CN107817239B - A kind of LIBS spectral correction method based on plasma position information - Google Patents
A kind of LIBS spectral correction method based on plasma position information Download PDFInfo
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Abstract
The present invention relates to a kind of the LIBS spectrum-stable method based on plasma position information, specific steps are as follows: 1) obtain the LIBS spectral signal and corresponding Plasma picture signal under different sample positions；2) plasma position information is extracted from Plasma picture information；3) relation function of LIBS spectrum region and value with corresponding plasma position is established by approximating method；The relation function of LIBS spectrum specific the intensity of spectral line and corresponding plasma position is established by approximating method；4) comprehensive correction function is established using relation function obtained in 3)；5) it is corrected using LIBS spectrum of the correction function to Location-Unknown.Characteristic spectral line after being corrected with this method has higher stability, provides more reliable spectral line information for quantitative (qualitative) analysis.
Description
Technical field
It is specifically a kind of based on plasma position the invention belongs to spectrum analysis and material composition constituent analysis field
The LIBS spectral correction method of confidence breath.
Background technique
Laser induced breakdown spectroscopy (LIBS) analytical technology is a kind of original of the plasma using laser excitation as light source
Sub- emission spectrographic analysis technology.Material composition qualitative and quantitative analysis based on LIBS technology is not required to complicated sample system with it
It is standby, it can be achieved that the features such as online multicomponent in situ is quickly analyzed, becomes many industry such as metallurgy, the energy, food, chemical industry and leads
The hot spot application technology in domain.However, since obtained spectral signal stability is not high, LIBS be more served only for qualitative analysis and
Semi-quantitative analysis.Therefore, the stability for improving LIBS signal, can just make it meet the needs of quantitative analysis, to be applied to real
When online in situ detection in.
The preprocessing procedures of the raising stability generallyd use at present, mainly selection reference line and full spectrum normalization
Method.The former needs the element in sample to be tested containing stable content, and the element has clearly within the scope of Detection wavelength
Characteristic spectral line；The latter assume within the scope of Detection wavelength all spectral intensities and value detect environment it is constant in the case where be perseverance
Fixed, when detection spectral coverage range is relatively narrow larger with the fluctuation of matrix element content, this hypothesis lacks reasonability.Pass through extraction
Plasma characteristics parameter is corrected spectral signal, is a kind of spectral correction method based on plasma physics feature,
But it needs to detect a wider spectral coverage range, and need within the scope of this comprising a plurality of clearly atom, ion line, and
It is modeled by complicated model of fit.
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, in turn
Correction is a kind of feasible means of stable spectra signal by the inconsistent caused spectral signal shake of sample to be tested apparent height.
Summary of the invention
Aiming at the defects existing in the prior art, the technical problem to be solved by the present invention is to pass through plasma
The plasma position information for including in image, founding mathematical models correct LIBS spectral signal, to obtain to be marked
The reliable and stable characteristic spectral line intensity of setting analysis.
Present invention technical solution used for the above purpose is: a kind of LIBS based on plasma position information
Spectral correction method, comprising the following steps:
Step 1: obtaining the LIBS spectral signal and corresponding Plasma picture under sample different height；
Step 2: the light emitting region of plasma is determined according to pixel value each in Plasma picture, according to luminous zone
The pattern and pixel value in domain determine plasma position；
Step 3: by approximating method, establish within the scope of LIBS spectra collection full spectral coverage and with plasma position information
Respective function relationship；Meanwhile by approximating method, the specific characteristic spectral line intensity of LIBS spectrum and plasma position information are established
Respective function relationship；
Step 4: the function obtained according to step 3 establishes the correction of plasma position information correction LIBS spectral signal
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 and corresponding Plasma picture of different height of specimen by mobile example, mobile
Distance is judged by Plasma picture.
The step 2 specifically: 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 within the scope of LIBS spectra collection
Functional relation is answered, specifically:
Calculate the intensity of spectral line under different location within the scope of obtained LIBS spectral detection spectral coverage and, pass through ISUM=fSUM
(h) corresponding relationship of spectral coverage intensity and value and plasma position parameter is fitted, wherein fSUMIt (h) is fitting function.
The expression way of the fitting function is as follows:
Wherein sgn () indicates that sign function, h are the parameter for indicating plasma position information, h0,σ1,σ2It is by quasi-
Close determining offset parameter and location parameter.
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, specifically:
Pass through Iλ=fλ(h) corresponding relationship of each characteristic spectral line intensity and plasma position parameter is determined, wherein fλ(h)
For fitting function.
