CN103175808A - 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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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 element qualitative and quantitative analysis.
Background technology
Fast development along with laser technology, people improve constantly material trace element understanding demand, and Laser-induced Breakdown Spectroscopy (Laser-induced Breakdown Spectroscopy is called for short LIBS) technology becomes a kind of Atomic Emission Spectral Analysis new technology based on Reciprocity of Laser ﹠ Materials that receives much concern and develop rapidly in recent years.By low-yield narrow width pulse Laser Focusing is carried out light splitting and detection in the plasma light spectrum signal that sample surfaces produces, 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, be not subjected to the restrictions such as material type, surface topography, state, electric conductivity, and generally do not need pre-treatment, the sample loss is little, and response can realize multielement express-analysis simultaneously rapidly; Have the advantages that noncontact is analyzed, be easy to remote sensing and control, can be used for remote on-line quick detection Laser-induced Breakdown Spectroscopy technology and be widely used in the industries such as iron and steel, coloured, coal, geology, archaeology, environment.
But up to now, this technology still rests on the Theoretical Design aspect, domesticly not yet can put into practice the LIBS technology, and is external or the development device is arranged, but only can realize qualitatively judging, and do not possess the function of quantitative test.
Summary of the invention
The invention provides a kind of Laser-induced Breakdown Spectroscopy analytic system, with component and the content thereof of realizing the qualitative and quantitative analysis sample.
For realizing above goal of the invention, the present invention provides following basic technical scheme:
the Laser-induced Breakdown Spectroscopy analytic system comprises control module, pulsed laser and the beam splitter that sets gradually along the pulse laser exit direction, the removable locating platform in order to place testing sample, spectrum collector unit, spectrometer and data handling system, described beam splitter is told main optical path and sampling light path with the emergent light pulse of pulsed laser according to the energy distribution ratio of setting, be disposed with laser bundle-enlarging collimation and Focused Optical system on main optical path, Sample location unit with described removable locating platform formation FEEDBACK CONTROL, be respectively arranged with the pulsed laser energy measurement module on the sampling light path, 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 the trigger pip generation unit, the output of delay control circuit square-wave signal is connected to the second input end of 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 output, and each control signal output terminal correspondence respectively 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 the twin-beam light-source system sends are radiated at the testing sample surface with the symmetrical of described main optical path and with fixed angle; Camera is used for taking the hot spot on testing sample surface, consists of FEEDBACK CONTROL with removable locating platform.When experimental situation illumination is low, also the LED illuminating lamp can be set.Twin-beam Sample location cell operation pattern can be: the energising of twin-beam light-source system, and the LED energising, the camera energising, removable locating platform starts; The unit power cut-off of twin-beam Sample location, the twin-beam outage, the LED outage, camera stops taking pictures, and removable locating platform is closed.
Above-mentioned spectrum collector unit is connected to spectrometer by coupling fiber, the concrete preferred Cassegrain telescope of spectrum collector unit.Laser excitation spectrum out with 2 π solid angles to external expansion, in order to obtain better spectral information, therefore adopt optical fiber as receiving-member (Cassegrain telescope is only needed slightly to do conventional accommodation), then the light signal input spectrum instrument that receives 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 is entered trigger action delay cell through surveying light after beam splitter by the diffuse reflection of pulsed laser energy measurement module, and the output square-wave signal is used for triggering spectrometer and gathers spectrum.
Above-mentioned Sample location unit is fixedly installed on main optical path all the time, whole symmetrical with main optical path, Sample location unit fixed head center drilling, its structure guarantee on through 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, the Sample location unit also just needn't require unscreened structure like this.
The plane of incidence of above-mentioned beam splitter and primary optical axis angle preferably are set to 45 °.
The outside of above-mentioned removable locating platform also is provided with light shield, can prevent like this ambient light interference, also is convenient to stay certain access port to the spectrum collector unit simultaneously, allows electric three-dimensional pan carriage external circuit conveniently leave interface.
The preferred 1064nm of the operation wavelength of above-mentioned pulsed laser, 532nm or 256nm, pulse energy 80-120 milli is burnt, pulse width 6-9 nanosecond; Described beam splitter adopts the 10:90 spectroscope, and namely pulse laser is through this beam splitter transmission 90% luminous energy reflection 10% luminous energy.
The course of work of the present invention mainly comprises the following steps:
(1) adjustment testing sample position
the Sample location cell operation, be radiated at the testing sample surface with the axisymmetric two bundle laser of key light with fixed angle, Sample location unit fixed head center drilling, its structure guarantees the Laser beam propagation after process laser bundle-enlarging collimation and Focused Optical system without impact, take respectively every light beam at the hot spot on testing sample surface with camera, control module collection gained hot spot picture is processed by software and is drawn the coordinate of facula mass center in picture, calculate the distance between two facula mass centers, judge whether the testing sample surface is in the focal plane position or Rayleigh range scope of described laser bundle-enlarging collimation and Focused Optical system.
