CN103529000A - Single-light-source dual-wavelength laser-induced breakdown spectroscopy measurement device and method - Google Patents
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Abstract
The invention discloses a single-light-source dual-wavelength laser-induced breakdown spectroscopy measurement device and method. The device mainly comprises a pulse laser, a frequency doubling crystal, a spectroscope, a first total reflector, a second total reflector, an optical shutter, a spectrometer and a synchronous delay controller; laser generated by the pulse laser passes through the frequency doubling crystal and is divided into fundamental frequency light and frequency doubling light which are irradiated on the spectroscope; the frequency doubling light is reflected by the first total reflector and then vertically irradiates the surface of the sample to be measured; the fundamental frequency light passes through the optical shutter, is reflected by the second total reflector and then irradiates 1-5mm above the surface of the sample to be detected in parallel; the spectral signal generated by the excited plasma of the sample to be measured is converged to the optical fiber collecting head and transmitted to the spectrometer. The invention realizes the high detection sensitivity of the double-pulse LIBS, has the advantages of simple structure, compact volume and low cost, and can be widely applied to the technical field of laser diagnosis and spectral analysis.
Description
Technical field
The invention belongs to laser diagnostics and field of spectral analysis technology, be specifically related to a kind of single light source dual-wavelength laser induced breakdown spectroscopy measurement mechanism and method of material element content analysis.
Background technology
Laser-induced Breakdown Spectroscopy (Laser-induced Breakdown Spectroscopy, LIBS) technology is to utilize high power density laser to focus on testing sample surface, produce the laser plasma of 10000K~20000K high temperature, the determination and analysis of the atom by comprising in plasma, ion, the light emitted spectrum wavelength of molecule, determines the composition of element in testing sample.LIBS technical operation cost is low, measuring speed is fast, have high sensitivity, without or or only need simple sample pretreatment, just can realize the multielement of sample is detected simultaneously and rapidly, attempted being applied to the fields such as object elemental composition diagnosis.
Tradition LIBS technology adopts single-pulse laser as light source, when laser pulses irradiate is when testing sample is surperficial, the electron density in the plasma region in laser pulse incident direction is larger, laser energy has been played to shielding action, make follow-up laser energy cannot arrive testing sample surface, stoped the continuation ablation of testing sample, therefore, the plasma signal detecting a little less than, limited its range of application.For addressing this problem, be more successfully to adopt double-pulse laser plasma signal to strengthen.
By literature search, patent " photoelectric double-pulse laser induced breakdown spectrograph and spectroscopic analysis methods " (CN101620183B), on the basis of monopulse LIBS, add second high electric field pulse to strengthen the atomic radiation intensity in plasma, to improve the sensitivity of spectral detection; Patented claim " method of double-pulse laser induced breakdown spectrograph system and spectral analysis thereof " (publication number is CN102854172A, and open day is 2013.01.02), is intended to realize the full-automation of spectral analysis; Patented claim " the flour constituent content measuring method based on double-pulse laser " (publication number is CN102788772A, and open day is 2012.11.21), the method is intended to improve the repeatability of online detection speed and test result; (publication number is CN102507511A in patented claim " a kind of infrared and ultraviolet double-pulse laser induced breakdown spectrum on line in situ detection device ", open day is 2012.06.20), this device is intended to strengthen the spectral radiance of laser plasma, improves the sensitivity of spectral detection.
Analyze known, in above-mentioned dipulse LIBS technology, the realization that plasma signal strengthens, or adopt two laser instruments, or one of them laser instrument is replaced with high-pressure discharging device; This has just caused proving installation to have complex structure, defect bulky, with high costs, has limited the range of application of LIBS technology.
