CN107014804A - A kind of microwave radiation technology excites the apparatus and method for suppressing LIBS self absorption effect - Google Patents
A kind of microwave radiation technology excites the apparatus and method for suppressing LIBS self absorption effect Download PDFInfo
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Abstract
The apparatus and method for suppressing LIBS self absorption effect are excited the invention discloses a kind of microwave radiation technology.Described device includes pulse laser, convergent lens, spectrometer, photodetector, computer, three-D displacement platform, microwave probe and microwave generator.The present invention is excited with good penetration using microwave radiation technology, the ground state particle of nearly all element excite simultaneously in plasma, avoid the self-absorption to the similar element emission spectrum in center, and go out the self absorption effect sent and suppress and eliminate plasma from source, to improve the degree of accuracy and the precision of LIBS quantitative analysis.The present invention carries out auxiliary laser induced breakdown spectroscopy using microwave, microwave energy is by probe near-field thermal radiation to laser plasma, without closing chamber, sample loading process it is simple, and remain LIBS can be realized in atmospheric environment quickly, it is in situ, in real time, multielement, remote analysis the advantages of.
Description
Technical field
The present invention relates to plasma emission spectrometry field, and in particular to a kind of microwave radiation technology excites suppression laser to lure
The apparatus and method for leading breakdown spectral self absorption effect.
Background technology
LIBS (laser-induced breakdown spectroscopy, abbreviation LIBS),
It is a kind of component spectrum detection and analysis technology.Its general principle is to utilize a branch of high energy pulse Laser Focusing to testing sample table
Face, ablation produces laser plasma, and the element of testing sample is obtained according to the wavelength and intensity of plasma emission spectroscopy
Species and its concentration.Because LIBS relative to traditional analytical technology has many intrinsic advantages, such as
Elementary analysis sample is extensive, sample pretreatment is simple, it is in situ in real time, remote detection etc..Therefore, LIBS
Have become study hotspot both domestic and external.
By the development of more than 50 years, LIBS qualitative analysis had been obtained for being widely recognized as.With traditional elementary analysis skill
Art is compared, and LIBS accuracy of quantitative analysis also has gap.At present, the research emphasis and difficult point of LIBS technologies concentrate on quantitative point
In terms of analysis.Due to LIBS using laser as excitaton source, the complexity of high-order harmonics spectrum result in laser plasma
The inhomogeneities of body spatial and temporal distributions, Plasma Center regional temperature is high, and outer layer regional temperature is low, contains substantial amounts of ground state grain
Son.When the outside emittance of the excited state particle in Plasma Center region, it can be absorbed by the ground state particle of outer layer, so that
The phenomenon for causing surveyed the intensity of spectral line to weaken and deform, i.e. self absorption effect (Self-absorption effect).Self-priming
Produce effects the presence severe jamming the answered emission spectrum of laser plasma, destroys between spectral intensity and concentration of element originally
Linear mapping relation, be cause LIBS quantitative analyses precision difference major reason.Therefore, to realize that LIBS's is precisely quantitative
Analysis, it is necessary to overcome negative effect caused by self absorption effect.
Chinese patent literature《A kind of method for suppressing LIBS self absorption effect》(notification number is CN
105067592A, the day for announcing is on November 18th, 2015) disclose a kind of suppression LIBS self absorption effect
Method, this method carries out ablation to testing sample using pulse laser and produced after plasma, recycles swashing for tunable wave length
Light device plasma carries out selective excitation to suppress self absorption effect.Although this method is relative to traditional self absorption effect
To go out to send elimination self absorption effect from the intrinsic physical characteristic of plasma for bearing calibration, however, this method exist with
The deficiency of lower two aspects, one is that this method can only once be suppressed for a kind of self-absorption of a spectral line of element, is imitated
Rate is low；Two be that used OPO Wavelength tunable lasers are expensive, volume is big, cumbersome, and to environmental requirement constant temperature
With constant humidity etc., cause difficult in maintenance.Therefore, how to realize and suppress or even eliminate laser plasma self absorption effect from source,
The suppression to the self absorption effect of multielement spectrum line is realized simultaneously, and reduces the cost of LIBS analytical instrument
By one of emphasis studied as LIBS.
