CN111624194B - Blade element nondestructive measurement method based on laser-induced breakdown spectroscopy - Google Patents

Blade element nondestructive measurement method based on laser-induced breakdown spectroscopy Download PDF

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CN111624194B
CN111624194B CN202010505598.5A CN202010505598A CN111624194B CN 111624194 B CN111624194 B CN 111624194B CN 202010505598 A CN202010505598 A CN 202010505598A CN 111624194 B CN111624194 B CN 111624194B
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blade
intensity value
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calibration curve
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CN111624194A (en
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方丽
赵南京
马明俊
孟德硕
殷高方
刘建国
刘文清
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Hefei Institutes of Physical Science of CAS
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    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
    • G01N21/718—Laser microanalysis, i.e. with formation of sample plasma
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract

The invention provides a blade element nondestructive measurement method based on laser-induced breakdown spectroscopy, which utilizes natural distribution non-uniformity of element content in a blade to establish a calibration relation and comprises the following steps: obtaining a leaf to be calibrated which is dried to constant weight, and preparing a dry leaf specimen; obtaining the distribution of the spectral intensity values of the elements to be detected on the dry leaf specimen by a laser-induced breakdown spectroscopy technology, dividing the dry leaf specimen into N calibration areas according to the size of the spectral intensity values, wherein each calibration area corresponds to one spectral intensity value; measuring the concentration of an element to be measured in each calibration area on the dry leaf specimen, and drawing a calibration curve with an abscissa as the concentration of the element to be measured and an ordinate as a spectrum intensity value according to the measurement result; and obtaining the blade to be measured which is dried to constant weight, obtaining the spectrum intensity value of the blade to be measured through a laser-induced breakdown spectroscopy technology, and obtaining the concentration of the element to be measured of the blade to be measured by comparing with a calibration curve. The method is suitable for laser-induced breakdown spectroscopy and nondestructive measurement of various elements in the blade sample.

