CN103175808B - Laser-induced breakdown spectroscopy analysis system and laser-induced breakdown spectroscopy analysis method - Google Patents
Laser-induced breakdown spectroscopy analysis system and laser-induced breakdown spectroscopy analysis method Download PDFInfo
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- CN103175808B CN103175808B CN201310082225.1A CN201310082225A CN103175808B CN 103175808 B CN103175808 B CN 103175808B CN 201310082225 A CN201310082225 A CN 201310082225A CN 103175808 B CN103175808 B CN 103175808B
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Abstract
The invention provides a laser-induced breakdown spectroscopy analysis system which comprises a control unit, a pulse laser, a beam splitter, a movable positioning platform, a spectrum collecting unit, a spectrograph and a data processing system, wherein the beam splitter, the movable positioning platform, the spectrum collecting unit, the spectrograph and the data processing system are sequentially arranged along the emitted direction of pulse lasers; the beam splitter splits the emitted light pulse of the pulsed laser into a main light path and a sampling light path; the main light path is provided with a laser beam expanding-collimating and focusing optical system and a sample positioning unit which forms a feedback control with the movable positioning platform; the sampling light path is provided with a pulse laser energy measurement module and a pulse trigger delay unit; the control unit outputs multiple control signals; the control signal output ends of the control unit are respectively correspondingly connected to the sample positioning unit; and the data output end of the spectrograph is connected to the data processing system.
Description
Technical field
The present invention relates to a kind of device for component qualitative elementary and quantitative test.
Background technology
Along with the fast development of laser technology, people are to material trace element the improving constantly of understanding demand, and Laser-induced Breakdown Spectroscopy (Laser-induced Breakdown Spectroscopy is called for short LIBS) technology becomes in recent years and receives much concern and a kind of Atomic Emission Spectral Analysis new technology based on Reciprocity of Laser & Materials developed rapidly.Carry out light splitting and detection by the plasma light spectrum signal produced in sample surfaces low-yield narrow spaces pulse laser focusing, obtain the information of element in testing sample, the element of final calculation sample quantitative and qualitative analysis.This technology possesses following advantage: less demanding to sample surfaces, and not by restrictions such as material type, surface topography, state, electric conductivity, generally do not need pre-treatment, sample loss is little, and response rapidly, can realize multielement express-analysis simultaneously; Have the advantages that noncontact is analyzed, be easy to remote sensing and control, can be used for remote on-line quick detection LIBS and be widely used in the industry such as iron and steel, coloured, coal, geology, archaeology, environment.
But up to now, this technology still rests on Theoretical Design aspect, domesticly not yet LIBS technology can be put into practice, external or have development device, but only can realize qualitatively judging, do not possess the function of quantitative test.
Summary of the invention
The invention provides a kind of Laser-induced Breakdown Spectroscopy analytic system, to realize component and the content thereof of qualitative and quantitative analysis sample.
For realizing above goal of the invention, the present invention provides following basic technical scheme:
Laser-induced Breakdown Spectroscopy analytic system, comprises control module, pulsed laser and the beam splitter set gradually along pulse laser exit direction, in order to place the removable locating platform of testing sample, spectral collection unit, spectrometer and data handling system, the emergent light pulse of pulsed laser is separated main optical path and sampling light path according to the energy distribution ratio of setting by described beam splitter, main optical path is disposed with laser bundle-enlarging collimation and Focused Optical system, the Sample location unit of FEEDBACK CONTROL is formed with described removable locating platform, sampling light path is respectively arranged with pulsed laser energy measurement module, trigger action delay cell, wherein, the signal output part of pulsed laser energy measurement module is connected to the first input end of control module, trigger action delay cell is successively by trigger pip generation unit, delay control circuit square-wave signal exports the second input end being connected to control module, the signal output part of described twin-beam Sample location unit is connected to the 3rd input end of control module, control module has multi-way control signals and exports, and each control signal output terminal respectively correspondence is connected to Sample location unit, removable locating platform, spectrometer, the data output end of spectrometer is connected to data handling system.
