CN103123320A - Laser-induced breakdown spectroscopy analysis method and implementation device based on single-light beam splitting - Google Patents
Laser-induced breakdown spectroscopy analysis method and implementation device based on single-light beam splitting Download PDFInfo
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- CN103123320A CN103123320A CN2012104893919A CN201210489391A CN103123320A CN 103123320 A CN103123320 A CN 103123320A CN 2012104893919 A CN2012104893919 A CN 2012104893919A CN 201210489391 A CN201210489391 A CN 201210489391A CN 103123320 A CN103123320 A CN 103123320A
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Abstract
The invention discloses a laser-induced breakdown spectroscopy analysis method and implementation device based on single-light beam splitting. The implementation device comprises a laser source, a laser beam splitting device, a straight optical transmission device, a bypass optical transmission device, an optical fiber detector, an optical spectrometer and a data analyzer, which are correspondingly connected through optical paths, wherein the laser beam splitting device is used for splitting a laser beam emitted from the laser source into two laser beams; one laser beam is vertically incident onto the surface of a sample after being focused by the straight optical transmission device, and the other laser beam is incident onto the surface of the sample by focusing after the laser incident angle is adjusted through the bypass optical transmission device to be an angle coincident with an action point of the vertical incident laser on the surface of the sample; the two laser beams stimulate the sample to generate plasmas; the optical fiber detector for collecting the plasmas is connected with the optical spectrometer through an optical fiber; a plasma emission spectrum is coupled into the optical spectrometer; the optical spectrometer is used for transmitting the collected spectrum data to the data analyzer through a USB (Universal Serial Bus) data wire; and the data analyzer is used for detecting and analyzing sample components to obtain sample component information.
Description
Technical field
The invention belongs to field of spectral analysis technology, relate to a kind of laser spectral analysis technology, especially a kind of Laser-induced Breakdown Spectroscopy analytical technology that produces twin-beam based on single beam beam splitting technology is specifically related to a kind of double light beam laser induced breakdown spectroscopy analytical approach and device for carrying out said thereof.
Background technology
Laser-induced Breakdown Spectroscopy (Laser Induced Breakdown Spectroscopy, LIBS) technology is a kind of New type atom Emission Spectroscopy, this technology is fast by feat of detection speed, simultaneous determination of multiponents, possess on-the-spot original position analysis ability and need not the complicated advantages such as sample pre-treatments, is widely used in the numerous areas such as oil-gas mining, geologic prospecting, metallurgical electric power and environmental monitoring.The sensitivity that it is lower and higher detection limit had become the bottleneck of restriction LIBS technical development, therefore obtained numerous LIBS researchist's great attention but in recent years.Solution for problems mainly comprises at present:
1. based on the auxiliary signal Enhancement Method of microwave: the method adds microwave energy around testing sample, by changing the living environment of laser induced plasma, realized the enhancing to the LIBS spectral signal;
2. based on the auxiliary signal Enhancement Method of effluve: the method adds two high-field electrodes at the laser induced plasma place, realizes secondary excitation by the effluve plasma, has realized the enhancing to the LIBS spectral signal;
3. based on the signal Enhancement Method of laser dipulse: the method utilizes two laser instruments and a chronotron to produce two laser pulses with certain time delay (Microsecond grade), by two laser pulses priorities and sample or laser induced plasma effect, realize the secondary excitation of plasma, promoted the intensity of LIBS spectral signal.
Above-mentioned solution is in the intensity that has promoted in varying degrees the LIBS spectral signal, although implementation method is different, but its ultimate principle belongs to a class together, the additional energy that namely provides based on second excitaton source (such as microwave, effluve, pulse laser etc.), increase the launching efficiency of laser induced plasma, and then reach the sensitivity that promotes LIBS and the purpose that reduces detection limit.This shows, the condition precedent that this type of scheme realizes is: increase an excitaton source in original LIBS system, for plasma provides extra excitation energy.Yet the excitaton source that increases will be extra device or the annex (such as microwave cavity, microwave generator, high-voltage pulse power source, laserresonator, pumping lamp water cooling plant etc.) of LIBS system's increase, such device or annex, volume is large, complex structure and expensive, will certainly increase the complexity that realizes cost and experimental provision of LIBS system, this will be unfavorable for the propagation and employment of LIBS Signal Enhanced Technology and relevant apparatus.
