CN104655595B - The analysis system and method for LIBS - Google Patents
The analysis system and method for LIBS Download PDFInfo
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- CN104655595B CN104655595B CN201510073090.1A CN201510073090A CN104655595B CN 104655595 B CN104655595 B CN 104655595B CN 201510073090 A CN201510073090 A CN 201510073090A CN 104655595 B CN104655595 B CN 104655595B
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Abstract
Present invention offer a kind of analysis system and method for two-dimentional energy associated laser induced breakdown spectroscopy, the system, including：Laser, spectrometer, delay time generator, optical fiber, sample and computer；The laser, impacts for periodically emission pulse laser and to the sample；The delay time generator is connected with the laser and the spectrometer respectively, for according to default delay time, being triggered to the spectrometer collection signal；The spectrometer is connected with the optical fiber and the computer respectively, for collecting the plasma optical signal that the sample sends by optical fiber.The present invention provides a kind of analysis system and method for the LIBS related based on two-dimentional energy, conventional LIBS is launched on laser energy yardstick, so as to more clearly visible parse spectral signature, the detectability and repeatability of conventional laser-induced breakdown spectral method are improved.
Description
Technical field
The present invention relates to technical field of analytical chemistry, more particularly to a kind of LIBS analysis system and side
Method.
Background technology
LIBS is a kind of new spectrographic detection means, and its principle is to utilize strong laser irradiation sample,
It is excited to plasma state, then the emission spectrum of plasma state is collected with spectrometer, so that the element in analyzing sample contains
Amount.In recent years, LIBS is applied to micro in steel, coal dust, mural painting, soil, timber equal samples
Element is measured.
At present, laser is needed to be punctured to obtain plasma state to sample in the measurements due to LIBS
Spectrum, the problems such as energy of lasers shake, sample surface inhomogeneities, plasma plume diffusion instability under the influence of,
The stability of LIBS measurement is very poor, causes many problems in quantification metering.It is existing to be hit in induced with laser
Wear in the measurement of spectrum, employ many methods for improving stability and repeatability.Such as repeatedly measurement is averaged or is utilized
Ionic state parameter is modified to spectrum.
However, these methods can improve measurement reproducibility, but it is not high to improve degree.Additionally, LIBS
Another problem is that its detectability is not high, on the one hand, some weaker element energy jump spectral lines are difficult to be identified, the opposing party
Face, some spectral lines are narrower, it is easy to together with other overlaps of spectral lines, cause to recognize mistake.
The content of the invention
The present invention in view of the shortcomings of the prior art, proposes a kind of analysis method and system of LIBS, can
More clearly visible to parse spectral signature, the detectability and repeatability of conventional laser-induced breakdown spectral method are improved.
In a first aspect, the present invention provides a kind of analysis system of two-dimentional energy associated laser induced breakdown spectroscopy, including：Swash
Light device, spectrometer, delay time generator, optical fiber, sample and computer；The laser, swashs for periodically launching pulse
Light is simultaneously impacted to the sample；The delay time generator is connected with the laser and the spectrometer respectively, for root
According to default delay time, the spectrometer collection signal is triggered；The spectrometer respectively with the optical fiber and described
Computer is connected, for collecting the plasma optical signal that the sample sends by optical fiber.
Preferably, the delay time generator is the picosecond accurate delay system controlled using FPGA.
Preferably, the system also includes：Converging device, the converging device is connected with the optical fiber, for converging
The plasma optical signal that sample sends is stated, and the spectrometer is delivered to through optical fiber.
Preferably, the converging device is the card Sa Gelin systems for being placed in the optical fiber front end.
Preferably, the system also includes：Beam splitter, the beam splitter is placed at the laser emitting position, is used for
10% pulsed laser energy that the laser is launched is reflexed on photodiode.