Based on above-mentioned basic technical scheme, the present invention can also do following optimization and limit and improve:
Above-mentioned Sample location unit comprises twin-beam light-source system and camera, and the two bundle laser that twin-beam light-source system sends are symmetrical and be radiated at testing sample surface with fixed angle with the optical axis of described main optical path; Camera, for taking the hot spot on testing sample surface, forms FEEDBACK CONTROL with removable locating platform.When experimental situation illumination is lower, also can LED illumination lamp be set.Twin-beam Sample location cell operation pattern can be: twin-beam light-source system is energized, and LED is energized, and camera is energized, and removable locating platform starts; The power cut-off of twin-beam Sample location unit, twin-beam power-off, LED power-off, camera stops taking pictures, and removable locating platform is closed.
Above-mentioned spectral collection unit is connected to spectrometer by coupling fiber, the concrete preferably Cassegrain telescope of spectral collection unit.Laser excitation spectrum out with 2 π solid angles to external expansion, in order to obtain spectral information better, therefore adopt optical fiber as receiving-member (only slightly need make conventional accommodation to Cassegrain telescope), then the light signal input spectrum instrument received is carried out photoelectric conversion.
Above-mentioned trigger action delay cell receives the diffuse reflection from pulsed laser energy measurement module light entrance face.Laser beam detects light and is entered trigger action delay cell by the diffuse reflection of pulsed laser energy measurement module after beam splitter, exports square-wave signal, is used for triggering spectrometer collection spectrum.
Above-mentioned Sample location unit is fixedly installed on main optical path all the time, overall symmetrical with the optical axis of main optical path, and Sample location unit fixed head center drilling, its structure ensures the laser beam after laser bundle-enlarging collimation and Focused Optical system without impact.Certainly, also can remove this Sample location unit before pulsed laser is started working, such Sample location unit is also just without requiring unscreened structure.
The plane of incidence and the primary optical axis angle of above-mentioned beam splitter are preferably set to 45 °.
The outside of above-mentioned removable locating platform is also provided with light shield, can prevent ambient light from disturbing like this, is also convenient to stay certain access port to spectral collection unit simultaneously, allows electric three-dimensional pan carriage external circuit conveniently leave interface.
Operation wavelength preferred 1064nm, 532nm or 256nm of above-mentioned pulsed laser, pulse energy 80-120 MJ, pulse width 6-9 nanosecond; Described beam splitter adopts 10:90 spectroscope, and namely pulse laser reflects 10% luminous energy through this beam splitter transmission 90% luminous energy.
The course of work of the present invention mainly comprises the following steps:
(1) testing sample position is adjusted
Sample location cell operation, testing sample surface is radiated at fixed angle with the axisymmetric two bundle laser of key light, Sample location unit fixed head center drilling, its structure ensures the Laser beam propagation after laser bundle-enlarging collimation and Focused Optical system without impact, the hot spot of every light beam on testing sample surface is taken respectively with camera, control module gathers gained hot spot picture and draws the coordinate of facula mass center in picture by software process, calculate the distance between two facula mass centers, judge within the scope of the focal plane position whether testing sample surface is in described laser bundle-enlarging collimation and Focused Optical system or Rayleigh range.
If so, then control module controls camera and stops taking pictures, and calculates facula area and optical density, and sends trigger pip pulsed laser is started working;
If not, then control module calculates the vertical range of the focal plane position of testing sample surface and laser bundle-enlarging collimation and Focused Optical system further, then controls removable locating platform and moves, and drives testing sample surface to focal plane position; Confirm that testing sample surface arrives within the scope of focal plane position or Rayleigh range, control module controls camera to be stopped taking pictures, and calculates facula area and optical density, and sends trigger pip pulsed laser is started working.
(2) spectrum is obtained
The spectrum that pulse laser inspires on testing sample to external expansion with 2 π solid angles, adopts Cassegrain telescope to receive, and by optical fiber, the light signal input spectrum instrument received is carried out photoelectric conversion.