Summary of the invention
For the present situation of above-mentioned existing LIBS Signal Enhanced Technology and the problem of existence, purpose of the present invention aims to provide a kind of new Laser-induced Breakdown Spectroscopy analytical approach and device for carrying out said thereof, the mode that strengthens to enrich the LIBS signal, overcome the device for carrying out said complex structure that existing LIBS Signal Enhanced Technology exists, the problems such as installation cost height.
double light beam laser induced breakdown spectroscopy analytical approach provided by the invention, the formation of its technical scheme mainly comprises: a laser pulse of lasing light emitter emission is divided into transmission laser and reflector laser two bundle laser, a branch of in two bundle laser is the forthright excitation laser, line focus impinges perpendicularly on sample surfaces and produces plasma, another Shu Jiguang is the bypass excitation laser, incide sample surfaces generation plasma through incident angle adjustment and focusing to be angle β with the vertical incidence excitation laser, and this incident excitation laser overlaps with the application point of vertical incidence excitation laser on sample surfaces at the application point on sample, utilize fibre-optical probe with the emission spectrum coupled into optical fibres of the plasma of generation, and be transferred to spectrometer and data-analyzing machine carries out spectral analysis, finally obtain the composition information of testing sample.
In technique scheme, described transmission laser and reflector laser all can be used as vertical incidence excitation laser or skew back incident excitation laser.Two bundle excitation lasers incide angle β on sample surfaces greater than 0
0Less than 90
0The scope effect that has the LIBS signal to strengthen, but preferably be controlled at 20
0~ 80
0Between.
the apparatus structure that is used for the double light beam laser induced breakdown spectroscopy method of enforcement the present invention proposition, the lasing light emitter that mainly comprises the corresponding connection of light path, the laser beam splitter device, the forthright optical transmission apparatus, the bypass optical transmission apparatus, and fiber-optical probe, spectrometer and data-analyzing machine, described laser beam splitter device is divided into two bundle laser with the beam of laser of lasing light emitter emission, wherein beam of laser impinges perpendicularly on sample surfaces after being focused on by the forthright optical transmission apparatus, another Shu Jiguang adjusts laser incident angle to the angle and the line focus that overlap with the application point of vertical incidence laser on sample surfaces by the bypass optical transmission apparatus and incides sample surfaces, the two common excited sample of bundle laser produce plasma, the fiber-optical probe that detection window is aimed at plasma is connected with spectrometer by optical fiber, plasma emission spectroscopy is coupled into spectrometer, spectrometer is transferred to data-analyzing machine by the usb data line with the spectroscopic data that gathers sample composition is detected analysis.
Owing to the present invention relates to a kind of laser spectrum quasi-instrument, for the ease of the relation between each device of statement, be " light input interface " with incident light direction and the node definition of device, be " light output interface " with emergent light direction and the node definition of device, when " the light output interface " of " the light input interface " of previous device and a rear device that is right after when being connected, the direction that represents the light beam that previous device is exported is identical with the light beam incident direction of a rear device, and by the incident node.according to above-mentioned definition, device for carrying out said of the present invention also can be described as: " the light output interface " of lasing light emitter is connected with " the light input interface " of laser beam splitter device, the laser beam splitter device is divided into forthright excitation laser and bypass excitation laser two bundle laser with this Shu Jiguang, wherein " the light output interface " of forthright excitation laser is connected with " the light input interface " of forthright optical transmission apparatus, " the light output interface " of bypass excitation laser is connected with " the light input interface " of bypass optical transmission apparatus, the laser action of " the light output interface " of forthright optical transmission apparatus and bypass optical delivery output same point to the sample surfaces, and generation plasma, the detection window of fiber-optical probe is aimed at plasma, and be connected with spectrometer through optical fiber, plasma emission spectroscopy is coupled into spectrometer, and spectrometer is transferred to data-analyzing machine by the usb data line with the spectroscopic data that gathers, and completes the analysis to sample composition.