Second aspect, the present invention provides a kind of analysis method of two-dimentional energy associated laser induced breakdown spectroscopy, including：
Spectrometer is measured to the dark background for not placing sample, obtains background spectrum, and deduct the background spectrum
Interference and this bulk noise；
Spectral measurement is carried out under energy perturbation state, by increasing the laser energy that laser is launched, the sample is obtained
This one-dimensional spectrum under breakdown conditions；
The exact numerical of laser energy is obtained, laser power calibration is carried out to the one-dimensional spectrum according to the exact numerical
And normalized；
Two-dimensional correlation spectra is calculated according to one-dimensional spectrum, the two-dimensional correlation spectra includes：Synchronous correlation spectrum and asynchronous
Correlation spectrum；
Separate the self correlated peak in two-dimensional correlation spectra, intersect peak, and it is corresponding with one-dimensional spectrum.
Preferably, the exact numerical for obtaining laser energy, is carried out according to the exact numerical to the one-dimensional spectrum
Laser power calibration and normalized, including：
Photodiode receives the laser energy of beam splitter feedback, and measures laser energy in real time；
Corresponding coefficient is multiplied by original spectrum according to deviation, and compensates the deviation of the laser energy；
The spectroscopic data with 50nm as window is recorded, to carrying out area normalization in window each described.
Preferably, it is described that spectral measurement is carried out under energy perturbation state, by increasing the laser energy that laser is launched,
The sample one-dimensional spectrum under breakdown conditions is obtained, including：
When impacting first, with basal energy as 100-200mJ, frequency impacts institute to the laser for the laser pulse of 10HZ
State sample；
After impacting first, increase by 5% basal energy impact sample every time, to obtain the spectroscopic data of gradual change.
Preferably, the synchronous correlation spectrum calculated according to one-dimensional spectrum in two-dimensional correlation spectra, including：
The synchronous correlation spectrum is calculated according to formula one：
Formula one
Wherein, SmaxIt is the spectral intensity maximum of the spectrometer collection, SminFor the spectrum of the spectrometer collection is strong
Degree minimum value, yj(υ1) and yj(υ2) it is the spectra values of different-waveband.
Preferably, the asynchronous correlation spectrum calculated according to one-dimensional spectrum in two-dimensional correlation spectra, including：
The asynchronous correlation spectrum is calculated according to formula two：
Formula two
Wherein, SmaxIt is the spectral intensity maximum of the spectrometer collection, SminFor the spectrum of the spectrometer collection is strong
Degree minimum value, yj(υ1) and yk (υ2) it is the spectra values of different-waveband.
The present invention provides a kind of analysis system and method for the LIBS related based on two-dimentional energy, can
Obtain with the two-dimensional correlation spectra of the LIBS that laser energy is disturbance, relative to one-dimensional spectrum, can be more
Accurately realize qualitative and quantitative determination.Can reveal that different peak values, peak position with laser energy variation relation, so as to realize
The reinforcing and feature extraction of some weak peak signals, can more clearly visible parse spectral signature, and raising is conventional laser-induced to puncture light
The detectability and repeatability of spectral method.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
The accompanying drawing to be used needed for having technology description is briefly described, it should be apparent that, drawings in the following description are only this
Some embodiments of invention, for those of ordinary skill in the art, on the premise of not paying creative work, can be with
Other accompanying drawings are obtained according to these accompanying drawings.
Fig. 1 is that the structure of the analysis system of two-dimentional energy associated laser induced breakdown spectroscopy provided in an embodiment of the present invention is shown
It is intended to；
Fig. 2 is that the flow of the analysis method of two-dimentional energy associated laser induced breakdown spectroscopy provided in an embodiment of the present invention is shown
It is intended to；
Fig. 3 is the part stream of the analysis method of two-dimentional energy associated laser induced breakdown spectroscopy provided in an embodiment of the present invention
Journey schematic diagram；
Fig. 4 is the main-process stream of the analysis method of two-dimentional energy associated laser induced breakdown spectroscopy provided in an embodiment of the present invention
Schematic diagram.
Reference：
1st, laser；2nd, spectrometer；3rd, delay time generator；4th, optical fiber；5th, sample；6th, computer.
Specific embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments, is based on
Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under the premise of creative work is not made
Embodiment, belongs to the scope of protection of the invention.
