CN104406942B - A kind of multi-mode laser induced breakdown spectroscopy device - Google Patents
A kind of multi-mode laser induced breakdown spectroscopy device Download PDFInfo
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- 238000002536 laser-induced breakdown spectroscopy Methods 0.000 title claims abstract description 32
- 239000007787 solid Substances 0.000 claims abstract description 44
- 230000003595 spectral effect Effects 0.000 claims abstract description 42
- 238000002679 ablation Methods 0.000 claims abstract description 14
- 238000003303 reheating Methods 0.000 claims abstract description 8
- 238000012545 processing Methods 0.000 claims abstract description 6
- 238000006073 displacement reaction Methods 0.000 claims description 25
- 230000003287 optical effect Effects 0.000 claims description 15
- 230000000452 restraining effect Effects 0.000 claims description 13
- 239000013307 optical fiber Substances 0.000 claims description 11
- 238000012544 monitoring process Methods 0.000 claims description 10
- 230000001960 triggered effect Effects 0.000 claims description 10
- 101000694017 Homo sapiens Sodium channel protein type 5 subunit alpha Proteins 0.000 claims description 8
- 238000003384 imaging method Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 6
- 238000002310 reflectometry Methods 0.000 claims description 6
- 229910052724 xenon Inorganic materials 0.000 claims description 6
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 6
- 230000009194 climbing Effects 0.000 claims description 4
- 230000005284 excitation Effects 0.000 claims description 2
- 238000005286 illumination Methods 0.000 claims 1
- 239000000523 sample Substances 0.000 description 88
- 238000001514 detection method Methods 0.000 description 14
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- 239000004411 aluminium Substances 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/718—Laser microanalysis, i.e. with formation of sample plasma
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Abstract
The invention discloses a kind of multi-mode laser induced breakdown spectroscopy device, with conllinear, reheating, three kinds of mode of operations of pre-ablation;In conllinear mode of operation:The light path of Double-impulse solid laser is climbed system provided with light path, and the light path of laser is coaxially exported for raising 1064nm/532nm so that laser focuses on sample surfaces directly over sample stage, produces plasma;In reheating and pre-ablation mode of operation:The first laser of Double-impulse solid laser is climbed system, the light path for raising first laser into light path so that first laser focuses on sample surfaces directly over sample stage, produces plasma;Delay time generator controls the triggering sequential of first laser and second laser;The second laser of Double-impulse solid laser directly focuses to plasma;Also include signal acquisition and processing system, the characteristic spectral line sent is cooled down according to plasma and first laser impacts the spatial information of sample, distributed intelligence of the display elements in sample surfaces.
Description
Technical field
The present invention relates to laser spectrum tech field, more particularly to a kind of multi-mode laser induced breakdown spectroscopy device.
Background technology
LIBS is Laser-Induced Breakdown Spectroscopy (laser induced breakdown spectrograph) abbreviation,
Plasma ablation that the technology is produced using pulse laser simultaneously excites material in sample (normally solid), and pass through spectrum
Instrument obtains the spectrum that Plasma-Atomic launched that is excited, and recognizes the element constituent in sample with this, and then can be with
Carry out identification, classification, the qualitative and quantitative analysis of material.The technology can be realized quickly without being pre-processed to sample
Remotely, it is micro- damage sample element (especially metallic element) is detected, available for solid, gas, fluid sample detection.Swash
The application field of photoinduction breakdown spectral is also quite varied, heavy metal analysis in such as biomedicine, archaeology, environmental monitoring, water
And explosive detection etc..
Compared with single-pulse laser induced breakdown spectroscopy, double-pulse laser induced breakdown spectrum can greatly enhance signal, carry
The detection limit of high element.The mode of operation of double-pulse laser induced breakdown spectrum can be divided into conllinear formula and rectilinear.It is rectilinear again
Pre-ablation pattern (pre-ablative) and reheat mode (re-heating) can be divided into.These three modes are each have their own excellent
Point.However, the domestic and international three kinds of mode of operations that there is no Patents to realize LIBS on same device.