In the technical scheme of above-mentioned device for carrying out said, the lasing light emitter preferred energy is burnt greater than 30 millis, wavelength is the pulse laser of 1064nm, the wavelength of lasing light emitter can be also the pulse laser of 532nm, 355nm or 266nm, as long as the energy of single bundle of pulsed laser is burnt greater than 30 millis, the wavelength of concrete lasing light emitter is selected and energy selects to depend on actual demand.
In the technical scheme of above-mentioned device for carrying out said, described laser beam splitter device is made of a laser beam splitter mirror that possesses the first mirror holder of spinfunction and be placed on mirror holder.The mirror holder that wherein possesses spinfunction is responsible for fixedly beam splitter, and changes the angle α of beam splitter axis and incident laser, wherein α ∈ (0 °, 90 °) by spinfunction.Beam splitter is responsible for the beam of laser pulse that lasing light emitter produces is divided into forthright excitation laser and bypass excitation laser two bundle laser, and the laser energy (due to the variation of angle [alpha], beam splitter can lose certain energy) of two after beam splitting bundle laser energy summation before less than or equal to beam splitting.
In the technical scheme of above-mentioned device for carrying out said, described forthright optical transmission apparatus is f by a burnt length
1The first condenser lens and the second mirror holder form, by the second mirror holder, first lens is fixed on sample surfaces top f
1The place, its purpose is in order to guarantee that the first condenser lens focus is at sample surfaces.
In the technical scheme of above-mentioned device for carrying out said, described bypass optical transmission apparatus is f by the first catoptron, burnt length at least
2The second condenser lens, to settle the 3rd mirror holder of the first catoptron, the 4th mirror holder, the radius that the second condenser lens is installed be R
1The first circular arc type track and radius be R
2The second circular arc type track form, described the 3rd mirror holder movably is arranged on the first circular arc type track, described the 4th mirror holder movably is arranged on the second circular arc type track, and the 3rd mirror holder and the 4th mirror holder are the mirror holder with spinfunction, and the radius R of the second circular arc type track
2With the burnt long f of the second condenser lens
2Unanimously, be used for ensureing that the focus of the second condenser lens is at sample surfaces.Namely in this device, when the first catoptron be used for to change the bypass excitation laser and incides sample surfaces and the angle β of sample surfaces vertical direction, β ∈ (20 ° 80 °); The burnt long f of the second condenser lens
2, be responsible for focusing on the bypass excitation laser, for the focus after the focusing that guarantees the bypass excitation laser overlaps (application point that definition forthright excitation laser focuses on rear and sample surfaces is initial point) with initial point, so R
2=f
2The center of circle of described the first circular arc type track and described the second circular arc type track preferably overlaps.
In the technical scheme of above-mentioned device for carrying out said, for adapt to the bypass laser that emits from the laser beam splitter device can not glancing incidence to the situation of the first catoptron, described bypass optical transmission apparatus preferably is designed with the bypass excitation laser and adjusts light path, described adjustment light path can be by the second catoptron, the 3rd catoptron, the 5th mirror holder and the 6th mirror holder that the second catoptron and the 3rd catoptron possess spinfunction is installed respectively forms, two catoptrons pass through the rotation change angle of mirror holder separately, and then realize the adjustment of bypass laser position.The second catoptron and the 3rd catoptron are preferably and be arranged in parallel.The position height of the position height of described the 3rd catoptron and the first catoptron preferably is consistent.
In the technical scheme of above-mentioned device for carrying out said, fiber-optical probe is used for collecting two bundle laser-produced plasma emission spectrum, and the spectrum of collecting is advanced spectrometer by coupling fiber; Spectrometer is used for gathering the collected spectrum of fiber-optical probe, and is translated into electric signal, is transferred to data-analyzing machine by the usb data line; Data-analyzing machine is used for calculating, analyzes and process the electric signal that spectrometer transmits, and shows by the spectrum of display with this sample at last.