The content of the invention
The device for suppressing LIBS self absorption effect, its mesh are excited the invention provides a kind of microwave radiation technology
Be reduce the cost of existing LIBS analyzer, reduce the volume of instrument, improve the facility that instrument is used
Property, and realized from source while the suppression of the self absorption effect to multielement spectrum line, is determined with improving LIBS
Measure accuracy of analysis and precision.
In order to reach above-mentioned target, the present invention is mainly achieved through the following technical solutions：
A kind of microwave radiation technology excite suppress LIBS self absorption effect device, including pulse laser,
Convergent lens, spectrometer, photodetector, computer, three-D displacement platform, microwave probe and microwave generator；Wherein：
The pulse laser is used to export pulse laser, and it exports the concentrated lens focus of laser to three-D displacement platform
Surface；
Focus point of the alignment convergent lens in microwave probe tip on three-D displacement platform, for the focusing
Point radiation microwave；Microwave probe input termination microwave generator, for feed-in microwave；
The spectrometer is used for the spectral information for gathering the focal spot, and its output connects photodetector, for light letter
Number be converted to electric signal；The photodetector output is connected with computer；The computer is used to handle photodetector biography
The spectroscopic data come；
During work, sample is placed in three-D displacement platform plane convergent lens focus position, in pulse laser and microwave
Under effect, plasma is produced；Plasma light spectrum information by spectrometer collection and is converted to electric signal by photodetector,
The compositional information of sample is obtained by computer disposal.
Further, described device also includes and digital delay pulse generator, for producing synchronization pulse；It is wrapped
Three synchronous signal output ends are included, the pulse laser triggering end, the triggering end of photodetector and microwave are connect respectively and is occurred
Device triggering end, the sequential for controlling each road signal, due to the inhomogeneities of the temporal evolution of plasma, is swashed using different
Hair time and collection delay, gate-width, the spectral quality obtained are different, so needing digital delay impulse generator to control them
Self-absorption inhibition of the work schedule to have obtained.
Further, the spectrometer carries spectra collection head, and it is popped one's head in close to described focus point, for gathering at this etc.
The emission spectrum of gas ions, due to the inhomogeneities of the spatial evolution of plasma, the collection higher self-absorption in position is more serious, institute
Will be close to the focus point with spectra collection head, it is therefore intended that the self-absorption inhibition obtained.
According to another aspect of the present invention, it is also proposed that a kind of microwave radiation technology excites suppression LIBS self-priming
Produce effects the method answered, comprise the following steps：
The first step, Laser Focusing is exported to testing sample by pulse laser；
Second step, by microwave probe and spectrometer collection head rest be near, alignment testing sample；
3rd step, makes laser and microwave export while acting on testing sample；
4th step, is converted to electric signal by spectrometer output, sends into computer disposal.
The present invention has following technical characterstic and advantage：
(1) present invention most prominent technical characterstic is to be excited using microwave radiation technology with good penetration, with body heat source
Formal equivalence gas ions integrally carry out the ground state particle of nearly all element in the characteristic of instantaneous heat temperature raising, plasma
Progress is excited simultaneously, it is to avoid self-absorption of the ground state particle of element to the similar element emission spectrum in its center, realization is to LIBS
The self-absorption of full spectrum suppresses, so as to improve the degree of accuracy and the precision of LIBS quantitative analysis.
(2) the inventive method is not to occur self absorption effect in spectrum to be corrected later, but special from intrinsic physics
Levy and set out, go out to send from source and suppress and eliminate the self absorption effect of plasma, it is to avoid what self absorption effect was brought quantifies
Analytical error.