In general, the realization of these three mode of operations needs two systems.Such as patent application CN101620183B and specially
Profit application CN102788772B realizes conllinear and non-colinear mode of operation with dual pulse welding and two lasers respectively.
Also patent utilization light path realizes a certain working method with a laser, but its effect does not reach making for LIBS technologies
With requiring.The induced with laser spectrum detection system that dipulse such as patent application CN103323435A defocuses pre-ablation utilizes 2 tunnels
Light path realizes the conllinear dipulse mode of operations of LIBS, but its beam of laser and the sequential of the second beam laser are uncontrollable,
Optimal spectral line can not be obtained.Although and the LIBS measurement apparatus described in patent application CN103529000A
Vertical operation pattern is realized using the single tunnel light path of laser 2, but is usually Millisecond using the control time of optical shutter,
The control requirement of LIBS Microsecond grades can not be realized.
The content of the invention
The integrated of three kinds of mode of operations of LIBS is realized on same device to realize, the invention discloses
A kind of multi-mode laser induced breakdown spectroscopy device, reduces system building cost, simple with regulation, and it is excellent that adjustable parameter is more etc.
Point.
The concrete technical scheme of the present invention is as follows:
A kind of multi-mode laser induced breakdown spectroscopy device, it is characterised in that including Double-impulse solid laser, sample stage
With the delay time generator for controlling Double-impulse solid laser triggering sequential;Double-impulse solid laser has 1064nm coaxial
Output, 532nm are coaxially exported, the different axle outputs of 1064nm and the different axle of 1064nm, 532nm export four kinds of way of outputs;
Described multi-mode laser induced breakdown spectroscopy device has conllinear, reheating, three kinds of mode of operations of pre-ablation;
In described conllinear mode of operation:The light path of the Double-impulse solid laser is climbed system provided with light path, should
Light path climbs system for raising the light path that 1064nm/532nm coaxially exports laser so that laser is focused on directly over sample stage
To sample surfaces, plasma is produced;
In described reheating and pre-ablation mode of operation:The first laser of the Double-impulse solid laser enters described
Light path climb system, the light path is climbed the light path that system is used to raise first laser so that first laser by sample stage just on
Side focuses on sample surfaces, produces plasma;During the triggering of described delay time generator control first laser and second laser
Sequence;The second laser of the Double-impulse solid laser directly focuses to plasma;
Also include signal acquisition and processing system, the characteristic spectral line sent is cooled down according to plasma and first laser is impacted
The spatial information of sample, distributed intelligence of the display elements in sample surfaces.
The present invention is built using a kind of Double-impulse solid laser (Lei Bao companies, Vlite200) and subsequent optical path system
Realize 3 kinds of mode of operations of LIBS, and a variety of operation wavelengths switching.With pre-ablation, reheat and
Conllinear Three models mode, wherein line mode have 2 operation wavelengths (532nm and 1064nm), and pre-ablation and reheating also have 2
Individual operation wavelength (2 tunnels are 1064nm, and 1064nm all the way, another road 532nm).
Energy attenuator is there also is provided on the optical axis of described Double-impulse solid laser and for detecting that record swashs in real time
The laser energy real-time monitoring system of light energy;Described first laser enters light after laser energy real-time monitoring system outgoing
Road is climbed system;Described second laser focuses to plasma after laser energy real-time monitoring system outgoing.Laser energy
Real-time detecting system is mainly used in the energy of detection recording laser in real time, for subsequent data analysis.
When being detected using LIBS, sample properties to be detected are different, the laser energy needed for it
Also it is different.To realize the detection of the fragile sample of such as plant leaf blade, animal tissue or reducing damage of the laser to sample, generally need
The energy of laser is decayed.However, laser energy can be caused not to energy progress decay by adjusting laser diode voltage
It is stable, and then influence testing result.The present invention is decayed using energy attenuator to laser energy, and its attenuation range is 1%
~99%.Laser energy real-time detecting system is mainly used in the energy of detection recording laser in real time, for judging energy of lasers
Fluctuation whether there is exception, and carry out subsequent data analysis., can be right according to energy variation when subsequently carrying out data analysis
The intensity of spectral line of acquisition is compensated.