optical delivery scheme such as Fig. 3 of the invention process device, Fig. 4 or shown in Figure 6, lasing light emitter produces the beam of laser pulse, be divided into a branch of forthright excitation laser and a branch of bypass excitation laser after beam splitter, wherein the forthright excitation laser is after the first condenser lens, perpendicular to sample surfaces incident, the bypass excitation laser changes transmission path through the second catoptron and the 3rd catoptron, and incide the first catoptron from horizontal direction, laser through the first mirror reflects incides the second condenser lens, finally focus on sample surfaces, and focus point overlaps with the application point of sample with the forthright excitation laser of vertical incidence.In whole optical delivery scheme, when β numerical value changes, the optics that needs to adjust comprises the second catoptron, the 3rd catoptron, the first catoptron and the second condenser lens, and detailed adjusting is described as follows, and wherein the space structure schematic diagram of these mirrors is as shown in Figure 5:
1. the regulative mode of the second catoptron: the effect of this catoptron is to realize the position adjustments of bypass excitation laser, before the explanation control method, need to calculate a critical angle, the laser of definition lasing light emitter emission is d with respect to the level height of sample surfaces, when not using the second catoptron to change bypass excitation laser level height, the angle β of the laser that the first catoptron reflects and forthright excitation laser
0=arccos (d/R
1), therefore as β＜β
0The time, need to the raise level height of bypass excitation laser of the Main Function of the second catoptron is as shown in the second catoptron in Fig. 3; Work as β〉β
0The time, the Main Function of the second catoptron need to reduce the level height of bypass excitation laser, and as shown in the second catoptron in Fig. 4, adjustment process is completed by the 4th mirror holder in the bypass optical transmission apparatus.
2. the regulative mode of the 3rd catoptron: the effect of this catoptron is to change the transmission path of bypass excitation laser, the purpose of its path changing is to make bypass excitation laser along continuous straight runs to incide the first catoptron, therefore the relative and keeping parallelism of the reflecting surface of the second catoptron and the 3rd catoptron, the height of the height of the 3rd catoptron and the first catoptron is consistent.
3. the regulative mode of the first catoptron: the effect of the first catoptron is to change the transmission path of bypass excitation laser, and the purpose of its path changing is to make the bypass excitation laser to incide sample surfaces according to predetermined angle β.Because the incident laser of the first catoptron is horizontal direction, according to the triangle geometry principle, the angle of the reflector laser of the first catoptron and incident laser is 90 °-β so, then according to principle of reflection as can be known, the axis of the first catoptron and the angle of horizontal direction are (45 °-β/2).Other the first catoptron is with respect to the level height h of sample surfaces
1, can calculate according to the triangle geometry principle equally, result of calculation is h
1=R
1Cos β.According to above-mentioned result of calculation, by spinfunction and the first circular arc type track of the second mirror holder, adjust the angle and height of the first catoptron.
4. the regulative mode of the second condenser lens: the effect of the second condenser lens is the reflector laser of the first catoptron is focused on, principle of work according to condenser lens, the position of the second condenser lens should guarantee that incident laser is through the geometric center of lens, and along the Propagation of these lens, so according to the triangle geometry principle, the axis of the second condenser lens and the angle of vertical direction are β, the height h of the second condenser lens
2=R
2Cos β.According to above-mentioned result of calculation, by spinfunction and the second circular arc type track of the 3rd mirror holder, adjust the angle and height of the second condenser lens.
The present invention compares with existing LIBS dipulse analytical technology on implementation method, has very outstanding difference in essence aspect the ultimate principle of its realization and Optical System Design, is described as follows:
1, ultimate principle is different.Existing LIBS Signal Enhanced Technology all realizes that by excitaton source of extra increase the LIBS signal strengthens, no matter this excitaton source is microwave, high-voltage power supply or laser pulse, all need to increase an excitaton source than basic LIBS system, the required energy of system has nearly increase at double.And the Enhancement Method that the present invention proposes, it is the single-pulse laser that basic LIBS system is produced, be divided into two bundle laser, the energy summation of this two bundles laser is less than or equal to the single-pulse laser energy before beam splitting, can find out, system capacity required for the present invention is identical with basic LIBS system, need not extra excitaton source, so the present invention all is better than existing LIBS Signal Enhanced Technology greatly on the cost of device and structure complexity.