Description

Blade element nondestructive measurement method based on laser-induced breakdown spectroscopy
Technical Field
The invention relates to the technical field of laser-induced breakdown spectroscopy analysis, in particular to a blade element nondestructive measurement method based on laser-induced breakdown spectroscopy.
Background
Laser-induced breakdown spectroscopy (Laser-Induced Breakdown Spectroscopy, LIBS) is a technique for rapidly analyzing elemental substances by ablating the surface of a probe substance with a short pulse Laser focused by a lens to produce a microplasma, and analyzing the spectral signals and intensities radiated from these plasmas to determine the presence and concentration of the element. This analytical technique has a number of outstanding advantages: the method does not need sample preparation, is lossless and rapid in real time, can detect multiple elements in situ and simultaneously, has various forms of detected objects, and has wide application prospect. However, when the blade heavy metal is actually measured, the technology is influenced by a sample matrix, and a standard sample with similar matrix is generally difficult to find and difficult to calibrate. In addition, the heavy metal of the blade is unevenly distributed, so that the sample is required to be analyzed after being ground for eliminating the influence, and calibration is performed based on the ground sample, so that the sample is required to be ground for ensuring consistency during measurement, and the measurement speed is greatly reduced. In order to eliminate or reduce the matrix effect, the currently adopted calibration methods mainly comprise an internal standard method, a standard addition method and a free calibration method. The application of the methods promotes the development of LIBS analysis technology, but is limited to laboratory analysis and research stages, and some methods have complex processes and are not beneficial to on-site on-line monitoring.
Disclosure of Invention
Based on the technical problems in the background technology, the invention provides a blade element nondestructive measurement method based on laser-induced breakdown spectroscopy.
The invention provides a blade element nondestructive measurement method based on laser-induced breakdown spectroscopy, which comprises the following steps:
s1, obtaining a leaf to be calibrated which is dried to constant weight, and preparing a dry leaf specimen;
s2, acquiring spectral intensity value distribution of an element to be detected on a dry leaf specimen through a laser-induced breakdown spectroscopy technology, dividing the dry leaf specimen into N calibration areas according to the size of the spectral intensity value, wherein each calibration area corresponds to one spectral intensity value;
s3, measuring the concentration of the element to be measured in each calibration area on the dry leaf specimen, and drawing a calibration curve with the abscissa being the concentration of the element to be measured and the ordinate being the spectrum intensity value according to the measurement result;
s4, obtaining the blade to be tested which is dried to constant weight, obtaining the spectrum intensity value of the blade to be tested through a laser-induced breakdown spectroscopy technology, and obtaining the concentration of the element to be tested of the blade to be tested by comparing with a calibration curve.
Preferably, in step S3: and carrying out normalization processing on the spectrum intensity value of each calibration area on the dry leaf specimen, and drawing a calibration curve according to the spectrum intensity value after normalization processing.
Preferably, in step S3, the model for normalizing the optical intensity values is:
Figure SMS_1
the method comprises the steps of carrying out a first treatment on the surface of the I is the spectral intensity value, ">
Figure SMS_2
For normalizing the processed spectral intensity values, +.>
Figure SMS_3
Is a mapping function with laser energy E and plasma temperature T as independent variables.
Preferably, the step S4 specifically includes the following steps:
s41, selecting a calibration curve corresponding to the blade to be tested;
s42, selecting an alloy sample serving as a reference standard, and obtaining a spectrum intensity value of the alloy sample in a dry leaf specimen measuring environment through a laser-induced breakdown spectroscopy technology;
s43, measuring the spectral intensity value of the blade to be measured and the spectral intensity value of the alloy sample in the same measuring environment through a laser-induced breakdown spectroscopy technology;
s44, carrying out normalization processing on the actually measured spectrum intensity value of the blade to be measured, and correcting the spectrum intensity value of the blade to be measured by combining the measurement results of the alloy sample in different environments to obtain a spectrum intensity value correction value of the blade to be measured;
s45, obtaining the content of the element to be measured of the blade to be measured according to the comparison result of the spectrum intensity value correction value and the calibration curve.
Preferably, in step S44, the calculation model of the correction value of the spectral intensity value is:
Figure SMS_4
the method comprises the steps of carrying out a first treatment on the surface of the Wherein (1)>
Figure SMS_5
For the correction value of the spectral intensity values +.>
Figure SMS_6
For normalizing the processed spectral intensity values, +.>
Figure SMS_7
Measuring the spectral intensity value of the alloy sample measured in the environment for the dry leaf specimen, +.>
Figure SMS_8
Spectral intensity values of alloy samples measured in the measuring environment for the blade to be measured>
Figure SMS_9
。
Preferably, in step S41, a calibration curve measured on a dry leaf specimen of the same type as the leaf to be measured is selected.
Preferably, in step S41, the method for selecting the calibration curve corresponding to the blade to be tested is as follows:
characteristic parameters influencing the slope of the calibration curve of the breakdown spectrum are listed, a neural network model taking the characteristic parameters as input and the slope of the calibration curve of the breakdown spectrum as output is obtained through sample training, the slope of the calibration curve of the blade to be tested is obtained through the neural network model, and the calibration curve is selected according to the slope of the calibration curve.
Preferably, the neural network model is specifically trained using a genetic-error back propagation neural network.
Preferably, the characteristic parameter includes a matrix element content of the blade, the matrix element content including: C. h, O, N, P, S, si, K, mn.
According to the blade element nondestructive measurement method based on the laser-induced breakdown spectroscopy, through presetting the calibration curve, the subsequent calibration of the concentration of the element to be measured directly according to the measured spectral intensity value of the blade to be measured is facilitated, the processing such as grinding and tabletting is not needed to be carried out on the blade to be measured, the field application of blade element LIBS nondestructive measurement is realized, the method is suitable for the laser-induced breakdown spectroscopy and simultaneously nondestructive measurement of various elements in a blade sample, the influence of different matrixes on quantitative analysis is overcome, and the method is suitable for field rapid detection.
Drawings
FIG. 1 is a flow chart of a method for nondestructive measurement of blade element based on laser induced breakdown spectroscopy according to embodiment 1;
fig. 2 is a flowchart of another method for non-destructive measurement of blade elements based on laser-induced breakdown spectroscopy according to embodiment 2.
Detailed Description
Example 1
Referring to fig. 1, the blade element nondestructive measurement method based on laser-induced breakdown spectroscopy provided by the invention comprises the following steps of.