Summary of the invention
The present invention overcomes the problem that above prior art exists, and a kind of single light source dual-wavelength laser induced breakdown spectroscopy measurement mechanism and spectral measurement method are provided.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
A dual-wavelength laser induced breakdown spectroscopy measurement mechanism, mainly comprises pulsed laser, frequency-doubling crystal, spectroscope, the first completely reflecting mirror, the second completely reflecting mirror, optical shutter, testing sample microscope carrier, optical fiber collection head, spectrometer, synchronization delay controller and computing machine;
The laser that described pulsed laser produces is divided into fundamental frequency light and frequency doubled light after by frequency-doubling crystal, is radiated on spectroscope;
Described spectroscope is to the high reflection of fundamental frequency light, to the high transmission of frequency doubled light, and after spectroscope, fundamental frequency light and frequency doubled light are divided into two light paths; Described frequency doubled light after described the first completely reflecting mirror reflection vertical irradiation in the surface of testing sample; Described fundamental frequency light is through described optical shutter, then by parallel radiation 1-5mm place above testing sample surface after described the second completely reflecting mirror reflection;
The spectral signal of the plasma generation that testing sample is inspired is assembled to optical fiber and is collected head, is sent to spectrometer;
Described computing machine is connected respectively with synchronization delay controller, spectrometer, in order to be responsible for parameter setting, communication and overall control; Described synchronization delay controller is controlled according to the synchronous and delay of pulse laser instrument, optical shutter and the spectrometer of computer installation; The spectral signal that described spectrometer obtains passes to computing machine and carries out data analysis.
Based on above-mentioned basic scheme, the present invention also does following optimization and limits and improve:
At the first completely reflecting mirror rear, be provided with the first convergent lens, at the second completely reflecting mirror rear, be provided with the second convergent lens, before optical fiber is collected head and testing sample microscope carrier, be provided with the 3rd convergent lens.
Above-mentioned testing sample microscope carrier is moveable platform, by moving horizontally of computer control moveable platform; Optical fiber is collected a spectral signal of collecting and is sent to spectrometer by multi-channel optical fibre.
Adopt above-mentioned single light source dual-wavelength laser induced breakdown spectroscopy measurement mechanism to carry out the method for spectral measurement, mainly comprise the following steps:
Step 1, place testing sample, utilize the parameter of computer installation synchronization delay controller, spectrometer and mobile platform;
Step 2, pulsed laser send high power laser light and are radiated on frequency-doubling crystal, and laser beam is divided into fundamental frequency light and frequency doubled light, and after spectroscope, fundamental frequency light and frequency doubled light are divided into two light paths; Frequency doubled light vertical irradiation after the first completely reflecting mirror reflection, on testing sample, produces plasma spark;
Step 3, after the time delay of 10-30 μ s, synchronization delay controller is opened order to optical shutter issue, fundamental frequency light is radiated on the second completely reflecting mirror after by optical shutter, the direction article on plasma body feathers that reflected light is parallel to testing sample surface heats again;
Step 4, after the time delay of 300-400ns, synchronization delay controller is to spectrometer trigger pip, spectrometer starts to collect spectral signal;
The spectral signal that step 5, spectrometer are collected sends computing machine analysis to, and plasma light spectrum signal and the standard spectrum of testing sample are analyzed, and draws element and concentration of element in testing sample.
In order to obtain conclusion more accurately and reliably, can also carry out step 6: testing sample moves under the drive of mobile platform, repeating step 1 to step 5 takes multiple measurements, to eliminate element erroneous judgement, to repeatedly measuring the concentration of element obtaining, average, to eliminate stochastic error; Finally, obtain contained element and concentration value thereof in testing sample.
Compare to prior art, tool of the present invention has the following advantages:
Adopted a laser instrument to realize the enhancing of dipulse LIBS signal, when improving LIBS technology detection sensitivity, that this device also has is simple in structure, volume compact and advantage with low cost, can be widely used in laser diagnostics and field of spectral analysis technology.
Accompanying drawing explanation
Fig. 1 is the structure principle chart of spectral measurement device of the present invention.
Wherein, 100-pulsed laser, 110-frequency-doubling crystal, 120-spectroscope, 131-completely reflecting mirror I, 132-completely reflecting mirror II, 140-optical shutter, 151-convergent lens I, 152-convergent lens II, 153-convergent lens III, 200-testing sample, 210-mobile platform, 220-optical fiber is collected head, 230-spectrometer, 300-synchronization delay controller, 400-computing machine.
Embodiment
Below in conjunction with accompanying drawing, provide a specific embodiment, the present invention is described in further details.