(3) conclusion is analyzed
The measurement data exported by spectrometer imports data handling system, comes component and the content thereof of this testing sample of qualitative and quantitative analysis based on the wavelength in measurement data and intensity corresponding relation.
The present invention has the following advantages:
Present invention employs a kind of new method for multielement component sample composition qualitative elementary with determine quantitative analysis.
Structure of the present invention is simple and clear, easy to operate, can realize component and content thereof that quantitative and qualitative analysis determines this sample.
In the present invention, Sample location unit accurately can ensure that sample surfaces is positioned at lens combination focal plane position, the pulsed laser work of control module trigging control and spectrum acquisition, and can record every state parameter, guarantees test data real-time and accuracy.
Accompanying drawing explanation
Fig. 1 is light channel structure schematic diagram of the present invention.
In figure: 1-pulsed laser, 2-beam splitter, 3-pulsed laser energy measurement module, 4-pulse signal detection and trigger delays, 5-laser bundle-enlarging collimation and Focused Optical system, 6-twin-beam Sample location unit, 7-sample chamber, 8-spectral collection unit, 9-spectrometer, 10-data handling system.
Fig. 2 is the schematic diagram of the Laser-induced Breakdown Spectroscopy analytic system of the embodiment of the present invention.
Fig. 3 is twin-beam Sample location unit fixed disc upward view, and center hole leads to light.
In figure: 11-first laser beam source, 12-second laser beam source, 13-LED light source, 14,15 two holes are used for fixing camera pedestal.
Fig. 4 is twin-beam Sample location light path schematic diagram.
In figure: 601-LD light source first light path, 602-LD light source second light path, 603-camera imaging optical system; 604-CCD; 605-main optical path optical axis.
Fig. 5 is the workflow diagram of twin-beam positioning unit.
Fig. 6 is the flow process of quantitative test single element.
Embodiment
A kind of Laser-induced Breakdown Spectroscopy analytic system that this embodiment provides, comprises pulsed laser 1, beam splitter 2, pulsed laser energy measurement module 3, trigger action delay cell 4, laser bundle-enlarging collimation and Focused Optical system 5, twin-beam Sample location unit 6, sample chamber 7, spectral collection unit (Cassegrain telescope) 8, spectrometer 9, data handling system 10 etc.
Pulsed laser specific requirement: pulse request wavelength 1064nm, pulse energy 100mJ, pulse width 7ns, external power supply gating pulse energy, configuration refrigeration unit.
Beam splitter requires 45 ° of incidences, can adopt 10:90 spectroscope, and 1064nm pulse laser reflects 10% luminous energy in strict accordance with 10:90 transmission 90% luminous energy.Energy of reflection light 10mJ enters Energy detection block.Pulsed laser energy measurement module can be accurately detected beam splitter and branch away luminous energy (i.e. the energy of light pulse 1/10th).
Trigger action delay cell detects from luminous energy measurement module diffuse reflection light signal out, then provides a square wave inhibit signal, then is triggered to spectrometer collection signal by trigger delays control lag time signaling.
Twin-beam Sample location unit requires: with axisymmetric two bundles laser (instruction collimated light beam) of key light to be radiated at sample surfaces with optical axis included angle 17 °, the hot spot of every light beam at sample surfaces is taken respectively with 20 ° with camera, drawn the vertical range of sample and optical system focal plane position by software process picture, then control D translation frame by control module and move to the direction of correspondence thus drive sample to move to focal plane position.Confirmatory sample surface exports a signal to pulsed laser power supply after arriving focal plane position, is that pulsed laser sends pulse laser.
Sample chamber can prevent ambient light from disturbing, and stays certain entrance to spectral collection unit, leaves interface to electric three-dimensional pan carriage external circuit.
Spectrometer spectral range 200nm ~ 900nm, to the strength sensitive of spectrum, accurately.Need during quantitative sample element to demarcate, the time starting to collect data is determined in strict accordance with pulse signal detection and delay units delay time.