Fig. 1 shows the analysis system of two-dimentional energy associated laser induced breakdown spectroscopy provided in an embodiment of the present invention, such as
Shown in Fig. 1, the analysis system of the two-dimentional energy associated laser induced breakdown spectroscopy of the present embodiment, including：Laser 1, spectrometer
2nd, delay time generator 3, optical fiber 4, sample 5 and computer 6；Wherein, delay time generator 3 connects with laser 1 and spectrometer 2 respectively
Connect, spectrometer 2 is connected with optical fiber 4 and 6 machines of calculating respectively,
In the present embodiment, laser 1 is used to periodically emission pulse laser and impact sample 5, and sample 5 can be with
It is steel, coal dust, mural painting, soil or timber etc., the pulse energy of laser 1 is 100-200mJ, and beating frequency is 10hz, excellent
Choosing, the basal energy that laser 1 impacts sample first is 150mJ, and hereafter, laser increases by 5% energy steadily every time, order
Impact sample 5, delay time generator 2 is used for according to default delay time, and the collection signal of spectrometer 2 is triggered, wherein, often
The delay time of secondary triggering is consistent with first time, due to that can first appear as continuous spectrum, therefore this reality after laser breakdown sample 5
Picosecond accurate delay system of the delay time generator 3 in example using FPGA controls is applied, and the collection signal of spectrometer 2 is touched
Hair, to ensure to obtain the strict spectroscopic data of sequential.
It should be noted that default delay time is 2 μ s in the present embodiment, but 2 μ s are not only limited to, in practice
In, can sets itself as needed.
Further, the spectrometer 2 in the present embodiment is used to collect the plasma light letter that sample 5 sends by optical fiber 4
Number, before sample 5 is measured, spectrometer 2 background correction should be disturbed and this bulk noise first, so that it will be accurate spectrum to obtain
Information.Therefore, measured with 2 pairs of dark backgrounds for not placing sample 5 of spectrometer, obtain background spectrum, be to demarcate foundation with it.
In another embodiment, the system also includes the converging device not shown in figure, converging device and optical fiber 4
Connection, for converging the plasma optical signal that sample 5 sends, and is delivered to spectrometer 2, alternatively, converging device through optical fiber 4
To be arranged at the card Sa Gelin systems of the front end of the optical fiber 4, it is hereby achieved that high-throughout optical signalling.
In the present embodiment, due to the problems such as laser 1 is inevitably present energy to be shaken, influencing whether the correlation of spectrum
Property analysis.Therefore, the present embodiment also includes the beam splitter not shown in figure, and beam splitter is placed in the exit position of laser 1, through dividing
, for impacting sample, a part is for feeding back for a laser part after beam device beam splitting
For example, beam splitter can be incident with 45° angle, using 10:90 spectroscopes, the pulse laser that laser 1 sends is tight
Lattice are according to 10:90 90% light energies of transmission, reflect 10% light energy, and the basal energy sent in laser 1 is the situation of 150mJ
Under, energy of reflection light is 15mJ, and energy of reflection light enters Energy detection block for 15mJ, and Energy detection block can be accurately detected
Beam splitter branches away the light energy i.e. energy of light pulse 1/10th, it is preferable that the Energy detection block in the present embodiment is to set
The photodiode at feedback laser beam position is put, photodiode can in real time measure laser energy, so as to strong to spectrum
Degree is modified.
Specifically, the pulsed laser energy of photodiode measurement 10% and using the logical computer 6 that is transmitted to of energy value as returning
One changes standard value, and the spectrum that laser induced plasma gives off is collected by optical fiber 4, is coupled in spectrometer 2 by optical fiber 4,
Spectral analysis data is transmitted to computer 6 by interface circuit.
In a particular application, spectroscopic data after acquisition, it is necessary to pre-processed to it, to eliminate making an uproar in measurement process
The erratic behavior problem that sound causes.First, laser energy deviation is compensated, correspondence is multiplied by original spectrum according to deviation
Coefficient.Secondly, institute's spectra re-recorded data carry out area normalization with 50nm as window in each window.I.e. per 50nm scopes
It is interior, the area of spectroscopic data is classified as 1, hereafter, the self correlated peak in two-dimensional correlation spectra can be separated and intersect peak.Auto-correlation
Peak and intersection peak indicate each spectral signature with the increased Changing Pattern of laser energy.With reference to the feature peak position of original spectrum
Put, obtain the correlation of each spectral signature change, and then separate the overlap peak being closer to, and relatively fainter spectrum
Peak.