(3) apparatus of the present invention substitute the laser of tunable wave length using magnetron or semiconductor microactuator wave device, produce micro-
Ripple carries out auxiliary laser induced breakdown spectroscopy, significantly reduces the cost of analytical instrument, and reduce to a certain extent
The volume of analyzer, improves analytical instrument flexibility and portability, advantageously in the actual use and popularization of instrument.
(4) microwave energy in apparatus of the present invention is coupled into coaxial cable and microwave probe (antenna) by impedance matching,
Near-field thermal radiation is carried out to laser plasma by microwave probe again, without closing chamber, which not only simplifies load sample
The process of product, and remain LIBS can be realized in atmospheric environment quickly, it is in situ, in real time, it is multielement, remote
The advantages of journey is analyzed.
(5) the inventive method carries out auxiliary laser induced breakdown spectroscopy, the also work with enhanced spectrum intensity using microwave
With (principle is injected after microwave energy, and the life-span of plasma can extend, and increases the spectra collection time of integration, spectral intensity is just
Can increase), therefore with the laser energy of very little just qualitative or quantitative analysis can be carried out to sample, really realize that laser is lured
The lossless advantage of breakdown spectral is led, undamaged occasion is needed to be suitable for detection jewelry, biology etc..
Brief description of the drawings
Fig. 1 is that a kind of microwave radiation technology of the present invention excites the device for suppressing LIBS self absorption effect
Schematic diagram；
Fig. 2 is that a kind of microwave radiation technology of the present invention excites the flow for suppressing LIBS self absorption effect
Schematic diagram.
Fig. 3 is the self-absorption result figure that present example suppresses Na I 589.00nm and Na I 589.59nm spectral lines.
Fig. 4 is that present example suppresses Na I 589.00nm, Na I 589.59nm and K I 766.49nm, K I simultaneously
769.90nm the self-absorption result figure of spectral line.
In the present invention marked as：1- pulse lasers, 3- speculums, 4- convergent lenses, 5- laser plasmas, 6- spectrum
Acquisition probe, 7- optical fiber, 8- spectrometers, 9- photodetectors, 10- computers, 11- three-D displacement platforms, 12- microwave probes,
13- microwave probe fixtures, 14- coaxial cables, 15- microwave generators, 16- digital delay impulse generators.
Embodiment
The embodiment to the present invention is described further below in conjunction with the accompanying drawings.Herein it should be noted that for
The explanation of these embodiments is used to help understand the present invention, but does not constitute limitation of the invention.In addition, disclosed below
As long as each of the invention embodiment in involved technical characteristic do not constitute conflict each other and can just be mutually combined.
The problem of for LIBS self absorption effect, the present invention proposes a kind of microwave radiation technology and excites suppression
The apparatus and method of LIBS self absorption effect, its principle is to carry out ablation to testing sample with pulse laser,
Excite after generation plasma, then produce microwave using magnetron or semiconductor microwave device, microwave energy passes through impedance matching
Coaxial cable and microwave probe (antenna) are coupled into successively, then near-field thermal radiation is carried out to laser plasma by microwave probe.
Electronics in plasma accelerates under microwave electric field effect, is excited with other atoms or molecule or ionization is touched
Hit, accuracy controlling is carried out by the microwave energy to injection, when control microwave radiation technology excites the acceleration of plasma internal particle
Between, its energy provided is met ground state particle in plasma and transit to first excited state energy level, so that self absorption effect is produced
The number of raw " arch-criminal "-ground state particle is reduced sharply, to realize the effect for suppressing self absorption effect.This method can be realized
Reduce the self absorption effect for even eliminating the full element of LIBS, improve LIBS quantitative analysis
While the degree of accuracy and precision, the volume of LIBS analysis can be reduced, lowering apparatus is produced and is manufactured into
This, improves the detection sensitivity of element, contributes to popularizing for LIBS.
