CN107817239A - A kind of LIBS spectral correction methods based on plasma position information - Google Patents
A kind of LIBS spectral correction methods based on plasma position information Download PDFInfo
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- 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
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- G—PHYSICS
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Abstract
The present invention relates to a kind of LIBS spectrum-stable methods based on plasma position information, concretely comprise the following steps：1) LIBS spectral signals and the corresponding Plasma picture signal under different sample positions are obtained；2) plasma position information is extracted from Plasma picture information；3) relation function of LIBS spectrums region and value with corresponding plasma position is established by approximating method；Relation function of the specific the intensity of spectral line of LIBS spectrum with corresponding plasma position is established by approximating method；4) relation function obtained in using 3) establishes comprehensive correction function；5) the LIBS spectrum of Location-Unknown are corrected using correction function.Characteristic spectral line after being corrected with this method, there is higher stability, more reliable spectral line information is provided for quantitative (qualitative) analysis.
Description
Technical field
The invention belongs to spectrum analysis and material composition constituent analysis field, is specifically that one kind is based on plasma position
The LIBS spectral correction methods of confidence breath.
Background technology
LIBS (LIBS) analytical technology, it is a kind of original of plasma using laser excitation as light source
Sub- emission spectrographic analysis technology.Material composition qualitative and quantitative analysis based on LIBS technologies, the sample system of complexity is not required to it
It is standby, the features such as online multicomponent in situ is quickly analyzed can be achieved, become many industry necks such as metallurgy, the energy, food, chemical industry
The hot spot application technology in domain.However, because obtained spectral signal stability is not high, LIBS be more served only for qualitative analysis and
Semi-quantitative analysis.Therefore, the stability of LIBS signals is improved, can just it is met the needs of quantitative analysis, so as to applied to real
When online in situ detection in.
The preprocessing procedures of the raising stability generally used at present, mainly choose reference line and full spectrum normalizes
Method.The former needs the element containing stable content in testing sample, and the element has clearly in the range of Detection wavelength
Characteristic spectral line；The latter assumes in the range of the Detection wavelength all spectral intensities and value is perseverance in the case where detection environment is constant
Fixed, it is this when detection spectral coverage scope is narrower larger with the fluctuation of matrix element content to assume to lack reasonability.Pass through extraction
Plasma characteristics parameter is corrected to spectral signal, is a kind of spectral correction method based on plasma physics feature,
But its need detect a wider spectral coverage scope, and need in the range of this comprising a plurality of clearly atom, ion line, and
Modeled by the model of fit of complexity.
Most directly reflect mode as luminescence of plasma situation, Plasma picture is always when analyzing plasma
The important channel that space division cloth and research plasma are formed.Plasma position information is extracted from Plasma picture, and then
Correction is shaken by the inconsistent caused spectral signal of testing sample apparent height, is a kind of feasible means of stable spectra signal.
The content of the invention
For in place of above shortcomings in the prior art, the technical problem to be solved in the present invention is to pass through plasma
The plasma position information included in image, founding mathematical models, LIBS spectral signals are corrected, so as to obtain into rower
The reliable and stable characteristic spectral line intensity of setting analysis.
The used to achieve the above object technical scheme of the present invention is：A kind of LIBS based on plasma position information
Spectral correction method, comprise the following steps：
Step 1：Obtain the LIBS spectral signals under sample different height and corresponding Plasma picture；
Step 2：The light-emitting zone of plasma is determined according to each pixel value in Plasma picture, according to luminous zone
The pattern and pixel value in domain determine plasma position；
Step 3：By approximating method, establish in the range of LIBS spectra collections full spectral coverage and with plasma position information
Respective function relation；Meanwhile by approximating method, establish the specific characteristic spectral line intensity of LIBS spectrum and plasma position information
Respective function relation；
Step 4：The function obtained according to step 3, establish the correction of plasma position information correction LIBS spectral signals
Function；
Step 5：The correction function that applying step 4 the obtains LIBS spectrum unknown to height of specimen is corrected.