The present embodiment is obtained in that with the two-dimensional correlation spectra of the LIBS that laser energy is disturbance.Relatively
In one-dimensional spectrum, qualitative and quantitative determination more can be accurately realized.Can reveal that different peak values, peak position with laser energy
Variation relation, so as to realize the reinforcing and feature extraction of some weak peak signals.
Fig. 2 shows the flow of two-dimentional energy associated laser induced breakdown spectroscopy analysis method provided in an embodiment of the present invention
Schematic diagram, as shown in Fig. 2 the two-dimentional energy associated laser induced breakdown spectroscopy analysis method of the present embodiment is as described below.
201st, spectrometer is measured to the dark background for not placing sample, obtains background spectrum, and deduct the bias light
The interference of spectrum and this bulk noise.
In the present embodiment, the background of spectrometer is gathered, and deduct baseline and dark current influence, rung with obtaining stable spectrum
Answer data.Specifically, before sample is measured, in order to obtain more accurate spectral information, spectrometer should background correction first
Interference and this bulk noise, therefore, the dark background for not placing sample is measured with spectrometer first, background spectrum is obtained, and
It is to demarcate foundation with it.
202nd, spectral measurement is carried out under energy perturbation state, by increasing the laser energy that laser is launched, institute is obtained
State sample one-dimensional spectrum under breakdown conditions.
For example, it is 100-200mJ that laser uses basal energy, and frequency is hit for the laser beam of 10hz to sample
Beat, then increase by 5% energy steadily every time and puncture sample, obtain the spectroscopic data of gradual change.I.e. by increasing laser energy steadily, obtain
Sample one-dimensional spectrum under breakdown conditions is obtained, to carry out the spectral measurement under energy perturbation state.
203rd, the exact numerical of laser energy is obtained, laser power is carried out to the one-dimensional spectrum according to the exact numerical
Calibration and normalized.
In the present embodiment, the exact numerical of laser energy is obtained using the method for feedback measurement, and use multiwindow area
The methods such as normalization improve the measurement stability and repeatability of spectrum, it is can be used for two-dimensional correlation spectra and calculate.
204th, two-dimensional correlation spectra is calculated according to the one-dimensional spectrum, the two-dimensional correlation spectra includes：Synchronous correlation light
Spectrum and asynchronous correlation spectrum.
205th, separate the self correlated peak in two-dimensional correlation spectra, intersect peak, and it is corresponding with one-dimensional spectrum.
It should be noted that self correlated peak and intersection peak indicate each spectral signature with the increased change rule of laser energy
Rule.With reference to the characteristic peak positions of original spectrum, the correlation of each spectral signature change is obtained, and then can separate and be closer to
Overlap peak, and relatively faint spectrum peak.
In step 204, the synchronous correlation spectrum is calculated according to formula one：
Formula one
Wherein, SmaxIt is the spectral intensity maximum of the spectrometer collection, SminFor the spectrum of the spectrometer collection is strong
Degree minimum value, yj(υ1) and yj(υ2) it is the spectra values of different-waveband.
The asynchronous correlation spectrum is calculated according to formula two：
Formula two
Wherein, SmaxIt is the spectral intensity maximum of the spectrometer collection, SminFor the spectrum of the spectrometer collection is strong
Degree minimum value, yj(υ1) and yk (υ2) it is the spectra values of different-waveband.
The method of the present embodiment can be obtained with the two-dimensional laser induced breakdown spectroscopy that energy of lasers is disturbance, realized normal
Expansion of the rule LIBS in energy scale.On the one hand, laser shake is effectively eliminated to spectral measurement repeatability
Influence；On the other hand, some weak peaks and overlap peak can be recognized by the auto-correlation information of spectral line, improves laser-induced breakdown
The detectability of spectrum.
Fig. 3 shows the part of two-dimentional energy associated laser induced breakdown spectroscopy analysis method provided in an embodiment of the present invention
Schematic flow sheet, specifically, Fig. 3 shows the schematic flow sheet of step 203 in Fig. 2, as shown in figure 3, step 203 is specifically wrapped
Include：
2031st, photodiode receives the laser energy of beam splitter feedback, and measures laser energy in real time.