The expression way of the fitting function is as follows:
Wherein sgn () indicates that sign function, h are the parameter for indicating plasma position information, h0,σ1,σ2It is by quasi-
Close determining offset parameter and location parameter.
The expression way of the correction function is as follows:
Wherein, I 'λThe intensity of spectral line after indicating correction, IλIt is original the intensity of spectral line, ISUMIt is original spectral coverage intensity and fλ
(h) be the specific characteristic spectral line intensity of LIBS spectrum and plasma position information respective function relationship fitting function, fSUM
It (h) is full spectral coverage and the fitting function with the respective function relationship of plasma position information within the scope of LIBS spectra collection,
Middle h is the plasma position parameter by extracting in Plasma picture, h0For fλ(h) h when maximum value is obtained.
The present invention has the following advantages and beneficial effects:
1. method proposed by the present invention, it is not required to detection wide spectrum to obtain spectroscopic data calculating plasma characteristic parameter,
It is not required to inhibit spectrum to shake by changing sample position, extracts plasma position from the Plasma picture of synchronous acquisition
Information, and spectral signal is directly corrected using mathematical model.
2. method proposed by the present invention, while characteristic spectral line itself and selected spectral coverage region entirety are considered with sample position
The fluctuation of variation makes built mathematical model while through plasma position information correction spectral signal, has taken into account full spectrum
The advantages of method for normalizing.
3. model needed for method proposed by the present invention, the location information as independent variable is not required to by testing stringent limit
System, can extract, the experimental implementation complexity for modeling is low from Plasma picture.
Detailed description of the invention
Fig. 1 is the method for the present invention implementation flow chart；
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 value of five kinds of elements of Si, Fe, Cu, Mn and Mg in aluminum alloy sample with plasma position
Set the matched curve of variation；
Fig. 5 is that the characteristic spectral line and the characteristic spectral line after full spectrum normalization after being corrected using the method for the present invention are directly marked
Fixed experimental result.
Specific embodiment
With reference to the accompanying drawing and example the present invention is described in further detail.
The present invention causes the laser depth of focus and spectrometer to detect position difference for sample to be tested 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
Location information is extracted in body image information, in conjunction with 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.The specific implementation steps are as follows:
Step 1: obtaining the LIBS spectral signal under sample different height (canonical correlation region LIBS spectrum is as shown in Figure 2)
With corresponding Plasma picture signal (classicalpiston image is as shown in Figure 3), wherein different height of specimen passes through adjusting
Example platform is realized.
Step 2: luminescence of plasma region being determined according to pixel value each in Plasma picture, according to light emitting region
Pattern and pixel value determine plasma position.Setting pixel threshold first determines heating region, wiping out background noise；So
Afterwards by the center of gravity of image in calculating length-width ratio, all directions pixel value downward gradient and region, determine that plasma position is joined
Number.
Step 3: by approximating method, establish within the scope of LIBS spectra collection full spectral coverage and with plasma position information
Respective function relationship.Calculate the intensity of spectral line under different location within the scope of obtained LIBS spectral detection spectral coverage and, pass through ISUM=
F (h) fits the corresponding relationship of spectral coverage intensity and value and plasma position parameter.Wherein,Sgn () indicates sign function, and h is table
Show the parameter of plasma position information, h0,σ1,σ2It is the offset parameter and location parameter determining by fitting.
Step 4: passing through I by the fitting function of step 3 for different characteristic spectral linesλ=f (h) determines each characteristic spectral line
The corresponding relationship of intensity and plasma position parameter；
Step 5: the fitting function determined in conjunction with 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 'λThe intensity of spectral line after indicating correction, IλIt is original the intensity of spectral line, ISUMIt is original spectral coverage intensity and fλ
It (h) is the determining fitting function of step 4, fSUMIt (h) is the determining fitting function of step 3, wherein h is by Plasma picture
The plasma position parameter of extraction, h0For fλ(h) h when maximum value is obtained.
Step 6: the model that applying step 5 the obtains LIBS spectrum unknown to height of specimen is analyzed and is corrected.
The correction spectral line that method obtains can be directly used for calibration analysis, also can be used as the input of complicated peg model, pass through
Multivariable technique further increases LIBS and quantifies (qualitative) analysis ability.