As shown in figure 1, a kind of microwave radiation technology that present example is provided excites suppression LIBS self-absorption
The device of effect, including pulse laser 1, cage cube 2, speculum 3, convergent lens 4, laser plasma 5, spectra collection
First 6, optical fiber 7, spectrometer 8, photodetector 9, computer 10, three-D displacement platform 11, microwave probe 12, microwave probe fixture
13, coaxial cable 14, microwave generator 15, and digital delay pulse generator 16.
Speculum 3 is placed in inside cage cube 2, and in the light extraction light path of pulse laser 1, with pulse laser
1 laser beam produced is changing 90 degree of directions with the laser beam for producing pulse laser 1, is making laser into 45 degree of angles, its purpose
Beam is vertically downward；Convergent lens 4 is located on the reflected light path of speculum 3, the laser beam ablation sample after convergence is produced laser
Plasma 5；Sample is placed on above three-D displacement platform 11, and the displacement platform can be moved up and down, and purpose exists
In causing laser not to be always ablation in same position, the stability of analysis is improved；
The signal of laser plasma 5 is acquired by spectra collection first 6, the signal after collection sends into light by optical fiber 7
Spectrometer 8, the optical signal of 8 pairs of collections of spectrometer carries out light-splitting processing；Described spectrometer 8 is connected with photodetector 9, and photoelectricity is visited
It can be that charge coupling device (CCD), enhanced CCD (ICCD) or photomultiplier (PMT) etc. can be by optical signals to survey device 9
Be converted to the device of electric signal；The electric signal that described photodetector 9 is exported is sent to computer 10 and carries out data processing；
Microwave generator 15 is made up of magnetron or semiconductor microactuator wave device, is generated by it microwave signal, microwave signal is again
Microwave probe 12 is sent to by coaxial cable 14, and the microwave probe 12 is fixed by microwave probe fixture and adjusts microwave
The position of probe 12, is excited, the microwave again by the microwave signal plasma 15 of the near-field thermal radiation of microwave probe 12
The shape of probe can be double needle configuration, single needle structure, circular ring structure or loop configuration etc..
Described pulse laser 1 is generally nanosecond, or picosecond or femtosecond, and laser output wavelength is from purple
Near infrared range is arrived outside.According to different detection objects, laser single-pulse energy can be in 0~800mJ scope flexible modulations.
Digital delay impulse generator 16 connects the Q-switch signal output parts of the pulse laser 1 and described micro-
The trigger signal input of wave producer 15, photodetector 9, described digital delay impulse generator 16 is used to control laser
Time delay between pulse signal and the collection signal of photodetector 9, and control laser pulse signal and microwave generator
Time delay between 14 microwave signals produced, time delay can be adjusted in the range of 10ns~100ms, can be to optical telecommunications
Number signal to noise ratio optimize.
Microwave radiation technology excites the schematic flow sheet for suppressing LIBS self absorption effect as shown in Fig. 2 the party
Method specifically includes following steps：
The first step, prepares testing sample, opens pulse laser outgoing laser beam, pulse laser is exported into Laser Focusing
To produce plasma on to testing sample；
Second step, opens microwave generator, produces microwave energy, microwave probe is sent to by coaxial cable, and will be micro-
Ripple probe and spectrometer collection head rest are near, be directed at testing sample；
3rd step, makes laser and microwave export while acting on testing sample；
4th step, electric signal is converted to by spectrometer output, sends into computer disposal, and record correspondence spectroscopic data is carried out
Qualitative or quantitative analysis.
In order to preferably explain the present invention, two specific embodiments given below：
Embodiment 1
This method is described in detail exemplified by detecting the sodium element in sodium chloride powder press sheet compression for the present embodiment.
