spheroidization of selection standard at first, utilize the laser spectral analysis system to obtain respectively the plasma spectrometry of different pearlitic spheroidization samples; The sample of each nodulizing grade obtains n group spectroscopic data, and every group of spectroscopic data comprises m pixel intensity, and 1-5 level nodularization sample obtains 5n group spectroscopic data altogether, is expressed as the spectroscopic data matrix of 5n * m dimension, that is:
X = x 11 x 12 . . . x 1 m x 21 x 22 . . . x 2 m . . . . . . . . . . . . x 5 n 1 x 5 n 2 . . . x 5 nm = [ x 1 x 2 . . . x m ] - - - ( 1 )
Wherein, x i=[x 1i, x 2i..., x 5ni] tbe i pixel intensive variable;
Second step: utilize the plasma spectrometry data of the 1-5 level pearlitic spheroidization sample obtained in the first step, by principal component analysis (PCA), set up the spectra database that different nodulizing grades are sorted out; By principal component analysis (PCA), obtain fully reflecting raw information and separate new variables by linear transformation, to retain the main information in X;
If [u i1u i2... u in] be the coefficient vector of linear combination, can obtain by y thus ithe new vector formed:
y i = u i 1 x 1 + u i 2 x 2 + . . . + u im x m = [ x 1 x 2 . . . x m ] u i 1 u i 2 . . . u i 5 n = Xu i - - - ( 2 ) ;
Y in formula ibe i major component, u ifor calculating i the coefficient vector that major component is required;
Therefore, the matrix that all major components form can be expressed as:
Y=XU （3）；
The original spectrum data matrix that in formula, X is a kind of acquisition of step, U is matrix of coefficients corresponding to each major component, Y is the major component matrix;
The original spectrum data message amount maximum known according to the definition of major component, that first principal component is expressed, Second principal component, takes second place, the accumulation contribution rate to 85% of the first two major component; Therefore, retain the first and second major components, set up the spectra database that 1-5 level pearlitic spheroidization is sorted out;
The 3rd step: for detected boiler heating surface pipeline, utilize the pulse laser in portable laser spectrum quick analysis system to impact continuously pipe surface, characteristic spectral line by No. 20 steel in the plasma spectrometry detected and oxide layer component changes simultaneously, judges whether laser has passed surface oxide layer and decarburized layer and be applied to the pipeline matrix;
The 4th step: confirm that in step 3, laser impacts continuously until be applied to the pipeline matrix, start to obtain the plasma spectrometry data that characterize tested heating surface piping matrix, and principal component analysis (PCA) is carried out in its substitution formula (1)-(3), obtain its first and second major component, and and step 1 in the spectra database set up the classification of 1-5 level pearlitic spheroidization contrasted, thereby judge the pearlitic spheroidization grade of tested heating surface piping.
2. the on-the-spot rapid analysis of No. 20 steel pearlite nodulizing grades according to claim 1, is characterized in that: the characteristic spectral line that has comprised No. 20 steel component Fe, C, Si, Mn, Cr, Ni and Cu in the spectroscopic data obtained in the described first step.
3. the on-the-spot rapid analysis of No. 20 steel pearlite nodulizing grades according to claim 1, is characterized in that: more than the accumulation contribution rate to 85% of the first and second major components that retain in described second step reaches.
4. the on-the-spot rapid analysis of No. 20 steel pearlite nodulizing grades according to claim 1, it is characterized in that: describedly judge whether laser has passed surface oxide layer and decarburized layer and the method that has been applied to the pipeline matrix is: by the Fe in the plasma spectrometry detected and Ca characteristic spectral line, when Ca line strength goes to zero and Fe line strength while tending towards stability, judgement laser has passed surface oxide layer and decarburized layer and has been applied to the pipeline matrix; Otherwise quite different.
5. the on-the-spot rapid analysis of No. 20 steel pearlite nodulizing grades according to claim 1 is characterized in that: describedly judge whether laser has passed surface oxide layer and decarburized layer and be applied to pipeline matrix steel used and the oxide layer component also has C, Si, Mn, Cr, Ni, Cu and Mg.
CN201310338134.XA 2013-08-05 2013-08-05 A kind of on-the-spot rapid analysis of No. 20 steel ball body of light nodulizing grades Active CN103439301B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103969103A (en) * 2014-04-25 2014-08-06 国家电网公司 Rating method for pearlitic steel microstructure subject to hydrogen damage
CN104390980A (en) * 2014-12-09 2015-03-04 中国石油天然气股份有限公司 Method and device for monitoring structure degradation degree of furnace tube of HP type hydrogen production furnace
CN111380859A (en) * 2018-12-27 2020-07-07 上汽通用汽车有限公司 Sample preparation verification method and sample preparation method

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103969103A (en) * 2014-04-25 2014-08-06 国家电网公司 Rating method for pearlitic steel microstructure subject to hydrogen damage
CN104390980A (en) * 2014-12-09 2015-03-04 中国石油天然气股份有限公司 Method and device for monitoring structure degradation degree of furnace tube of HP type hydrogen production furnace
CN111380859A (en) * 2018-12-27 2020-07-07 上汽通用汽车有限公司 Sample preparation verification method and sample preparation method

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