Step 1 obtains the LIBS spectrum of different height of specimen and corresponding Plasma picture, movement by mobile example
Distance is judged by Plasma picture.
The step 2 is specially：Setting pixel threshold first determines heating region, wiping out background noise；Then lead to
Cross calculate length-width ratio, in all directions pixel value downward gradient and region image center of gravity, determine plasma position parameter.
It is described by approximating method, establish full spectral coverage and pair with plasma position information in the range of LIBS spectra collections
Functional relation is answered, is specially：
Calculate the intensity of spectral line under diverse location in the range of obtained LIBS spectral detection spectral coverages and, pass through ISUM=fSUM
(h) corresponding relation of spectral coverage intensity and value and plasma position parameter, wherein f are fittedSUM(h) it is fitting function.
The expression way of the fitting function is as follows：
Wherein sgn () represent sign function, h be represent plasma position information parameter, h0,σ1,σ2It is to pass through plan
Close the offset parameter and location parameter determined.
It is described by approximating method, it is corresponding with plasma position information to establish the specific characteristic spectral line intensity of LIBS spectrum
Functional relation, it is specially：
Pass through Iλ=fλ(h) corresponding relation of each characteristic spectral line intensity and plasma position parameter, wherein f are determinedλ(h)
For fitting function.
The expression way of the fitting function is as follows：
Wherein sgn () represent sign function, h be represent plasma position information parameter, h0,σ1,σ2It is to pass through plan
Close the offset parameter and location parameter determined.
The expression way of the correction function is as follows：
Wherein, I 'λRepresent the intensity of spectral line after correction, IλIt is original the intensity of spectral line, ISUMIt is original spectral coverage intensity and fλ
(h) fitting function for being the specific characteristic spectral line intensity of LIBS spectrum with the respective function relation of plasma position information, fSUM
(h) it is full spectral coverage and the fitting function with the respective function relation of plasma position information in the range of LIBS spectra collections, its
Middle h is the plasma position parameter by being extracted in Plasma picture, h0For fλ(h) h during maximum is obtained.
The present invention has advantages below and beneficial effect：
1. method proposed by the present invention, it is not required to detect wide spectrum to obtain spectroscopic data calculating plasma characteristic parameter,
It is not required to shake to suppress spectrum by changing sample position, plasma position is extracted from the Plasma picture of synchronous acquisition
Information, and directly correct spectral signal using mathematical modeling.
2. method proposed by the present invention, while characteristic spectral line is considered in itself with selected spectral coverage region entirety with sample position
The fluctuation of change, built mathematical modeling is set to have taken into account full spectrum while by plasma position information correction spectral signal
The advantages of method for normalizing.
3. model needed for method proposed by the present invention, it is not required to by testing strict limit as the positional information of independent variable
System, can be extracted, the experimental implementation complexity for modeling is low from Plasma picture.
Brief description of the drawings
Fig. 1 is the inventive method implementation process figure；
Fig. 2 is the LIBS spectrum of specific region under different sample positions；
Fig. 3 is the Plasma picture under different sample positions；
Fig. 4 is the characteristic spectral line intensity level of five kinds of elements of Si, Fe, Cu, Mn and Mg in aluminum alloy sample with plasma position
Put the matched curve of change；
Fig. 5 is that the characteristic spectral line after being corrected using the inventive method is directly marked with the characteristic spectral line after full spectrum normalization
Fixed experimental result.
Embodiment
Below in conjunction with the accompanying drawings and example the present invention is described in further detail.
The present invention causes Laser Focusing depth different with spectrometer test position for testing sample position difference, and then produces
The problem of third contact of a total solar or lunar eclipse spectrum shake, by Plasma picture, plasma position information is obtained, founding mathematical models are to different samples
The spectroscopic data obtained under position is standardized, to realize the correction of spectroscopic data.