Wherein, described signal acquisition and processing system includes:Optical fiber collection system, for collecting plasma cooling hair
The characteristic spectral line gone out;Beam splitting system, for carrying out light splitting to characteristic spectral line;ICCD detectors, for the light of beam splitting system to be believed
Number be converted to electric signal;Sample surface imaging system, for monitoring first laser impact sample position, obtains the space of sampled point
Information;Computer, according to the spatial information of described electric signal and sampled point, distributed intelligence of the display elements in sample surfaces.
It is preferred that, described beam splitting system is echelle spectrometer.
Echelle spectrometer is the spectrometer using echelle grating as dispersion element, can one without raster scanning
Secondary property obtains full modal data, is avoided that conventional spectrograph multichannel head and the tail section Bonding Problem.Nothing inside echelle spectrometer
Mechanical part, stability is higher, and resolution ratio can reach 0.08nm, can meet spectral line light splitting requirement.
Wherein, described sample surface imaging system includes:LED light source for illuminating for illuminating sample from positive direction, position
Beam splitter on LED light source for illuminating optical axis, CCD camera and imaging lens, the sample surfaces figure for gathering beam splitter reflection
As information.
It is preferred that, described light path climb system by the first speculum, the second speculum and the 3rd speculum group into described
Second speculum is located at the surface of the first speculum, and the 3rd speculum is located at the surface of sample stage;The first described reflection
Mirror, the second speculum and the 3rd speculum are Nd:YAG double-frequency laser speculums.
The light path system of climbing is mainly used in lifting light path, and laser will be converted into and vertically propagate in the horizontal direction.
Can be prevented effectively from rise laser positions using the light path system of climbing causes the laser factors of instability.Laser is directly over sample
Sample surfaces are impacted, are conducive to effectively exciting for plasma, it is ensured that plasma is uniformly and symmetrically distributed.
Described delay time generator control Double-impulse solid laser adjusts Q triggered times and xenon lamp to open the triggered time, prolongs
When generator set Double-impulse solid laser adjust Q signal triggered time xenon lamp signal triggering after 150 ± 20 μ s.This when
The setting of sequence can at utmost ensure the energy stability of Double-impulse solid laser.
It is preferred that, first laser and the second laser focusing is arranged on along the lens that optical axis is slidably matched with lens and installed
On frame;Described first laser light path focusing plates V-arrangement film with lens surface, and its reflectivity at 532nm, 1064nm is less than
0.25%.
The distance of lens and sample is the important parameter of LIBS, directly affects laser in object to be excited
Laser parameter.As a rule, the distance of lens and sample should be less than the focal length of lens.When lens and sample distance reduce,
The diameter of impact point will increase, and radiancy and fluence can reduce.Therefore, lens are arranged on to slide along optical axis and matched somebody with somebody
The Lens mounting carrier of conjunction can be according to sample properties and the distance of actual demand accurate adjustment lens and sample.Due to dipulse solid
The optical maser wavelength of laser is 532nm and 1064nm, to reduce loss of the laser energy in light path system, it is ensured that laser energy
Effective rate of utilization, described lens surface plating V-arrangement film, its reflectivity 532nm, 1064nm at is less than 0.25%.Described
Lens plating V-arrangement film can effectively for selected Double-impulse solid laser wavelength, make its reflection at 532nm, 1064nm
Rate is less than 0.25%.
As an improvement, described sample stage includes the electric displacement platform with four-degree-of-freedom, the liter being movably arranged on electric displacement platform
Drop plate and the objective table being slidably fitted on electric displacement platform;The lifter plate is provided with transparent constraint window, laser light constraint
Sample is impacted after window;The lower section of the lifter plate is provided with restraining plate, and the restraining plate, which is placed on the surface of sample, restraining plate, to be divided
Cloth Constrained chamber, the constraint chamber is used for the plasma for constraining sample excitation.