This test laser 1 is using radium treasured Vlite-200Nd:The laser of YAG models, optical maser wavelength is 1064nm, is swashed
Light energy is 40mJ, and laser repetition rate is 1Hz, and spectrometer 8 uses the light of Ai Wantisi AvaSpec-2048FT-8RM models
Spectrometer, the time of integration of photodetector 9 is 2ms, and time delay is 2us, average 2 times；The power of microwave generator 15 is
120W。
The first step, sodium chloride powder is made under 20MPa pressure of tablet press machine a diameter of 40mm thickness 4mm disk, put
Put after sample, adjusting light path makes the focal position of convergent lens 4 be located at below sample at 4mm；
Second step, is located at sample surfaces above 2mm by microwave probe, using the microwave probe of double needle configuration, between crosspointer
Away from for 2mm, crosspointer is parallel with sample surfaces, laser beam is just passed through from the gap between crosspointer, by spectrometer collection head rest
Closely, testing sample is directed at, to collect plasma emission spectrum signal；
3rd step, opens three-D displacement platform 11, it is moved by defined path, then opens microwave generator 15, produces
Raw continuous microwave energy, microwave probe 12 is sent to by coaxial cable 14, then opens the outgoing laser beam of pulse laser 1,
The reflected mirror 3 of laser beam and convergent lens 4 focus on and plasma are produced on testing sample, and microwave probe is by microwave energy near field
Radiate to laser plasma；
4th step, is converted to electric signal by spectrometer output, sends into computer disposal, the present embodiment essential record and analysis
The data of Na atom spectrum (Na I 589.00nm and Na 589.59nm).
The self-absorption result figure for suppressing Na I 589.00nm and Na I 589.59nm spectral lines in the present embodiment is shown in Fig. 3 institutes
Show, it can be seen that when there is microwave action, not only significantly inhibit self absorption effect, but also with the enhanced work of spectrum
With.
Embodiment 2
Whether there is the effect for suppressing multiple element self-absorptions simultaneously for the checking present invention, the present embodiment is with while detect potassium
Exemplified by sodium and potassium element in feldspar (GBW03116) press sheet compression, this method is described in detail.
This test laser 1 is using radium treasured Vlite-200Nd:The laser of YAG models, optical maser wavelength is 1064nm, is swashed
Light energy is 40mJ, and laser repetition rate is 1Hz, and spectrometer 8 uses the light of Ai Wantisi AvaSpec-2048FT-8RM models
Spectrometer, the time of integration of photodetector 9 is 2ms, and time delay is 2us, average 2 times；The power of microwave generator 15 is
100W。
The first step, potassium feldspar powder is made under 20MPa pressure of tablet press machine a diameter of 40mm thickness 4mm disk, put
Put after sample, adjusting light path makes the focal position of convergent lens 4 be located at below sample at 4mm, then opens pulse laser
Device outgoing laser beam, plasma is produced using laser beam ablation testing sample surface；
Second step, is located at sample surfaces above 2mm by microwave probe, using the microwave probe of double needle configuration, between crosspointer
Away from for 2mm, crosspointer is parallel with sample surfaces, laser beam is just passed through from the gap between crosspointer, by spectrometer collection head rest
Closely, testing sample is directed at, to collect plasma emission spectrum signal；Crosspointer formation microwave electric field, plasma just in centre,
Plasma is conducive to be excited.
3rd step, opens three-D displacement platform 11, it is moved by defined path, then opens microwave generator 15, produces
Raw continuous microwave energy, microwave probe 12 is sent to by coaxial cable 14, then opens the outgoing laser beam of pulse laser 1,
The reflected mirror 3 of laser beam and convergent lens 4 focus on and plasma are produced on testing sample, and microwave probe is by microwave energy near field
Radiate to laser plasma；
4th step, is converted to electric signal by spectrometer output, sends into computer disposal, the present embodiment essential record and analysis
Na atom spectrum (Na I 589.00nm, Na 589.59nm) and potassium atom spectrum (K I 766.49nm, K I 769.90nm)
Data.