As shown in Figure 1, this single light source dual-wavelength laser induced breakdown spectroscopy measurement mechanism, mainly comprises that pulsed laser 100, frequency-doubling crystal 110, spectroscope 120, completely reflecting mirror I131, completely reflecting mirror II132, optical shutter 140, convergent lens I151, convergent lens II152, convergent lens III153, mobile platform 210, optical fiber collect 220, spectrometer 230, synchronization delay controller 300 and computing machine 400;
Described pulsed laser 100 is electric-optically Q-switched Nd:YAG laser instrument, and pulse repetition rate is 1-20Hz, and single pulse energy is 20-80mJ;
The laser that described pulsed laser 100 produces is divided into fundamental frequency light (wavelength 1064nm) and frequency doubled light (wavelength 532nm) after by frequency-doubling crystal 110, is radiated on spectroscope 120; Described frequency-doubling crystal 110 adopts KDP crystal;
The high reflection of 120 pairs of fundamental frequency light of described spectroscope, to the high transmission of frequency doubled light, after spectroscope 120, fundamental frequency light and frequency doubled light are divided into two light paths; On described mobile platform 210, be placed with testing sample 200; Described frequency doubled light after completely reflecting mirror I131 reflection, convergent lens I151 assemble vertical irradiation on testing sample 200 surfaces; Described fundamental frequency light is totally reflected mirror II132 reflection by optical shutter 140 and assembles rear parallel radiation on testing sample 200 surfaces by convergent lens II152;
The spectral signal of plasma generation is assembled into optical fiber and is collected 220 through convergent lens III153, and optical fiber is collected 220 spectral signal of collecting and transmitted into spectrometer 230 and analyzed by multi-channel optical fibre;
Described computing machine 400 is connected with synchronization delay controller 300, mobile platform 210 and spectrometer 230, in order to be responsible for parameter setting, communication and overall control; Synchronous and the delay of pulse laser instrument 100, optical shutter 140 and the spectrometer 230 that described synchronization delay controller 300 arranges according to computing machine 400 is controlled; The spectral signal that described spectrometer 230 obtains passes to computing machine 400 and carries out data analysis.
More than introduced single light source dual-wavelength laser induced breakdown spectroscopy measurement mechanism of the present invention, the present invention, when disclosing said apparatus, has also disclosed a kind of method of utilizing said apparatus to carry out spectral measurement, and described method comprises the steps:
Step 1, place testing sample 200, utilize computing machine 400 to set the parameter of synchronization delay controller 300, spectrometer 230 and mobile platform 210;
Step 2, pulsed laser 100 send high power laser light and are radiated on frequency-doubling crystal 110, and laser beam is divided into fundamental frequency light and frequency doubled light, then after spectroscope 120, fundamental frequency light and frequency doubled light are divided into two light paths; Frequency doubled light vertical irradiation after completely reflecting mirror I131 reflection, convergent lens I151 assemble, on testing sample 200 surfaces, produces plasma spark;
Step 3, after the time delay of 10-30 μ s, synchronization delay controller 300 opens order to optical shutter 140 issues, it is upper that fundamental frequency light is radiated at completely reflecting mirror II132 after by optical shutter 140, and the direction article on plasma body feathers that is then parallel to testing sample 200 surfaces after convergent lens II152 assembles heats again;
Step 4, after the time delay of 300-400ns, synchronization delay controller 300 is given spectrometer 230 trigger pips, spectrometer 230 starts to collect spectral signal;
The spectral signal that step 5, spectrometer 230 are collected sends computing machine 400 to and analyzes, and plasma light spectrum signal and the standard spectrum of testing sample 200 are analyzed, and draws element and concentration of element in testing sample 200;
Step 6, testing sample 200 move under the drive of mobile platform 210, and repeating step 1 to step 5 is carried out 10 measurements, to eliminate element erroneous judgement, measure the concentration of element obtaining and average, to eliminate stochastic error to 10 times; Finally, obtain contained element and concentration value thereof in testing sample 200.