If so, control module control camera stops taking pictures, and calculates facula area and optical density, and the transmission trigger pip is started working pulsed laser;
If not, control module further calculates the vertical range of testing sample surface and the focal plane position of laser bundle-enlarging collimation and Focused Optical system, then controls removable locating platform and moves, and drives the testing sample surface to focal plane position; Confirmation testing sample surface arrives in focal plane position or Rayleigh range scope, and control module is controlled camera and stopped taking pictures, and calculates facula area and optical density, and the transmission trigger pip is started working pulsed laser.
(2) obtain spectrum
The spectrum that pulse laser inspires on testing sample, adopts Cassegrain telescope to receive, and by optical fiber, the light signal input spectrum instrument that receives is carried out photoelectric conversion to external expansion with 2 π solid angle.
(3) analyze conclusion
The measurement data of spectrometer output is imported data handling system, come 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:
The present invention has adopted a kind of new method for multielement component sample composition element qualitative and quantitative analysis.
Structure of the present invention is simple and clear, and is easy to operate, can realize that quantitative and qualitative analysis determines component and the content thereof of this sample.
In the present invention, the Sample location unit can guarantee accurately that sample surfaces is positioned at the lens combination focal plane position, and control module triggers the gating pulse laser works and spectrum receives, and can record every state parameter, guarantees test data real-time and accuracy.
Description of drawings
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, the detection of 4-pulse signal and trigger delays, 5-laser bundle-enlarging collimation and Focused Optical system, 6-twin-beam Sample location unit, 7-sample chamber, 8-spectrum collector 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-the first laser beam source, 12-the 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 the first light path, 602-LD light source the 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, spectrum collector unit (Cassegrain telescope) 8, spectrometer 9, data handling system 10 etc.
The pulsed laser specific requirement: pulse requires wavelength 1064nm, pulse energy 100mJ, pulse width 7ns, external power supply gating pulse energy, configuration refrigeration unit.
Beam splitter requires 45 ° of incidents, can adopt the 10:90 spectroscope, and the 1064nm pulse laser is in strict accordance with 10:90 transmission 90% luminous energy reflection 10% luminous energy.Energy of reflection light 10mJ enters the energy detection module.The pulsed laser energy measurement module can branch away luminous energy (being the energy of light pulse 1/10th) to beam splitter by accurate detection.
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 the spectrometer collection signal by trigger delays control lag time signaling.
Twin-beam Sample location unit requires: restraint laser (indication collimated light beam) to be radiated at sample surfaces with 17 ° of optical axis included angles with key light axisymmetric two, take respectively every light beam at the hot spot of sample surfaces with camera with 20 °, process by software the vertical range that picture draws sample and optical system focal plane position, move to the direction of correspondence and drive sample and move to focal plane position thereby then control the D translation frame by control module.After the confirmatory sample surface arrives focal plane position, signal of output to the pulsed laser power supply, is that pulsed laser sends pulse laser.
The sample chamber can prevent the ambient light interference, stays certain entrance for the spectrum collector unit, leaves interface for electric three-dimensional pan carriage external circuit.
Spectrometer spectral range 200nm～900nm is to the strength sensitive of spectrum, accurately.Quantitatively need to demarcate during the sample element, the time that begins to collect data survey in strict accordance with pulse signal and the delay units delay time definite.
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, do definite wavelength and the corresponding relation of receiving spectrum by receiving system and spectrometer.In addition for for the purpose of quantitative test is more accurate, can also the indoor stable neighbourhood noise of collected specimens, as calculating parameter.
Control module is coordinated whole collection spectroscopy procedure.By twin-beam Sample location unit 6, sample surfaces is adjusted to the pulse laser focal plane position, power supply begins to export predetermined voltage, 1064nm pulsed laser 1 sends laser pulse through energy beam splitter 2, the 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 and survey and trigger delays 4, survey trigger pip and be given to control module.Rest light energy by laser beam expanding, collimate, focus on the testing sample surface in the sample chamber, sample produces the plasma exciatiaon process under the light laser energy exposure, outwards launch with 2 π solid angles, the characteristic spectral line that the sample element produces in this process is received laggardly to enter spectrometer and generate spectroscopic data by Cassegrain telescope.Process element and the content that finally obtains sample through a series of data.
Line strength formula that actual measurement obtains is as follows:
F is the instrument receiving efficiency, C
xBe the content of particle x in plasma, Amn is the spontaneous transition probability from the m energy level transition to the n energy level, g
mThe statistical weight of m energy level, E
mThe excitation energy of m energy level, k
BExpression Boltzmann constant, T is plasma temperature, U
x(T) be the partition function of particle x under temperature T.