Realize the parameter that quantitative test may relate to: laser power density after laser instrument self output wavelength, output pulse energy, pulse width, optical system focal length, focusing, done the corresponding relation of wavelength and the receiving spectrum determined by receiving system and spectrometer.In addition for the purpose of quantitative test more accurately, the indoor stable neighbourhood noise of all right collected specimens, as calculating parameter.
Control module coordinates whole collection spectroscopy procedure.By twin-beam Sample location unit 6, sample surfaces is adjusted to pulse laser focal plane position, power supply starts to export predetermined voltage, 1064nm pulsed laser 1 sends laser pulse through energy beam splitter 2, sub-fraction luminous energy enters pulsed laser energy measurement module 3 and obtains energy datum as carrying out the luminous energy of LIBS with reference to calculated value, enter pulse signal by the irreflexive light of measurement module to detect and trigger delays 4, carry out detection trigger pip and be given to control module.Rest light energy by laser beam expanding, collimate, focus in sample chamber testing sample surface, sample produces plasma exciatiaon process under light laser energy exposure, outwards launch with 2 π solid angles, in the process sample element produce characteristic spectral line by Cassegrain telescope receive laggard enter spectrometer generate spectroscopic data.Element and the content of sample is finally obtained through a series of data processing.
Line strength formula that actual measurement obtains is as follows:
F is instrument receiving efficiency, C
xbe the content of particle x in plasma, Amn is the spontaneous transition probability from m energy level transition to n energy level, g
mthe statistical weight of m energy level, E
mthe excitation energy of m energy level, k
brepresent Boltzmann constant, T is plasma temperature, U
x(T) be the partition function of particle x under temperature T.
From the plasma light spectral curve of entire scan, first select the spectral line paid close attention to, again measure the intensity of this spectral line, read centre wavelength and the intensity of every bar line simultaneously.According to the electron temperature (T) of the relative intensity of spectral line and described formula estimation plasma above, according to the Stark broadening estimation plasma electron density (n of spectral line
e), according to electron temperature T and electron density n
ethe concentration C of often kind of element in estimation sample
xand spectral bandwidth L.Then loop iteration and adjustment is adopted, start iteration, a region is regarded as below each crest envelope, calculating plasma chemical composition, then absorption coefficient is calculated, then spectral radiance is calculated, whether the spectrum that judgement calculates and measure spectrum are distinguished minimum from light intensity and waveform, if not, so adjust electron density, electron temperature, the parameters such as the relative content of wavelength pulsewidth and each element calculate again, if difference is minimum, but it is larger than the threshold value set before, so, crest envelope region is separated a part, then electron density is adjusted, electron temperature, the parameters such as the relative content of wavelength pulsewidth and each element calculate and the threshold value of setting before being less than again, so calculate end, finally determine sample composition element and corresponding content.
Claims (8)
1. Laser-induced Breakdown Spectroscopy analytic system, is characterized in that: comprise control module, pulsed laser and the beam splitter set gradually along pulse laser exit direction, in order to place the removable locating platform of testing sample, spectral collection unit, spectrometer and data handling system, the emergent light pulse of pulsed laser is separated main optical path and sampling light path according to the energy distribution ratio of setting by described beam splitter, main optical path is disposed with laser bundle-enlarging collimation and Focused Optical system, the Sample location unit of FEEDBACK CONTROL is formed with described removable locating platform, sampling light path is respectively arranged with pulsed laser energy measurement module, Pulse-trigger control unit, wherein, the signal output part of pulsed laser energy measurement module is connected to the first input end of control module, trigger action delay cell is successively by trigger pip generation unit, delay control circuit square-wave signal exports the second input end being connected to control module, the signal output part of described Sample location unit is connected to the 3rd input end of control module, control module has multi-way control signals and exports, and each control signal output terminal respectively correspondence is connected to Sample location unit, removable locating platform, spectrometer, the data output end of spectrometer is connected to data handling system,
Described Sample location unit comprises twin-beam light-source system and camera, and the two bundle laser that twin-beam light-source system sends are symmetrical and be radiated at testing sample surface with fixed angle with the optical axis of described main optical path; Camera, for taking the hot spot on testing sample surface, forms FEEDBACK CONTROL with removable locating platform.