2, overcome one of the prior art and be familiar with mistaken ideas.The Optical System Design scheme of present existing dipulse technology mainly comprises two classes: 1. vertical collinearity, and namely two laser pulses successively incide sample surfaces from vertical direction; 2. right-angled intersection, namely a laser pulse is perpendicular to sample surfaces incident, and another laser pulse is parallel to sample surfaces incident.Existing document all shows with actual test, when such scheme all requires be not less than 2 microsecond two time delays between laser pulse, just can produce obvious humidification to LIBS spectrum wire size, if time delay too short (less than 1 microsecond), the LIBS spectral signal not only can not strengthen, the trend that can occur weakening on the contrary.And twin-beam of the present invention is produced by a laser pulse, only determined by the optical path difference of two bundle laser the interval time that two bundle laser arrive sample surfaces, the optical path difference of two bundle laser is generally less than 1 meter, namely the interval time of two bundle laser arrival sample surfaces will be less than 5 nanoseconds (being far smaller than 1 microsecond), as seen by the understanding of prior art, the monopulse double-beam technique that the present invention proposes is that the LIBS spectral signal is strengthened.But the inventor is by deep research and discovery, change existing dipulse design proposal, a brand-new double-pulse laser incident path geometric model is proposed, i.e. the first bundle laser vertical sample surfaces incident, and the second bundle laser and the first bundle laser incident from the side at an angle, through experimental verification, the geometric model that the present invention proposes is not in the situation that two bundle laser almost have delay (less than 5 nanoseconds) can realize equally the enhancing of LIBS spectral signal.
3, device for carrying out said is simple in structure, and cost of manufacture is low.Device for carrying out said of the present invention only has a lasing light emitter, lifting LIBS spectral signal intensity device for carrying out said compared to prior art, increase an excitaton source in original LIBS system, for plasma provides extra excitation energy, saved an excitaton source and supporting device or annex with it.Increase an excitaton source, the LIBS system need be equipped with a plurality of servicing units or annex simultaneously, as microwave cavity, microwave generator, high-voltage pulse power source, laserresonator, pumping lamp water cooling plant etc., and this type of servicing unit or accessory structure are complicated, expensive, volume is larger, has therefore greatly increased the manufacturing cost of LIBS system and device and the complexity of experimental provision, is unfavorable for the propagation and employment of LIBS Signal Enhanced Technology and relevant apparatus.
Description of drawings:
Fig. 1 is device for carrying out said one-piece construction schematic block diagram of the present invention;
Fig. 2 is the laser beam splitter apparatus structure schematic diagram in device for carrying out said;
Fig. 3 is the optical delivery conceptual design figure (β＜β 0) of device for carrying out said of the present invention;
Fig. 4 is the optical delivery conceptual design figure (β〉β 0) of device for carrying out said of the present invention;
Fig. 5 is the locus schematic diagram of optical mirror slip in the bypass optical transmission apparatus;
Fig. 6 is with the device for carrying out said optical delivery conceptual design figure of transmission laser as the vertical incidence excitation laser;
Fig. 7 is the Mirror frame structure schematic diagram that possesses spinfunction;
When Fig. 8 was two bundle excitation laser incident angle β=60 °, two bundle excitation lasers strengthened design sketch with the spectral signal of common activated plasma respectively;
When Fig. 9 was two bundle excitation laser incident angle β=30 °, two bundle excitation lasers strengthened design sketch with the spectral signal of common activated plasma respectively.
The object that in above-mentioned accompanying drawing, each shown by reference numeral table is known is respectively: the 1-lasing light emitter; 2-laser beam splitter device; 3-forthright optical transmission apparatus; 4-bypass optical transmission apparatus; The 5-fiber-optical probe; The 6-spectrometer; The 7-data-analyzing machine; The 8-beam splitter; 9-forthright excitation laser; 10-bypass excitation laser; 11-the first condenser lens; 12-the second catoptron; 13-the 3rd catoptron; 14-the first catoptron; 15 first circular arc type tracks; 16-the second focus lamp; 17-the second circular arc type track; The 18-sample; 19-mirror holder external frame; 20-mirror holder inner frame; 21-mirror holder swingle; 22-mirror holder fixed screw.