Sample stage limits enhanced line intensity by space, and energy plasma is laterally and row constraint, and root are entered in longitudinal direction
The big minor adjustment the intensity of spectral line of constraint space is adjusted according to different sample requirements, the intensity of spectral line enhancing scope is 2~10 times.Constrain window
Mouth is mainly used in plasma and longitudinally enters row constraint, and the characteristic spectral line produced to incident laser and plasma has preferably
Transmissivity.The transverse direction that restraining plate is mainly used in plasma enters row constraint, and characteristic spectral line is carried out constraint propagation, improves
Spectral line collection efficiency and the intensity of spectral line.
It is preferred that, described lifter plate is provided with light-transmitting opening, the light-transmitting opening covered with light-passing board, the light-transmitting opening with thoroughly
The described constraint window of tabula rasa composition.
Wherein, light-passing board is poly (methyl methacrylate) plate, and the selection of material is N-BK7, and thickness is 1~5mm, and transmitance is more than 90%,
Energy threshold is more than 10J/cm2.Line enhancement effect suffers restraints window from the influence with a distance from sample.By properties of samples and institute
The element spectral line intensity to be detected is different, and constraint window of the invention can be moved in vertical direction, as needed regulation spectrum
Line strength.To ensure that laser effectively excites effective collection with characteristic spectral line, light-passing board is saturating to optical maser wavelength and characteristic spectral line
The rate of mistake should be greater than 90%.Meanwhile, to prevent laser from being caused damage to poly (methyl methacrylate) plate, its energy threshold should be greater than 10J/cm2。
Restraining plate is the aluminium sheet of chromium plating, and thickness is 1~3mm.Aluminium sheet constraint intracavitary carry out chromium plating, make inner chamber have compared with
High reflectivity, makes characteristic spectral line constraint propagation, improves spectral line collection efficiency.
The Double-impulse solid laser that the present invention is used, its energy hole is realized by energy attenuator, it is to avoid utilize voltage
Directly regulation causes energy of lasers unstable.Laser is adjusted using sample stage and the Lens mounting carrier that can be moved along optical axis direction
Running parameter.First mode of operation is conllinear mode of operation, and delay time generator control first laser launches sequential in second laser
Before transmitting, it is only necessary to control the displacement of sample stage Z-direction to adjust the spot size of Laser Focusing point.Second mode of operation is to add again
Thermal technology's operation mode, delay time generator control first laser transmitting sequential controls sample stage, adjusts Z before second laser transmitting
Direction displacement height, makes second laser (1064nm) light-emitting window higher than 1 ± 0.5mm above plasma confinement plate, regulation first,
Second lens group mounting bracket controls the spot size of Laser Focusing point.3rd mode of operation is pre-ablation mode of operation, delay hair
Raw device control first laser transmitting sequential controls sample stage, adjusts Z-direction displacement height after second laser transmitting, makes the
Dual-laser (1064nm) light-emitting window adjusts first, second lens group mounting bracket higher than 1 ± 0.5mm above plasma confinement plate
Control the spot size of Laser Focusing point.Because the shape and characteristic of sample have differences, sample stage uses 4DOF (X, Y, Z
And W) sample stage, including 3 single-degree-of-freedom (X, Y and Z) pulse electric displacement platforms and rotary freedom (W) electronic rotation
Platform.When sample is spherical (such as apple, pear and other fruits), from whole frees degree;When sample surfaces are regular planar, select
XYZ Three Degree Of Freedoms can meet requirement.
The invention has the advantages that:
(1) three kinds of mode of operations of double-pulse laser induced breakdown spectrum are realized, for selection optimum working mode detection
Sample elements content provides condition.
(2) the real-time monitoring to laser energy is realized, is conducive to improving the repeatability of detection technique.
(3) distance and laser energy of lens and object according to different samples, can be adjusted, optimal noise is obtained
Than.
(4) sample stage limits enhanced line intensity by space, and energy plasma is laterally and row constraint is entered in longitudinal direction, carries
High spectral line collection efficiency and the intensity of spectral line, are avoided that and excite particle to cover sample surfaces again, and smooth sample surfaces are (especially
Such as fresh blade out-of-flatness sample), the distance of sample to condenser lens is kept constant repeated so as to improve detection.