First select the spectral line of concern from the plasma light spectral curve of entire scan, again measure the intensity of this spectral line, centre wavelength and the intensity of reading simultaneously every line.According to the relative intensity of spectral line and the electron temperature (T) of top described formula estimation plasma, 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 every kind of element in the estimation sample
xAnd spectral bandwidth L.then adopt loop iteration and adjustment, the beginning iteration, regard a zone below each crest envelope as, the calculating plasma chemical composition, then calculate absorption coefficient, then calculate spectral radiance, whether the spectrum that judgement calculates and measure spectrum be minimum from light intensity and waveform difference, if not, adjust so electron density, electron temperature, the parameters such as relative content of wavelength pulsewidth and each element are calculated again, if difference is minimum, but larger than the threshold value of setting before, so, a part is told in crest envelope zone, then adjust electron density, electron temperature, the parameters such as relative content of wavelength pulsewidth and each element are calculated and again less than the threshold value of setting before, calculate so and finish, the final content of determining sample composition element and correspondence.
Claims (9)
1. the Laser-induced Breakdown Spectroscopy analytic system, is characterized in that: comprise control module, pulsed laser and the beam splitter that sets gradually along the pulse laser exit direction, the removable locating platform in order to place testing sample, spectrum collector unit, spectrometer and data handling system, described beam splitter is told main optical path and sampling light path with the emergent light pulse of pulsed laser according to the energy distribution ratio of setting, be disposed with laser bundle-enlarging collimation and Focused Optical system on main optical path, Sample location unit with described removable locating platform formation FEEDBACK CONTROL, be respectively arranged with the pulsed laser energy measurement module on the sampling light path, the 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 the trigger pip generation unit, the output of delay control circuit square-wave signal is connected to the second input end of 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 output, and each control signal output terminal correspondence respectively is connected to Sample location unit, removable locating platform, spectrometer, the data output end of spectrometer is connected to data handling system.
2. Laser-induced Breakdown Spectroscopy analytic system according to claim 1 is characterized in that:
Described Sample location unit comprises twin-beam light-source system and camera, and the two bundle laser that the twin-beam light-source system sends are radiated at the testing sample surface with the symmetrical of described main optical path and with fixed angle; Camera is used for taking the hot spot on testing sample surface, consists of FEEDBACK CONTROL with removable locating platform.
3. Laser-induced Breakdown Spectroscopy analytic system according to claim 1 is characterized in that:
Described spectrum collector unit is connected to spectrometer by coupling fiber, and the spectrum collector unit adopts Cassegrain telescope.
4. Laser-induced Breakdown Spectroscopy analytic system according to claim 1 is characterized in that:
Described trigger action delay cell receives and diffuses from the pulsed laser energy measurement module, and provides the square-wave signal of adjustable delay.
5. 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, whole symmetrical with main optical path, and at Sample location unit fixed head center drilling, its structure guarantee on through the Laser beam propagation after laser bundle-enlarging collimation and Focused Optical system without impact.
6. 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 °.
7. 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.
8. Laser-induced Breakdown Spectroscopy analytic system according to claim 1 is characterized in that:
The operation wavelength of described pulsed laser is got 1064nm, 532nm or 256nm, and pulse energy 80-120 milli is burnt, pulse width 6-9 nanosecond; Described beam splitter adopts the 10:90 spectroscope, and namely pulse laser is through this beam splitter transmission 90% luminous energy reflection 10% luminous energy.
9. 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 definite testing sample position
The Sample location cell operation, be radiated at the testing sample surface with the axisymmetric two bundle laser of key light with fixed angle, open the LED illuminating lamp, take respectively every light beam at the hot spot on testing sample surface with camera, control module collection gained hot spot picture is processed by software and is drawn the coordinate of facula mass center in picture, calculate the distance between two facula mass centers, judge whether the testing sample surface is in the focal plane position or Rayleigh range scope of described laser bundle-enlarging collimation and Focused Optical system;
If so, control module control camera stops taking pictures, and calculates size and the corresponding hot spot optical density of hot spot, and the transmission trigger pip is started working pulsed laser; If not, control module further calculates the vertical range of testing sample surface and the focal plane position of laser bundle-enlarging collimation and Focused Optical system, then controls removable locating platform and moves, and drives the testing sample surface to focal plane position; Confirm that in testing sample surperficial arrival focal plane position or Rayleigh range scope, control module is controlled camera and stopped taking pictures, calculate size and the corresponding hot spot optical density of hot spot, and the transmission trigger pip is started working pulsed laser;
(2) obtain spectrum
The spectrum that pulse laser inspires on testing sample, adopts Cassegrain telescope to receive, and by optical fiber, the light signal input spectrum instrument that receives is carried out photoelectric conversion to external expansion with 2 π solid angle;
(3) analyze conclusion
The measurement data of spectrometer output is imported data handling system, come 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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| CN113252618B (en) * | 2021-05-10 | 2023-08-11 | 河南丰博自动化有限公司 | Linkage device of laser-induced breakdown spectroscopy analysis system and spectroscopy analysis system |
| CN117007561A (en) * | 2023-09-27 | 2023-11-07 | 苏州元脑智能科技有限公司 | Spectrum measuring system, method and device for semiconductor material |
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