Embodiment:
Provide specific embodiments of the invention below in conjunction with accompanying drawing, and by embodiment, the present invention is further described specifically.Be necessary to point out at this, the following examples just are used for setting forth better principle of work of the present invention and practical application thereof, so that the technician in other field is used for the present invention the various facilities in its field, and improve according to the imagination of various special-purposes.Although the present invention discloses its first-selected embodiment by word; but but can understand wherein optimization and alterability by reading these technology explanatory notes; and improve not departing from scope and spirit of the present invention, but such improvement should still belong to the protection domain of claim of the present invention.
Embodiment
The present embodiment is used for measuring the device of solid sample composition, and its structured flowchart installs the optical delivery conceptual design as shown in Figure 3 and Figure 4 as shown in Figure 1.with wavelength 1064nm, single beam laser pulse energy 100mJ, the Nd:YAG laser instrument of pulse width 8ns is lasing light emitter 1, the pulse laser of lasing light emitter emission is divided into a branch of forthright excitation laser 9 and a branch of bypass excitation laser 10 through after beam splitter 8, wherein the forthright excitation laser is after the first condenser lens 11, perpendicular to the surperficial incident of sample 18, and focus is positioned at sample surfaces, the bypass excitation laser is through the second catoptron 12, make its beam Propagation path from left to right change into vertical direction from bottom to up by horizontal direction, and incide the 3rd catoptron 13, make its beam Propagation path change into from bottom to up horizontal direction from left to right by vertical direction, and incide the first catoptron 14, laser through the first catoptron 14 reflections incides the second condenser lens 16, and focus on sample surfaces, and focus overlaps with the focus that the forthright excitation laser converges to sample surfaces, acting in conjunction due to two bundle laser, can produce plasma at sample surfaces, the emission spectrum of plasma is collected by fiber-optical probe 5, and be coupled to spectrometer 6 and carry out data acquisition and photosignal and transform, finally be transferred to data-analyzing machine 7 by the usb data line and carry out spectrum analysis.Wherein the second catoptron, the 3rd catoptron, the first catoptron and the second condenser lens are arranged on the second mirror holder, the 3rd mirror holder, the 4th mirror holder and the 5th mirror holder successively, mirror holder possesses spinfunction, its structure as shown in Figure 7, external frame 19 is used for mirror holder and is fixed on other poles, inner frame 20 is used for installing catoptron or condenser lens, swingle 21 is used for rotating inner frame, to reach the angle of inclination of adjusting eyeglass on inner frame, after fixed screw 22 is screwed down, angle of inclination that can the fixing internal framework.In the adjustable optical mirror slip of these angles, the second catoptron and the 3rd catoptron just need to carry out angular setting when this device is built, in case device is built complete, when beginning to carry out analytical test, need not to adjust angle, only need to carry out angular adjustment to the first catoptron and the second condenser lens, to reach the incident angle that changes bypass excitation laser and forthright excitation laser.
The operating process of adopting double light beam laser induced breakdown spectroscopy analytical equipment of the present invention to measure solid sample can be divided into following three phases:
1. preparatory stage: before the experiment beginning, at first according to above-mentioned optical delivery scheme, adjust the angle of inclination of beam splitter, the second catoptron and the 3rd catoptron, and by fixed screw, the pitch angle of these three optical mirror slips is fixed.Then solid sample to be measured is carried out compressing tablet, and adjust the sample surfaces height by sample stage, make the focus of the upper surface of sample and the first condenser lens in same level.
2. parameter arranges the stage: the angle β when forthright excitation laser preassigned according to experiment condition and bypass excitation laser incide sample surfaces, and the control method of above-mentioned the first catoptron and the second condenser lens, calculating the axis of the first catoptron and the angle of horizontal direction is that (45 °-β/2), the first catoptron are R with respect to the height of sample surfaces
1The axis of cos β, the second condenser lens and the angle of vertical direction are that β, the second condenser lens are R with respect to the height of sample surfaces
2Cos β, and adjust the first catoptron and the second condenser lens according to result of calculation, then start laser instrument, and the first catoptron and the second condenser lens are finely tuned at the first circular arc type track 15 and the second circular arc type track 17, overlap at sample surfaces with the focus point of guaranteeing two bundle laser.Experimental specific requirement arranges the experiment parameters such as energy, repetition frequency, spectrometer integral time, spectrometer time delay and average testing time of laser instrument.