Brief description of the drawings
Fig. 1 is the structure chart of multi-mode laser induced breakdown spectroscopy device;
Fig. 2 is the structure chart of sample stage;
Fig. 3 is the top view of sample stage in Fig. 2;
Fig. 4 is the schematic diagram that sample is impacted on sample stage;
Fig. 5 is unconfined plasma figure;
Fig. 6 is the constraints graph with constraint window and constraint chamber plasma.
Embodiment
As shown in figure 1, the multi-mode laser induced breakdown spectroscopy device in the present invention includes:Double-impulse solid laser 1,
Delay time generator 2, energy attenuator 3, laser energy real-time monitoring system 4, light path is climbed system 5, ICCD detectors 6, light splitting
System 7, the second condenser lens 8, sample stage 9, the first condenser lens 10, optical fiber collection system 11, sample surface imaging system 12.
Double-impulse solid laser 1 has 4 kinds of mode of operations:(1) 1064nm is coaxially exported, and (2) 532nm is coaxially exported,
(3) the different axle outputs of 1064nm, the different axle outputs of (4) 1064nm, 532nm.Double-impulse solid laser 1 can be by 2 pulses
1064nm solid state lasers, frequency-doubling crystal and combined beam light road are realized.
The control Double-impulse solid laser 1 of delay time generator 2 adjusts Q triggered times, xenon lamp to open triggered time and ICCD spies
Survey the gate duration of device 6.Delay time generator sets Double-impulse solid laser to adjust the triggered time of Q signal to be triggered in xenon lamp signal
150 ± 20 μ s afterwards, detector controls the opening time to be 1.5 μ s (detectors after the second road laser Q-switching switch triggering time
The control opening time need to be optimized according to signal to noise ratio).
Variable energy attenuator 2 is made up of 1/2 wave plate 31 and the first beam splitter 32.Laser energy monitors reponse system in real time
It is made up of the 41, second beam splitter 42 of thermoelectric pulse probe, USB connecting lines, computer 13.The laser to be monitored is by 3:7 points
Shu Jing separates 30% laser energy, is popped one's head in and received by thermoelectric pulse, computer is connected to by USB connecting lines, special soft
The energy of recording laser is shown on part in real time, for subsequent data analysis.
Light path system 5 of climbing is made up of the first speculum 52, the second speculum 51 and the 3rd speculum 53.First speculum
52nd, the second speculum 51 and the 3rd speculum 53 are from 1 inch of double frequency Nd:YAG laser mirrors, 532, the reflection at 1064nm
Rate is more than 98%.
First condenser lens 10 and the second condenser lens 8 are installed on the Lens mounting carrier for having the free degree along optical axis direction
In, for adjusting the distance of sample and lens, so as to control impact to the laser parameter on sample.
Optical fiber collection system 11 is made up of light collector and optical fiber.Sample surface imaging system 12 include CCD camera 124,
Imaging lens 123, the 3rd beam splitter 122, LED light source for illuminating 121.
Beam splitting system 7 is echelle spectrometer.First condenser lens 10 and the second condenser lens 8 select N-BK7, plating
V-arrangement film, its reflectivity at 532,1064nm is less than 0.25%.