S1, obtaining the leaf to be calibrated which is dried to constant weight, and preparing a dry leaf specimen.
In the specific implementation, the collected leaves are clamped in a grid specimen clamp and dried at 60 ℃ to constant weight, so that a dry leaf specimen is prepared and stored in a sealing manner, and the leaf specimen is kept flat while water is evaporated. Specifically, the grid specimen holder is made of polytetrafluoroethylene, can resist high temperature and does not influence blade element measurement. The screen mesh of the grid specimen clamp is more than 15 meshes, so that the dried blade is not deformed, and after the blade is clamped, a gap of 0.5cm is formed in the middle, and grid indentation on the surface of the blade caused by clamping is avoided.
S2, acquiring spectral intensity value distribution of an element to be detected on the dry leaf specimen through a laser-induced breakdown spectroscopy technology, dividing the dry leaf specimen into N calibration areas according to the size of the spectral intensity value, wherein each calibration area corresponds to one spectral intensity value.
Specifically, when LIBS (laser induced breakdown spectroscopy) scans and measures, one pulse obtains an intensity value of an element to be measured, so that the spectrum intensity value corresponding to each calibration area is the average value of a plurality of spectrum intensity values obtained in the calibration area. S3, measuring the concentration of the element to be measured in each calibration area on the dry leaf specimen, and drawing a calibration curve with the abscissa being the concentration of the element to be measured and the ordinate being the spectrum intensity value according to the measurement result.
Specifically, in the step, the dry leaf specimen is digested after being cut according to the calibration area, so as to obtain the concentration of the element to be detected. In this embodiment, N coordinate points are formed according to the spectral intensity values of the N calibration areas and the concentrations of the elements to be measured, and are used to draw a calibration curve. It can be seen that the larger the value of N, the more the spectral intensity value is segmented, the more the calibration area is divided, and the more accurate the calibration curve is finally obtained. In this embodiment, N is 5 or more.
S4, obtaining the blade to be tested which is dried to constant weight, obtaining the spectrum intensity value of the blade to be tested through a laser-induced breakdown spectroscopy technology, and obtaining the concentration of the element to be tested of the blade to be tested by comparing with a calibration curve.
Example 2
In contrast to embodiment 1, in step S3 of the present embodiment: and carrying out normalization processing on the spectrum intensity value of each calibration area on the dry leaf specimen, and drawing a calibration curve according to the spectrum intensity value after normalization processing.
Therefore, through normalization processing of the spectrum intensity values, normalization correction of spectral lines is realized, and influence of system parameters and environmental condition changes is eliminated. In the specific implementation, the spectrum can be normalized by combining the fluctuation of laser energy, plasma temperature and the like as external references so as to improve the spectrum measurement precision and the comparability between spectrums
Specifically, the model for normalizing the optical intensity values is:
Figure SMS_10
the method comprises the steps of carrying out a first treatment on the surface of the I is the spectral intensity value, ">
Figure SMS_11
For normalizing the processed spectral intensity values, +.>
Figure SMS_12
Is a mapping function with laser energy E and plasma temperature T as independent variables. Specifically, the laser energy E can be obtained by an energy meter at the time of measurement; the plasma temperature T can be calculated by utilizing the Boltzmann planar method according to the obtained LIBS spectral line. Step S4 of the present embodiment specifically includes the following steps:
s41, selecting a calibration curve corresponding to the blade to be tested.
In specific implementation, the calibration curve measured by the dry leaf specimen of the same type as the leaf to be measured is preferentially selected. Specifically, the same blade can be sheared along the central axis, half of the blade is used as a dry blade specimen for calculating a calibration curve, and the other half of the blade is used as a blade to be measured. Therefore, the measurement of the blades of the same type according to the calibration curve is facilitated, and the calibration curve can be verified through the measurement result of the blade to be tested.
The calibration curve may also be screened in the following manner.
Firstly, characteristic parameters influencing the slope of a breakdown spectrum calibration curve are listed, and a neural network model taking the characteristic parameters as input and the slope of the breakdown spectrum calibration curve as output is obtained through sample training; and obtaining the slope of a calibration curve of the blade to be tested through the neural network model, and selecting the calibration curve according to the slope of the calibration curve.
The method for screening the calibration curve according to the characteristic parameters provided by the embodiment meets the calibration requirements of different blades to be tested, and is beneficial to eliminating the influence of factors such as matrix effect and the like on the same type of blades.
Specifically, in this embodiment, the neural network model is specifically trained using a genetic-error back propagation neural network. The characteristic parameters comprise the matrix element content of the blade, wherein the matrix element content comprises the following components: C. h, O, N, P, S, si, K, mn.
S42, selecting an alloy sample serving as a reference standard, and obtaining a spectrum intensity value of the alloy sample in a dry leaf specimen measuring environment through a laser-induced breakdown spectroscopy technology. Specifically, the alloy sample is selected from a type that is stable in properties and easy to preserve.
S43, measuring the spectral intensity value of the blade to be measured and the spectral intensity value of the alloy sample in the same measuring environment through a laser-induced breakdown spectroscopy technology.
S44, carrying out normalization processing on the actually measured spectrum intensity value of the blade to be measured, and correcting the spectrum intensity value of the blade to be measured by combining the measurement results of the alloy sample in different environments to obtain the spectrum intensity value correction value of the blade to be measured.
Specifically, the calculation model of the correction value of the spectrum intensity value is:
Figure SMS_13
the method comprises the steps of carrying out a first treatment on the surface of the Wherein (1)>
Figure SMS_14
For the correction value of the spectral intensity values +.>
Figure SMS_15
For normalizing the processed spectral intensity values, +.>
Figure SMS_16
Measuring the spectral intensity value of the alloy sample measured in the environment for the dry leaf specimen, +.>
Figure SMS_17
Spectral intensity values of alloy samples measured in the measuring environment for the blade to be measured>
Figure SMS_18
. In this embodiment, the influence of energy fluctuation, system parameters, plasma temperature, measurement environment, and the like on the optical intensity value is eliminated by the normalization processing and the correction of the alloy sample.
S45, obtaining the content of the element to be measured of the blade to be measured according to the comparison result of the spectrum intensity value correction value and the calibration curve.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be able to apply equivalents and modifications to the technical solution and the inventive concept thereof within the scope of the present invention.