3. analytical test stage: when Preparatory work of experiment stage and parameter arrange the stage complete after, start laser instrument and send a synchronizing signal to spectrometer, open forthright optical transmission apparatus 3 and bypass optical transmission apparatus 4, make forthright excitation laser and bypass excitation laser almost focus on simultaneously same point on sample surfaces, the spectral analysis software of operational data analysis device is analyzed the spectrogram that obtains, store.
In order further to set forth the present invention in the advantage aspect the enhancing of LIBS signal, the below is take the standard model (GBW03104) of shale as example, and provides concrete experiment parameter and the result of this experiment.Si in selected shale is element to be measured, and the wavelength of its atomic emissions characteristic spectral line is 288.15nm; The running parameter of laser instrument and spectrometer: single beam laser pulse energy 100mJ, laser instrument repetition frequency 5Hz, spectrometer 3ms integral time, spectrometer signals collecting μ s time delays 3.5, data average time 50 times; Angle β when forthright excitation laser and bypass excitation laser incide sample surfaces is chosen as respectively 30 ° and 60 °.Under these conditions, when β=60 °, beam splitter is replaced with catoptron, open the forthright optical transmission apparatus, close the bypass optical transmission apparatus, only use the forthright excitation laser excited sample of vertical direction, the test result of average 50 times, and the data of preservation spectrometer collection, Z=3 curve in experimental result such as Fig. 8; Remove beam splitter, open the bypass optical transmission apparatus, close the forthright optical transmission apparatus, only use bypass excitation laser excited sample, the test result of average 50 times, and preserve the data that spectrometer gathers, Z=2 curve in experimental result such as Fig. 8; Recover the installation of beam splitter, open simultaneously forthright optical transmission apparatus and bypass optical transmission apparatus, use forthright excitation laser and the acting in conjunction of bypass excitation laser at sample surfaces, the test result of average 50 times, and the data of preservation spectrometer collection, Z=1 curve in experimental result such as Fig. 8 can be found out method provided by the invention and device for carrying out said, can effectively strengthen the LIBS signal.
For the incident angle β that proves forthright excitation laser and bypass excitation laser strengthens the impact of effect on LIBS, the β angle of above-mentioned experiment condition is set to 30 °, and repeat above-mentioned analytical test step, experimental result as shown in Figure 9, wherein only use the forthright excitation laser excitation result of vertical direction to be the Z=3 curve, only use bypass excitation laser excitation result to be the Z=2 curve, open simultaneously forthright optical transmission apparatus and bypass optical transmission apparatus, use forthright excitation laser and the acting in conjunction of bypass excitation laser at sample, acquired results is the Z=1 curve.By comparison diagram 8 and Fig. 9, can find out, the different enhancing effects that can affect spectral line of the angle of two bundle laser, this is also the purpose that changes two bundle excitation laser incident angles.
The invention is not restricted to embodiment mentioned above, the suitable modification of carrying out on architecture basics of the present invention and optimization are as long as the scope that defines in claim all belongs to category of the present invention.
Claims (11)
1. Laser-induced Breakdown Spectroscopy analytical approach based on the single beam beam splitting, it is characterized in that: the beam of laser pulse of lasing light emitter emission is divided into transmission laser and reflector laser two bundle laser, a branch of in two bundle laser is the forthright excitation laser, line focus impinges perpendicularly on sample surfaces and produces plasma, another Shu Jiguang is the bypass excitation laser, incide sample surfaces generation plasma through incident angle adjustment and focusing to be angle β with the forthright excitation laser, and this incident laser overlaps with the application point of forthright excitation laser on sample surfaces at the application point on sample, utilize fibre-optical probe with the emission spectrum coupled into optical fibres of the plasma of generation, and be transferred to spectrometer and data-analyzing machine carries out spectral analysis, finally obtain the composition information of testing sample.