As shown in Figure 2, Figure 3 and Figure 4, sample stage 9 includes gear rack elevating bar 901, gear slider 902, right angle pinboard
903, plasma confinement window 904, cylindrical guide 905, plasma confinement plate 906, V-type sliding block 907 combines electric displacement platform
909, pull bar 910 constrains chamber 911.Electric displacement platform 909 is combined using four-degree-of-freedom (x, y, z, w) combination electric displacement platform, including three lists
The free degree (x, y and z) pulse electric displacement platform and rotary freedom (w) electric rotary table.Gear rack elevating bar 901 is pacified vertically
On combination electric displacement platform 909, gear slider 902 is engaged with gear rack elevating bar 901, can vertically be moved up and down.Right angle
Pinboard 903 is secured by bolts on gear slider 902, and plane is provided with the light-transmitting opening of rectangle, and light-transmitting opening edge is provided with support
Light-passing board is provided with step, light-transmitting opening, plasma confinement window 904 is formed.Cylindrical guide 905 is fixed on combination electric displacement platform
909, plasma confinement plate 906 can be slided up and down along cylindrical guide 905.Cylindrical guide 905 and gear rack elevating bar 901 pass through
Bolt-connection is on combination electric displacement platform 909.Combination electric displacement platform 909 is provided with V-groove, and V-type sliding block 907 can under the effect of pull bar 910
Horizontally slipped along V-groove, pull bar 910 is threadably secured in V-type sliding block 907.Sample 908 places V-type sliding block 907 (quite
In objective table) on, laser is impacted down from above, by plasma confinement window 904, and passes through plasma confinement plate
906, sample surfaces are arrived in impact, excite plasma, and cooling sends characteristic spectral line and collected by optical fiber collection system 11.
The material of plasma confinement window 904 is N-BK7, and thickness is 1~5mm, and transmitance is more than 90%, energy threshold
More than 10J/cm2.Plasma confinement window 904 is mainly used in plasma and longitudinally enters row constraint, and to incident laser with
The characteristic spectral line that plasma is produced has preferable transmissivity.N-BK7 is a kind of common optical glass, can be passed through
The light of 350nm~2000nm wave bands, the transmissivity of its laser is more than 90%, and energy threshold is more than 10J/cm2.Therefore plasma
It is N-BK7 to constrain the selection of material of window 904, and thickness is 1~3m.Plasma confinement window 904 can be acted in gear slider 902
Under vertically move.Line enhancement effect suffers restraints window from the influence with a distance from sample.Due to properties of samples and
The element spectral line intensity to be detected is different, and plasma confinement window 904 of the invention can be moved in vertical direction, root
According to need adjust the intensity of spectral line.
In the present embodiment, the material of plasma confinement plate 906 is the aluminium sheet of chromium plating, and thickness is 1mm, and it is middle uniform
Cone constraint chamber 911 is furnished with, upper conical surface diameter and lower conical surface diameter are 2mm and 3mm respectively.Distance should between constraining chamber 911
It is consistent with combining the planning displacement of electric displacement platform 909.The transverse direction that plasma restraining plate 6 is mainly used in plasma enters row constraint,
And characteristic spectral line is carried out constraint propagation, spectral line collection efficiency and the intensity of spectral line are improved, the intensity of spectral line enhancing scope is 2~10
Times.Chromium plating is carried out in the constraint chamber 911 of aluminium sheet, makes inner chamber that there is higher reflectivity, makes characteristic spectral line constraint propagation, is improved
Spectral line collection efficiency.Constraint chamber uses conical structure, and due to its up-small and down-big structure, the structure compared with cylindrical type can be more preferably
Obtain plasma and enter row constraint.In addition, when plasma is projected from cone constraint chamber, because its space constraint is increased,
Its electron density can be strengthened with movement velocity, therefore advantageously in the enhancing of spectral line signal.The plasma of the present invention
Distance is consistent with combining the planning displacement of electric displacement platform 909 between the constraint chamber of body restraining plate 906, can be suitably used for laser-induced breakdown
The working method of spectrum Surface scan.Using plasma restraining plate 906 of the present invention covers sample surfaces, is conducive to smooth sample table
Detection repeatability is improved in face, while avoiding exciting the other regions to be measured of particle contamination.When testing sample is the surfaces such as fresh blade
During out-of-flatness sample, its region to be measured has differences with lens distance, and then influences the laser parameter of laser arrival sample.Laser
The detection stability and the laser parameter in region to be detected of induced breakdown spectroscopy are closely bound up, therefore smooth sample surfaces are conducive to
Fixed laser parameter improves the repeatability of detection.In addition, the up-small and down-big conical structure of plasma confinement plate 906 is conducive to
Farthest avoid exciting particle contamination by a upper detection zone, it is ensured that detect the element that object is region to be detected.