In the present embodiment, the light energy of beam splitter reflection 10%, energy of reflection light enters photodiode, photodiode energy
It is accurately detected beam splitter and branches away light energy, it is possible to measure laser energy in real time, so as to is modified to spectral intensity.
2032nd, corresponding coefficient is multiplied by original spectrum according to deviation, and compensates the deviation of the laser energy.
For example, spectroscopic data is drawn, it is necessary to pre-processed to it after acquisition with the noise eliminated in measurement process
The erratic behavior problem for rising.First, laser energy deviation is compensated, corresponding system is multiplied by original spectrum according to deviation
Number.
2033rd, the spectroscopic data with 50nm as window is recorded, to carrying out area normalization in window each described.
It is understood that in the range of i.e. per 50nm, the area of spectroscopic data is classified as into 1.
The present embodiment is punctured using the laser of graded energy to sample, then plasma spectrometry to puncturing acquisition enters
Row treatment, is disturbance with the laser energy of gradual change, calculates two-dimensional correlation laser spectrum, to obtain the laser launched in energy dimension
Induced breakdown spectroscopy.
Fig. 4 shows the flow of two-dimentional energy associated laser induced breakdown spectroscopy analysis method provided in an embodiment of the present invention
Schematic diagram, as shown in figure 4, the two-dimentional energy associated laser induced breakdown spectroscopy analysis method of the present embodiment is as described below.
401st, spectrometer background spectrum collection, spectrum dark background is deducted.
In the present embodiment, by gathering the background of spectrometer, baseline and dark current influence are deducted, to obtain stable spectrum
Response data.
402nd, laser is set sample, spectra re-recorded data is punctured with basal energy.
For example, laser punctures sample with the basal energy of 100-200mJ first.
403rd, laser increases by 5% energy steadily every time, punctures sample, spectra re-recorded data.
It is understood that by increasing laser energy steadily, obtaining sample breakdown conditions in laser energy situation of change
Under one-dimensional spectrum, the spectral measurement under energy perturbation state can be carried out.
404th, accurate laser energy is obtained by installing the method for photodiode after beam splitter.
It should be noted that because laser unavoidably has energy, influencing whether the correlation of spectrum
Analysis.Therefore, the present invention installs beam splitter in laser emitting position, and the laser part after beam splitting is being fed back for feeding back
Laser beam position installs photodiode.Diode measures laser energy in real time, so as to be modified to spectral intensity.
405th, institute's spectra re-recorded data carry out area normalization with 50nm as window in each window.
In the present embodiment, laser energy deviation is compensated, i.e., corresponding system is multiplied by original spectrum according to deviation
Number.Secondly, institute's spectra re-recorded data carry out area normalization with 50nm as window in each window.In the range of i.e. per 50nm, will
The area of spectroscopic data is classified as 1, the erratic behavior problem caused with the noise eliminated in measurement process.
406th, two dimension synchronization correlation spectrum is calculated.
In the present embodiment, the synchronous correlation spectrum is calculated according to formula one：
Formula one
Wherein, SmaxIt is the spectral intensity maximum of the spectrometer collection, SminFor the spectrum of the spectrometer collection is strong
Degree minimum value, yj(υ1) and yj(υ2) it is the spectra values of different-waveband.
407th, two-dimentional asynchronous correlation spectrum is calculated.
In the present embodiment, the asynchronous correlation spectrum is calculated according to formula two：
Formula two
Wherein, SmaxIt is the spectral intensity maximum of the spectrometer collection, SminFor the spectrum of the spectrometer collection is strong
Degree minimum value, yj(υ1) and yk (υ2) it is the spectra values of different-waveband.
408th, separate the self correlated peak in two-dimensional correlation spectra, intersect peak, and it is corresponding with one-dimensional spectrum.
It should be noted that self correlated peak and intersection peak indicate each spectral signature with the increased change rule of laser energy
Rule.With reference to the characteristic peak positions of original spectrum, the correlation of each spectral signature change is obtained, and then can separate and be closer to
Overlap peak and the faint spectrum peak of comparing.
It should be noted that the analysis system of the two-dimentional energy associated laser induced breakdown spectroscopy in the embodiment of the present invention can be held
Whole flows in row Fig. 2 to Fig. 4 methods, no longer describe in detail herein.