2. the Laser-induced Breakdown Spectroscopy analytical approach based on the single beam beam splitting according to claim 1, is characterized in that the angle β that two bundle excitation lasers incide on sample surfaces is 20
0~ 80
0
3. implement the device of the described Laser-induced Breakdown Spectroscopy analytical approach based on the single beam beam splitting of claim 1 or 2, it is characterized in that mainly comprising the lasing light emitter (1) of the corresponding connection of light path, laser beam splitter device (2), forthright optical transmission apparatus (3), bypass optical transmission apparatus (4), and fiber-optical probe (5), spectrometer (6) and data-analyzing machine (7), described laser beam splitter device is divided into two bundle excitation lasers with the beam of laser of lasing light emitter emission, wherein a branch of excitation laser impinges perpendicularly on sample surfaces after being focused on by the forthright optical transmission apparatus, another bundle excitation laser is adjusted laser incident angle to the angle and the line focus that overlap with the application point of forthright excitation laser on sample surfaces by the bypass optical transmission apparatus and is incided sample surfaces, the two common excited sample of bundle excitation laser produce plasma, the fiber-optical probe that detection window is aimed at plasma is connected with spectrometer by optical fiber, plasma emission spectroscopy is coupled into spectrometer, spectrometer is transferred to data-analyzing machine by the usb data line with the spectroscopic data that gathers sample composition is detected analysis.
4. the Laser-induced Breakdown Spectroscopy analytical equipment based on the single beam beam splitting according to claim 3, is characterized in that described lasing light emitter is that energy is not less than 30 milli Jiao, wavelength is the pulse laser of 1064nm, 532nm, 355nm or 266nm.
5. the Laser-induced Breakdown Spectroscopy analytical equipment based on the single beam beam splitting according to claim 3, is characterized in that described laser beam splitter device (2) is made of a laser beam splitter mirror (8) that possesses the first mirror holder of spinfunction and be placed on mirror holder.
6. the Laser-induced Breakdown Spectroscopy analytical equipment based on the single beam beam splitting according to claim 3, is characterized in that described forthright optical transmission apparatus is f by a burnt length
1The first condenser lens and the second mirror holder form, by the second mirror holder, first lens is fixed on sample surfaces top f
1The place.
One of according to claim 3 to 6 described Laser-induced Breakdown Spectroscopy analytical equipment based on the single beam beam splitting, it is characterized in that described bypass optical transmission apparatus (4) by at least one first catoptron (14), burnt long be f
2The second condenser lens (16), the 3rd mirror holder that the first catoptron is installed, the 4th mirror holder, the radius that the second condenser lens is installed be R
1The first circular arc type track (15) and radius be R
2The second circular arc type track (17) form, described the 3rd mirror holder movably is arranged on the first circular arc type track (15), described the 4th mirror holder movably is arranged on the second circular arc type track (17), and the radius R of the second circular arc type track
2With f
2Unanimously, the 3rd mirror holder and the 4th mirror holder are the mirror holder with spinfunction.
8. the Laser-induced Breakdown Spectroscopy analytical equipment based on the single beam beam splitting according to claim 7, it is characterized in that described bypass optical transmission apparatus (4) also is provided with the bypass excitation laser and adjusts light path, this adjustment optical routing second catoptron (12), the 3rd catoptron (13), the 5th mirror holder and the 6th mirror holder the second catoptron and the 3rd catoptron being installed and being possessed spinfunction respectively form, two catoptrons pass through the rotation change angle of mirror holder separately, and then realize the adjustment of bypass excitation laser position.
9. the Laser-induced Breakdown Spectroscopy analytical equipment based on the single beam beam splitting according to claim 8, is characterized in that the second catoptron (12) and the 3rd catoptron (13) that described bypass excitation laser is adjusted in light path be arranged in parallel.
10. the Laser-induced Breakdown Spectroscopy analytical equipment based on the single beam beam splitting according to claim 9, is characterized in that the position height of described the 3rd catoptron (13) and the position height of the first catoptron (14) are consistent.
11. the Laser-induced Breakdown Spectroscopy analytical equipment based on the single beam beam splitting according to claim 7 is characterized in that the center of circle of described the first circular arc type track (15) and described the second circular arc type track (17) overlaps.
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