As shown in figure 1, method by LIBS experiment porch obtains spectroscopic data and Plasma picture after starting, from plasma
Positional information is extracted in body image information, with reference to the intensity of individual features spectral line and spectral coverage, establishes model of fit, and by obtaining
Fitting function spectrum to be analyzed is corrected.It is as follows to implement step：
Step 1：Obtain the LIBS spectral signals under sample different height (canonical correlation region LIBS spectrum are as shown in Figure 2)
With corresponding Plasma picture signal (classicalpiston image is as shown in Figure 3), wherein different height of specimen pass through regulation
Example platform is realized.
Step 2：Luminescence of plasma region is determined according to each pixel value in Plasma picture, according to light-emitting zone
Pattern and pixel value determine plasma position.Setting pixel threshold first determines heating region, wiping out background noise；So
Afterwards by calculate length-width ratio, in all directions pixel value downward gradient and region image center of gravity, determine that plasma position is joined
Number.
Step 3：By approximating method, establish in the range of LIBS spectra collections full spectral coverage and with plasma position information
Respective function relation.Calculate the intensity of spectral line under diverse location in the range of obtained LIBS spectral detection spectral coverages and, pass through ISUM=
F (h) fits the corresponding relation of spectral coverage intensity and value and plasma position parameter.Wherein,
Sgn () represent sign function, h be represent plasma position information parameter, h0,σ1,σ2It is to be determined by being fitted
Offset parameter and location parameter.
Step 4：For different characteristic spectral lines, by the fitting function of step 3, pass through Iλ=f (h) determines each characteristic spectral line
The corresponding relation of intensity and plasma position parameter；
Step 5：The fitting function determined with reference to step 3, step 4, passes through plasma position information correction LIBS spectrum
The collective model of signal.Specific correction function form is as follows：
Wherein, I 'λRepresent the intensity of spectral line after correction, IλIt is original the intensity of spectral line, ISUMIt is original spectral coverage intensity and fλ
(h) be step 4 determine fitting function, fSUM(h) be step 3 determine fitting function, wherein h is by Plasma picture
The plasma position parameter of extraction, h0For fλ(h) h during maximum is obtained.
Step 6：The model that applying step 5 the obtains LIBS spectrum unknown to height of specimen is analyzed and corrected.
The correction spectral line that method obtains, demarcation analysis is can be directly used for, can also be passed through as the input of complicated peg model
Multivariable technique further improves quantitative (qualitative) analysis ability of LIBS.
It is corresponding to five kinds of elements of Si, Fe, Cu, Mn and Mg in 5 pieces of aluminum alloy samples that calibration model is established as stated above
5 characteristic spectral lines under the shake of 1mm sample positions the spectrum that gathers corrected, and entered using the intensity of spectral line after correction
Direct demarcation is gone.Obtained matched curve is as shown in figure 4, specific fitting parameter value such as following table：
Using the result that the intensity of spectral line after correction is demarcated to concentration of element with being demarcated using full spectrum normalized intensity
Result it is as shown in Figure 5.Wherein blue line corresponds to full spectral normalization method, and red line represents method proposed by the present invention.It is determined that it is
Number (R2), relative standard deviation (RSD), the performance indications such as root-mean-square error (RMSE) all illustrate that this method can reach than full spectrum
The contrast of the more preferable spectral line calibration result of method for normalizing, more specifically index see the table below：
Claims (8)
1. a kind of LIBS spectral correction methods based on plasma position information, it is characterised in that comprise the following steps：
Step 1：Obtain the LIBS spectral signals under sample different height and corresponding Plasma picture；
Step 2：The light-emitting zone of plasma is determined according to each pixel value in Plasma picture, according to light-emitting zone
Pattern and pixel value determine plasma position；
Step 3：By approximating method, full spectral coverage and corresponding with plasma position information is established in the range of LIBS spectra collections
Functional relation；Meanwhile by approximating method, establish pair of the specific characteristic spectral line intensity of LIBS spectrum and plasma position information
Answer functional relation；
Step 4：The function obtained according to step 3, establish the correction function of plasma position information correction LIBS spectral signals；
Step 5：The correction function that applying step 4 the obtains LIBS spectrum unknown to height of specimen is corrected.