V-type sliding block 907 can be moved under the effect of pull bar 910 along V-groove, using this V-type sliding block guide track structure, it is to avoid rise
The troublesome operation such as plasma confinement window mouthful and plasma restraining plate.Company between plasma confinement plate 906 and cylindrical guide 905
It is connected in be close to and connects, plasma confinement plate 906 can not freely glides under gravity.
So that LIBS system reheats mode of operation as an example, when this sample stage works, control combination electromigration
Platform 909 makes the pyramid type constraint chamber 911 of plasma confinement plate 906 corresponding with the position of top laser, sets combination electromigration
The work step-length of platform 909 is cone constraint chamber neighbor distance or multiple.Beam of laser B passes through light path system, and line focus is saturating
Mirror is propagated down from above, through plasma confinement window 904, and by cone constraint chamber impact sample.Plasma
Its laser transmittance for constraining window 904 is more than 90%, and energy threshold is more than 10J/cm2.Second beam laser A vertically leads to
Over-focusing lens focus is impacted onto the plasma inspired, enhanced line signal.Plasma cooling sends characteristic spectral line C
Collected by the optical fiber collection system 11 of top.The number of times that each position can be impacted according to needed for being selected actual requirement, when completion one
After individual position multiple position spectra collections are carried out by combining the movement of electric displacement platform 909.As shown in Figure 5 and Figure 6, when without plasma
When body constrains window 904 and plasma confinement plate 906, the plasma D inspired is free excited state;When to exciting
After plasma D is limited, plasma D density increase, plasma temperature rise enhances the spectral line of excited atom
Intensity.
Double-impulse solid laser 1 sends pulse laser, by the damping capacity of energy attenuator 3, by optical system, hits
Get on sample, plasma is formed when energy density is higher than the threshold value excited, plasma cooling sends different wave length
Characteristic spectral line, is collected via optical fiber collection system 11, by beam splitting system 7, is detected by ICCD detectors 6, and in computer 13
Upper display processing.The device can realize that 3 kinds of mode of operations and different operating wavelength are cut by adjusting output laser and light path
Change.Conllinear (collinear) that tri- kinds of different mode of operations of dipulse LIBS refer to, pre-ablation (pre-ablative), again plus
Hot (re-heating).
Mode of operation 1 (conllinear):The mode of operation of Double-impulse solid laser 1 is coaxial 532nm or coaxial 1064nm, electricity
Brain control delay time generator 2 gives the modulating signal of Double-impulse solid laser 1 and adjusts Q signal, and Double-impulse solid laser 1 starts work
Make.Laser sequentially passes through the first speculum 52 (532nm/1064nm) and second speculum 51 (532nm/1064nm) improving laser
Light path;Adjusting the reflector mount of the second speculum 51 makes laser be located above sample, and light path is changed through the 3rd speculum 53, to
It is lower to propagate.Laser focuses on sample surfaces via plating the first condenser lens of V film glass 10, when laser energy density is higher than what is excited
During threshold value, sample produces plasma, and plasma cooling, atom occurs transition, produces the characteristic spectral line for characterizing element.Spectral line
Collected, via beam splitting system 7 (echelle spectrometer) light splitting, converted by ICCD detectors 6 by optical fiber collection system 11
For electric signal, it is connected to by USB in computer 13, carries out data statistics and analysis in computer 13, determine certain in sample
The content of material.
Mode of operation 2 (reheating):The mode of operation of Double-impulse solid laser 1 is different axle 532nm/1064nm, 1064nm
Output, computer control delay time generator 2 awards the modulating signal of Double-impulse solid laser 1 and adjusts Q signal, Double-impulse solid laser
1 starts working.First laser (532nm/1064nm) sequentially passes through the first speculum 52 (532nm/1064nm) and the second reflection
The light path of mirror 51 (532nm/1064nm) improving laser;Adjusting the reflector mount of the second speculum 51 makes laser be located on sample
Side, changes light path through the 3rd speculum 53 (532nm/1064nm), propagates downwards.Laser is focused on via plating V film glass first
Mirror 10 focuses on sample surfaces, and when laser energy density is higher than the threshold value excited, sample produces plasma.Control sample stage
9, Z-direction displacement height is adjusted, second laser (1064nm) light-emitting window is higher than 9061 ± 0.5mm of plasma confinement plate.The
Dual-laser (1064nm) is focused on by the second condenser lens of plating V film glass plano-convex 8, focuses on the plasma signal ejected
On, enhanced line signal.Spectral line is collected by optical fiber collection system 11, via beam splitting system 7 (echelle spectrometer) point
Light, electric signal is converted into by ICCD detectors 6, is connected to by USB in computer 13, computer 13 carry out data statistics with
Analysis, determines the content of the material of certain in sample.