The method of the present embodiment can be used for LIBS measurement, micronutrient levels measurement, steel such as in coal dust
Elemental purity measurement, composition measurement of aerosol etc. in iron, cut down the error that energy of lasers shake is caused to a certain extent,
And improve the detectability of weak peak and overlap peak.
Obviously, those skilled in the art can carry out various changes and modification without deviating from essence of the invention to the present invention
God and scope.So, if these modifications of the invention and modification belong to the scope of the claims in the present invention and equivalent technologies
Within, then the present invention is also intended to comprising these changes and modification.
Claims (5)
1. a kind of analysis method of two-dimentional energy associated laser induced breakdown spectroscopy, it is characterised in that including：
Spectrometer is measured to the dark background for not placing sample, obtains background spectrum, and deduct the interference of the background spectrum
With this bulk noise；
Spectral measurement is carried out under energy perturbation state, by increasing the laser energy that laser is launched, the sample is obtained and is existed
One-dimensional spectrum under breakdown conditions；
The exact numerical of laser energy is obtained, laser power calibration is carried out to the one-dimensional spectrum according to the exact numerical and is returned
One change is processed；
Two-dimensional correlation spectra is calculated according to the one-dimensional spectrum, the two-dimensional correlation spectra includes：Synchronous correlation spectrum and asynchronous
Correlation spectrum；
Separate the self correlated peak in two-dimensional correlation spectra, intersect peak, and it is corresponding with one-dimensional spectrum.
2. method according to claim 1, it is characterised in that the exact numerical of the acquisition laser energy, according to described
Exact numerical carries out laser power calibration and normalized to the one-dimensional spectrum, including：
Photodiode receives the laser energy of beam splitter feedback, and measures laser energy in real time；
Corresponding coefficient is multiplied by original spectrum according to deviation, and compensates the deviation of the laser energy；
Recorded by the spectroscopic data after laser energy deviation compensation by window of 50nm, to carrying out area in window each described
Normalization.
3. method according to claim 1, it is characterised in that described that spectral measurement is carried out under energy perturbation state, leads to
The laser energy for increasing laser transmitting is crossed, the sample one-dimensional spectrum under breakdown conditions is obtained, including：
When impacting first, with basal energy as 100-200mJ, frequency impacts the sample to the laser for the laser pulse of 10HZ
This；
After impacting first, increase by 5% basal energy impact sample every time, to obtain the spectroscopic data of gradual change.
4. method according to claim 1, it is characterised in that described that two-dimensional correlation spectra calculated according to one-dimensional spectrum
Synchronous correlation spectrum, including：
The synchronous correlation spectrum is calculated according to formula one：
Wherein, SmaxIt is the spectral intensity maximum of the spectrometer collection, SminFor the spectrometer collection spectral intensity most
Small value, yj(υ1) and yj(υ2) it is the spectra values of different-waveband.
5. method according to claim 1, it is characterised in that described that two-dimensional correlation spectra calculated according to one-dimensional spectrum
Asynchronous correlation spectrum, including：
The asynchronous correlation spectrum is calculated according to formula two：
Wherein, SmaxIt is the spectral intensity maximum of the spectrometer collection, SminFor the spectrometer collection spectral intensity most
Small value, yj(υ1) and yk(υ2) it is the spectra values of different-waveband.
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| CN108020540B (en) * | 2017-12-11 | 2020-10-20 | 中国科学院光电研究院 | Laser-induced breakdown spectroscopy detection system |
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| CN111257305B (en) * | 2020-03-31 | 2023-06-27 | 北京农业智能装备技术研究中心 | Two-dimensional correlation LIBS spectrum measurement method, system and device |
| CN112255460A (en) * | 2020-10-27 | 2021-01-22 | 天津市英贝特航天科技有限公司 | Method and device for eliminating signal noise of conductivity analyzer |
| CN114813709B (en) * | 2022-06-28 | 2022-10-04 | 华谱智能科技(天津)有限公司 | Soil component detection method, equipment and system |
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| CN104007090A (en) * | 2014-05-27 | 2014-08-27 | 四川大学 | Portable elementary composition analysis device based on laser-induced breakdown spectroscopy technology |
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