2. a kind of LIBS spectral correction methods based on plasma position information according to claim 1, its feature exist
In step 1 obtains the LIBS spectrum of different height of specimen and corresponding Plasma picture, displacement by mobile example
Judged by Plasma picture.
3. a kind of LIBS spectral correction methods based on plasma position information according to claim 1, its feature exist
In the step 2 is specially：Setting pixel threshold first determines heating region, wiping out background noise；Then calculating is passed through
The center of gravity of image, determines plasma position parameter in length-width ratio, all directions pixel value downward gradient and region.
4. a kind of LIBS spectral correction methods based on plasma position information according to claim 1, its feature exist
In, it is described by approximating method, establish full spectral coverage and the corresponding letter with plasma position information in the range of LIBS spectra collections
Number relation, it is specially：
Calculate the intensity of spectral line under diverse location in the range of obtained LIBS spectral detection spectral coverages and, pass through ISUM=fSUM(h) intend
Close out the corresponding relation of spectral coverage intensity and value and plasma position parameter, wherein fSUM(h) it is fitting function.
5. a kind of LIBS spectral correction methods based on plasma position information according to claim 4, its feature exist
In the expression way of the fitting function is as follows：
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Wherein sgn () represent sign function, h be represent plasma position information parameter, h0,σ1,σ2It is true by being fitted
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6. a kind of LIBS spectral correction methods based on plasma position information according to claim 1, its feature exist
In, it is described by approximating method, establish the respective function of the specific characteristic spectral line intensity of LIBS spectrum and plasma position information
Relation, it is specially：
Pass through Iλ=fλ(h) corresponding relation of each characteristic spectral line intensity and plasma position parameter, wherein f are determinedλ(h) it is plan
Close function.
7. a kind of LIBS spectral correction methods based on plasma position information according to claim 6, its feature exist
In the expression way of the fitting function is as follows：
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Wherein sgn () represent sign function, h be represent plasma position information parameter, h0,σ1,σ2It is true by being fitted
Fixed offset parameter and location parameter.
8. a kind of LIBS spectral correction methods based on plasma position information according to claim 1, its feature exist
In the expression way of the correction function is as follows：
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Wherein, I 'λRepresent the intensity of spectral line after correction, IλIt is original the intensity of spectral line, ISUMIt is original spectral coverage intensity and fλ(h) it is
The fitting function of the specific characteristic spectral line intensity of LIBS spectrum and the respective function relation of plasma position information, fSUM(h) it is
Full spectral coverage and the fitting function with the respective function relation of plasma position information, wherein h are in the range of LIBS spectra collections
By the plasma position parameter extracted in Plasma picture, h0For fλ(h) h during maximum is obtained.
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| CN110751048A (en) * | 2019-09-20 | 2020-02-04 | 华中科技大学 | Laser probe classification method and device based on image characteristic automatic spectral line selection |
| CN111272735A (en) * | 2020-03-26 | 2020-06-12 | 中国科学院空天信息创新研究院 | Detection method of laser-induced breakdown spectroscopy |
| CN111289496A (en) * | 2020-03-26 | 2020-06-16 | 中国科学院空天信息创新研究院 | Detection method and device for long-distance zoom laser-induced breakdown spectroscopy |
| CN112611744A (en) * | 2020-12-11 | 2021-04-06 | 中国海洋大学 | Underwater LIBS spectrum correction method based on sound wave signals |
| CN113624746A (en) * | 2021-08-05 | 2021-11-09 | 合肥金星机电科技发展有限公司 | LIBS spectrum drift online correction method and system |
| CN113624745A (en) * | 2021-07-01 | 2021-11-09 | 清华大学 | Method for improving long-term stability of laser-induced breakdown spectroscopy based on light spots |
| CN114894781A (en) * | 2022-05-25 | 2022-08-12 | 中国海洋大学 | Underwater LIBS spectrum standardization generalization method and system based on external signal |
| WO2023221282A1 (en) * | 2022-05-18 | 2023-11-23 | 合肥金星智控科技股份有限公司 | Model correction method, spectroscopy device, computer device, and storage medium |
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