Example suppresses Na I 589.00nm, Na I 589.59nm and K I 766.49nm, K I simultaneously in the present embodiment
The self-absorption design sketch of 769.90nm spectral lines is as shown in Figure 4, it can be seen that the present invention can suppress simultaneously Na and K element from
(by carrying out accuracy controlling to microwave Implantation Energy, control microwave radiation technology excites plasma internal particle to add to sink effect
The fast time, the energy of its energy and plasma self absorption effect needs that provide is set to match, i.e., the energy can make just
Ground state particle transits to energy level corresponding to the i.e. non-central similar element emission spectrum of a certain excited level, then different members
The ground state population of plain species is reduced sharply).
The above described is only a preferred embodiment of the present invention, not making any formal to the structure of the present invention
Limitation.Any simple modification, equivalent variations and the modification made in every technical spirit according to the present invention to above example,
Belong to technical scheme scope.
Claims (6)
1. a kind of microwave radiation technology excites the device for suppressing LIBS self absorption effect, it is characterised in that including arteries and veins
Rush laser (1), convergent lens (4), spectrometer (8), photodetector (9), computer (10), three-D displacement platform (11),
Microwave probe (12) and microwave generator (15)；Wherein：
The pulse laser (1) is used to export pulse laser, and its output concentrated lens of laser (4) focuses on three-D displacement and put down
Platform (11) surface；
Focus point of microwave probe (12) the tip alignment convergent lens (4) on three-D displacement platform (11), is used for
Microwave is radiated to the focus point；Microwave probe (12) input termination microwave generator (15), for feed-in microwave；
The spectrometer (8) is used for the spectral information for gathering the focal spot, and its output connects photodetector (9), for light
Signal is converted to electric signal；Photodetector (9) output is connected with computer (10)；The computer (10) is used to handle
The spectroscopic data that photodetector (9) is transmitted；
During work, sample is placed in three-D displacement platform (11) plane convergent lens (4) focus position, in pulse laser and microwave
In the presence of, produce plasma；Plasma light spectrum information is gathered and changed by photodetector (9) by spectrometer (8)
For electric signal, the compositional information for obtaining sample is handled by computer (10).
2. device according to claim 1, it is characterised in that also including with digital delay pulse generator (16), be used for
Produce synchronization pulse；It includes three synchronous signal output ends, and the pulse laser (1) triggering end, photoelectricity are connect respectively
The triggering end and microwave generator (15) triggering end of detector (9), the sequential for controlling each road signal.
3. device according to claim 1, it is characterised in that the spectrometer carries spectra collection head (6), its probe is leaned on
The nearly focus point, the emission spectrum for gathering plasma at this.
4. device according to claim 1, it is characterised in that the oscillating device of the microwave generator is magnetron or half
Conductor microwave device, the microwave probe is shaped as double needle configuration, single needle structure, circular ring structure or loop configuration.
5. device according to claim 1, it is characterised in that the photodetector charge coupling device (CCD), enhancing
Type CCD (ICCD) or photomultiplier (PMT).
6. a kind of microwave radiation technology excite suppress LIBS self absorption effect method, it is characterised in that including with
Lower step：
The first step, Laser Focusing is exported to testing sample by pulse laser；
Second step, by microwave probe and spectrometer collection head rest be near, alignment testing sample；
3rd step, makes laser and microwave export while acting on testing sample；
4th step, is converted to electric signal by spectrometer output, sends into computer disposal.
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| CN107607520A (en) * | 2017-08-17 | 2018-01-19 | 华中科技大学 | The Laser Photoacoustic composite detection method and its system of a kind of element and defect |
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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 |
| CN113970540A (en) * | 2021-09-09 | 2022-01-25 | 华南师范大学 | Element isotope analysis system and method based on laser-induced plasma |
| CN113970540B (en) * | 2021-09-09 | 2023-07-04 | 华南师范大学 | Elemental isotope analysis system and method based on laser-induced plasma |
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