Our experiments show that: apparatus of the present invention and method are identical with the detection sensitivity of two light source dipulse LIBS technology to the detection sensitivity of spectrum, but apparatus of the present invention have advantages of simple in structure, volume compact, with low cost.
Above-mentioned specific embodiment is the preferred embodiments of the present invention; and should be considered as the restriction to the claims in the present invention; other any change or other equivalent substitute mode that does not deviate from technical scheme of the present invention and make, within being all included in protection scope of the present invention.
Claims (5)
1. a single light source dual-wavelength laser induced breakdown spectroscopy measurement mechanism, is characterized in that: comprise pulsed laser, frequency-doubling crystal, spectroscope, the first completely reflecting mirror, the second completely reflecting mirror, optical shutter, testing sample microscope carrier, optical fiber collection head, spectrometer, synchronization delay controller and computing machine;
The laser that described pulsed laser produces is divided into fundamental frequency light and frequency doubled light after by frequency-doubling crystal, is radiated on spectroscope;
Described spectroscope is to the high reflection of fundamental frequency light, to the high transmission of frequency doubled light, and after spectroscope, fundamental frequency light and frequency doubled light are divided into two light paths; Described frequency doubled light after described the first completely reflecting mirror reflection vertical irradiation in the surface of testing sample; Described fundamental frequency light is through described optical shutter, then by parallel radiation 1-5mm place above testing sample surface after described the second completely reflecting mirror reflection;
The spectral signal of the plasma generation that testing sample is inspired is assembled to optical fiber and is collected head, is sent to spectrometer;
Described computing machine is connected respectively with synchronization delay controller, spectrometer, in order to be responsible for parameter setting, communication and overall control; Described synchronization delay controller is controlled according to the synchronous and delay of pulse laser instrument, optical shutter and the spectrometer of computer installation; The spectral signal that described spectrometer obtains passes to computing machine and carries out data analysis.
2. single light source dual-wavelength laser induced breakdown spectroscopy measurement mechanism according to claim 1, it is characterized in that: at the first completely reflecting mirror rear, be provided with the first convergent lens, at the second completely reflecting mirror rear, be provided with the second convergent lens, before optical fiber is collected head and testing sample microscope carrier, be provided with the 3rd convergent lens.
3. single light source dual-wavelength laser induced breakdown spectroscopy measurement mechanism according to claim 1 and 2, is characterized in that: described testing sample microscope carrier is moveable platform, by moving horizontally of computer control moveable platform; Optical fiber is collected a spectral signal of collecting and is sent to spectrometer by multi-channel optical fibre.
4. adopt single light source dual-wavelength laser induced breakdown spectroscopy measurement mechanism as claimed in claim 3 to carry out the method for spectral measurement, it is characterized in that: comprise the following steps:
Step 1, place testing sample, utilize the parameter of computer installation synchronization delay controller, spectrometer and mobile platform;
Step 2, pulsed laser send high power laser light and are radiated on frequency-doubling crystal, and laser beam is divided into fundamental frequency light and frequency doubled light, and after spectroscope, fundamental frequency light and frequency doubled light are divided into two light paths; Frequency doubled light vertical irradiation after the first completely reflecting mirror reflection, on testing sample, produces plasma spark;
Step 3, after the time delay of 10-30 μ s, synchronization delay controller is opened order to optical shutter issue, fundamental frequency light is radiated on the second completely reflecting mirror after by optical shutter, the direction article on plasma body feathers that reflected light is parallel to testing sample surface heats again;
Step 4, after the time delay of 300-400ns, synchronization delay controller is to spectrometer trigger pip, spectrometer starts to collect spectral signal;
The spectral signal that step 5, spectrometer are collected sends computing machine analysis to, and plasma light spectrum signal and the standard spectrum of testing sample are analyzed, and draws element and concentration of element in testing sample.
5. the method for spectral measurement according to claim 4, is characterized in that:
Also comprise step 6: testing sample moves under the drive of mobile platform, repeating step 1 to step 5 takes multiple measurements, and to eliminate element erroneous judgement, averages, to eliminate stochastic error to repeatedly measuring the concentration of element obtaining; Finally, obtain contained element and concentration value thereof in testing sample.
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