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 according to the above method
5 characteristic spectral lines under the shake of 1mm sample position the spectrum that acquires corrected, and using the intensity of spectral line after correction into
Direct calibration is gone.Obtained matched curve is as shown in figure 4, specific fitting parameter value is as follows:
It is demarcated using the result that the intensity of spectral line after correction demarcates concentration of element with 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.Determine system
Number (R2), relative standard deviation (RSD), the performance indicators such as root-mean-square error (RMSE) all illustrate that this method can reach than composing entirely
The better spectral line calibration result of method for normalizing, more specific index comparison see the table below:
Claims (5)
1. a kind of LIBS spectral correction method based on plasma position information, which comprises the following steps:
Step 1: obtaining the LIBS spectral signal and corresponding Plasma picture under sample different height；
Step 2: the light emitting region of plasma is determined according to pixel value each in Plasma picture, according to light emitting region
Pattern and pixel value determine plasma position；
Step 3: by approximating method, establishing within the scope of LIBS spectra collection full spectral coverage and corresponding with plasma position information
Functional relation；Meanwhile by approximating method, pair of LIBS spectrum specific characteristic spectral line intensity and plasma position information is established
Answer functional relation；
Step 4: the function obtained according to step 3 establishes the correction function of plasma position information correction LIBS spectral signal；
Step 5: the correction function that applying step 4 the obtains LIBS spectrum unknown to height of specimen is corrected；
It is described by approximating method, establish full spectral coverage and the corresponding letter with plasma position information within the scope of LIBS spectra collection
Number relationship, specifically:
Calculate the intensity of spectral line under different location within the scope of obtained LIBS spectral detection spectral coverage and, pass through ISUM=fSUM(h) intend
The corresponding relationship of spectral coverage intensity and value and plasma position parameter is closed out, wherein fSUMIt (h) is fitting function；
It is described by approximating method, establish the respective function of LIBS spectrum specific characteristic spectral line intensity and plasma position information
Relationship, specifically:
Pass through Iλ=fλ(h) corresponding relationship of each characteristic spectral line intensity and plasma position parameter is determined, wherein fλIt (h) is quasi-
Close function；
The expression way of the correction function is as follows:
Wherein, I 'λThe intensity of spectral line after indicating 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 respective function relationship of the specific characteristic spectral line intensity of LIBS spectrum and plasma position information, fSUM(h) it is
Full spectral coverage and the fitting function with the respective function relationship of plasma position information within the scope of LIBS spectra collection, wherein h be
By the plasma position parameter extracted in Plasma picture, h0For fλ(h) h when maximum value is obtained.
2. a kind of LIBS spectral correction method based on plasma position information according to claim 1, feature exist
In step 1 obtains the LIBS spectrum and corresponding Plasma picture of different height of specimen, moving distance by mobile example
Judged by Plasma picture.
3. a kind of LIBS spectral correction method based on plasma position information according to claim 1, feature exist
In the step 2 specifically: setting pixel threshold first determines heating region, wiping out background noise；Then pass through calculating
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 method based on plasma position information according to claim 1, feature exist
In the expression way of the fitting function is as follows:
Wherein sgn () indicates that sign function, h are the parameter for indicating plasma position information, h0,σ1,σ2It is true by being fitted
Fixed offset parameter and location parameter.
5. a kind of LIBS spectral correction method based on plasma position information according to claim 1, feature exist
In the expression way of the fitting function is as follows:
Wherein sgn () indicates that sign function, h are the parameter for indicating plasma position information, h0,σ1,σ2It is true by being fitted
Fixed offset parameter and location parameter.
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| CN110751048B (en) * | 2019-09-20 | 2022-06-14 | 华中科技大学 | Laser probe classification method and device based on image characteristic automatic spectral line selection |
| CN111272735B (en) * | 2020-03-26 | 2023-06-30 | 中国科学院空天信息创新研究院 | Detection method of laser-induced breakdown spectroscopy |
| CN111289496B (en) * | 2020-03-26 | 2023-05-19 | 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 |
| CN112611744B (en) * | 2020-12-11 | 2021-12-10 | 中国海洋大学 | Underwater LIBS spectrum correction method based on sound wave signals |
| CN113624745B (en) * | 2021-07-01 | 2022-10-18 | 清华大学 | Method for improving long-term stability of laser-induced breakdown spectroscopy based on light spots |
| CN113624746B (en) * | 2021-08-05 | 2022-09-30 | 合肥金星智控科技股份有限公司 | LIBS spectral drift online correction method and system |
| CN114636688B (en) * | 2022-05-18 | 2022-08-12 | 合肥金星智控科技股份有限公司 | Model correction method, spectroscopic apparatus, computer apparatus, and storage medium |
| CN114894781B (en) * | 2022-05-25 | 2023-06-06 | 中国海洋大学 | Underwater LIBS spectrum standardization generalization method and system based on external signals |
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