Claims (5)

1. The blade element nondestructive measurement method based on the laser-induced breakdown spectroscopy is characterized by comprising the following steps of:
s1, obtaining a leaf to be calibrated which is dried to constant weight, and preparing a dry leaf specimen;
s2, acquiring spectral intensity value distribution of an element to be detected on a dry leaf specimen through a laser-induced breakdown spectroscopy technology, dividing the dry leaf specimen into N calibration areas according to the size of the spectral intensity value, wherein each calibration area corresponds to one spectral intensity value;
s3, measuring the concentration of the element to be measured in each calibration area on the dry leaf specimen, and drawing a calibration curve with the abscissa being the concentration of the element to be measured and the ordinate being the spectrum intensity value according to the measurement result;
s4, obtaining a blade to be tested which is dried to constant weight, obtaining a spectrum intensity value of the blade to be tested through a laser-induced breakdown spectroscopy technology, and obtaining the concentration of an element to be tested of the blade to be tested by comparing with a calibration curve;
the step S4 specifically includes the following steps:
s41, selecting a calibration curve corresponding to the blade to be tested;
s42, selecting an alloy sample serving as a reference standard, and obtaining a spectrum intensity value of the alloy sample in a dry leaf specimen measuring environment through a laser-induced breakdown spectroscopy technology;
s43, measuring the spectral intensity value of the blade to be measured and the spectral intensity value of the alloy sample in the same measuring environment through a laser-induced breakdown spectroscopy technology;
s44, carrying out normalization processing on the actually measured spectrum intensity value of the blade to be measured, and correcting the spectrum intensity value of the blade to be measured by combining the measurement results of the alloy sample in different environments to obtain a spectrum intensity value correction value of the blade to be measured;
s45, obtaining the content of the element to be detected of the blade to be detected according to the comparison result of the spectrum intensity value correction value and the calibration curve;
in the step S41, the method for selecting the calibration curve corresponding to the blade to be tested is as follows:
characteristic parameters influencing the slope of a breakdown spectrum calibration curve are listed, a neural network model taking the characteristic parameters as input and the slope of the breakdown spectrum calibration curve as output is obtained through sample training, the slope of the calibration curve of the blade to be tested is obtained through the neural network model, and a calibration curve is selected according to the slope of the calibration curve;
in the step S44, the calculation model of the correction value of the spectral intensity value is:
Figure QLYQS_1
the method comprises the steps of carrying out a first treatment on the surface of the Wherein (1)>
Figure QLYQS_2
For the correction value of the spectral intensity values +.>
Figure QLYQS_3
To normalize the processed spectral intensity values,
Figure QLYQS_4
measuring the spectral intensity value of the alloy sample measured in the environment for the dry leaf specimen, +.>
Figure QLYQS_5
Spectral intensity values of alloy samples measured in the measuring environment for the blade to be measured>
Figure QLYQS_6
。
2. The method for non-destructive measurement of a blade element based on laser induced breakdown spectroscopy of claim 1, wherein in step S3: and carrying out normalization processing on the spectrum intensity value of each calibration area on the dry leaf specimen, and drawing a calibration curve according to the spectrum intensity value after normalization processing.
3. The method for non-destructive measurement of a blade element based on laser induced breakdown spectroscopy of claim 2, wherein in step S3, the model for normalizing the intensity values of the spectrum is:
Figure QLYQS_7
the method comprises the steps of carrying out a first treatment on the surface of the I is the spectral intensity value, ">
Figure QLYQS_8
For normalizing the processed spectral intensity values, +.>
Figure QLYQS_9
Is a mapping function with laser energy E and plasma temperature T as independent variables.
4. The method for non-destructive measurement of a leaf element based on laser induced breakdown spectroscopy of claim 1 wherein the neural network model is specifically trained using a genetic-error back propagation neural network.
5. The method for non-destructive measurement of a blade element based on laser induced breakdown spectroscopy of claim 1, wherein the characteristic parameter comprises a matrix element content of the blade, the matrix element content comprising: C. h, O, N, P, S, si, K, mn.
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