2. Laser-induced Breakdown Spectroscopy analytic system according to claim 1, is characterized in that:
Described spectral collection unit is connected to spectrometer by coupling fiber, and spectral collection unit adopts Cassegrain telescope.
3. Laser-induced Breakdown Spectroscopy analytic system according to claim 1, is characterized in that:
Described trigger action delay cell receives and diffuses from pulsed laser energy measurement module, and provides the square-wave signal of adjustable delay.
4. Laser-induced Breakdown Spectroscopy analytic system according to claim 1, is characterized in that:
Described Sample location unit is fixed on main optical path all the time, overall symmetrical with the optical axis of main optical path, and at Sample location unit fixed head center drilling, its structure ensures the Laser beam propagation after laser bundle-enlarging collimation and Focused Optical system without impact.
5. Laser-induced Breakdown Spectroscopy analytic system according to claim 1, is characterized in that:
The plane of incidence of described beam splitter and optical axis included angle are 45 °.
6. Laser-induced Breakdown Spectroscopy analytic system according to claim 1, is characterized in that:
The outer setting of described removable locating platform has light shield.
7. Laser-induced Breakdown Spectroscopy analytic system according to claim 1, is characterized in that:
The operation wavelength of described pulsed laser gets 1064nm, 532nm or 256nm, pulse energy 80-120 MJ, pulse width 6-9 nanosecond; Described beam splitter adopts 10:90 spectroscope, and namely pulse laser reflects 10% luminous energy through this beam splitter transmission 90% luminous energy.
8. adopt Laser-induced Breakdown Spectroscopy analytic system as claimed in claim 1 to carry out the method for sample analysis, mainly comprise the following steps:
(1) adjust and determine testing sample position
Sample location cell operation, testing sample surface is radiated at fixed angle with the axisymmetric two bundle laser of key light, open LED illumination lamp, the hot spot of every light beam on testing sample surface is taken respectively with camera, control module gathers gained hot spot picture and draws the coordinate of facula mass center in picture by software process, calculate the distance between two facula mass centers, judge within the scope of the focal plane position whether testing sample surface is in described laser bundle-enlarging collimation and Focused Optical system or Rayleigh range;
If so, then control module controls camera and stops taking pictures, and calculates the size of hot spot and corresponding hot spot optical density, and sends trigger pip pulsed laser is started working; If not, then control module calculates the vertical range of the focal plane position of testing sample surface and laser bundle-enlarging collimation and Focused Optical system further, then controls removable locating platform and moves, and drives testing sample surface to focal plane position; Confirm that testing sample surface arrives within the scope of focal plane position or Rayleigh range, control module controls camera to be stopped taking pictures, and calculates the size of hot spot and corresponding hot spot optical density, and sends trigger pip pulsed laser is started working;
(2) spectrum is obtained
The spectrum that pulse laser inspires on testing sample to external expansion with 2 π solid angles, adopts Cassegrain telescope to receive, and by optical fiber, the light signal input spectrum instrument received is carried out photoelectric conversion;
(3) conclusion is analyzed
The measurement data exported by spectrometer imports data handling system, comes component and the content thereof of this testing sample of qualitative and quantitative analysis based on the wavelength in measurement data and intensity corresponding relation.
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| CN102608079B (en) * | 2012-03-03 | 2015-04-08 | 南昌航空大学 | Detection method of long-distance laser induced plasma spectrum |
| CN102788763A (en) * | 2012-09-03 | 2012-11-21 | 四川大学 | Difference absorption spectrum atmospheric monitoring system with laser induced breakdown spectrum serving as light source |
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