Mode of operation 3 (pre-ablation):The mode of operation of Double-impulse solid laser 1 is different axle 532nm/1064nm, 1064nm
Output, computer control delay time generator 2 awards the modulating signal of Double-impulse solid laser 1 and adjusts Q signal, Double-impulse solid laser
1 starts working.Sample stage 9 is controlled, Z-direction displacement height is adjusted, second laser (1064nm) light-emitting window is higher than plasma
9061 ± 0.5mm of restraining plate.Second laser (1064nm) is focused on by the second condenser lens of plating V film glass plano-convex 8, focuses on sample
Top, can lead to inert gas.First laser (532nm/1064nm) sequentially pass through the first speculum 52 (532nm/1064nm) and
The light path of second speculum 51 (532nm/1064nm) improving laser;Adjusting the reflector mount of the second speculum 51 is located at laser
Above sample, change light path through the 3rd speculum 53 (532nm/1064nm), propagate downwards.Laser is via plating V film glass first
Condenser lens 10 focuses on sample surfaces, and when laser energy density is higher than the threshold value excited, sample produces plasma.Spectral line
Optical fiber collection system 11 is collected, and via beam splitting system 7 (echelle spectrometer) light splitting, electricity is converted into by ICCD detectors 6
Signal, is connected in computer 13 by USB, is carried out data statistics and analysis in computer 13, is determined the material of certain in sample
Content.
Claims (8)
1. a kind of multi-mode laser induced breakdown spectroscopy device, it is characterised in that including Double-impulse solid laser, sample stage and
For controlling Double-impulse solid laser to trigger the delay time generator of sequential;Double-impulse solid laser has 1064nm coaxially defeated
Go out, 532nm is coaxially exported, the different axle outputs of 1064nm and the different axle of 1064nm, 532nm export four kinds of way of outputs;
Described multi-mode laser induced breakdown spectroscopy device has conllinear, reheating, three kinds of mode of operations of pre-ablation;
In described conllinear mode of operation:The light path of the Double-impulse solid laser is climbed system, the light path provided with light path
System of climbing is used to raise the light path that 1064nm/532nm coaxially exports laser so that laser focuses on sample directly over sample stage
Product surface, produces plasma;
In described reheating and pre-ablation mode of operation:The first laser of the Double-impulse solid laser enters described light
Road is climbed system, and the light path is climbed the light path that system is used to raise first laser so that first laser is poly- directly over sample stage
Jiao arrives sample surfaces, produces plasma;Described delay time generator control first laser and the triggering sequential of second laser;Institute
The second laser for stating Double-impulse solid laser directly focuses to plasma;
Also include signal acquisition and processing system, the characteristic spectral line sent is cooled down according to plasma and first laser impacts sample
The spatial information of obtained sampled point, distributed intelligence of the display elements in sample surfaces;
Described light path climb system by the first speculum, the second speculum and the 3rd speculum group into second speculum
Positioned at the surface of the first speculum, the 3rd speculum is located at the surface of sample stage;Described the first speculum, the second reflection
Mirror and the 3rd speculum are double frequency Nd:YAG laser mirrors;The focusing of the first laser and second laser is installed with lens
On the Lens mounting carrier that can be slidably matched along optical axis direction;Focusing in the light path of the first laser plates V with lens surface
Shape film, its reflectivity at 532nm, 1064nm is less than 0.25%.
2. multi-mode laser induced breakdown spectroscopy device as claimed in claim 1, it is characterised in that described dipulse solid
Energy attenuator is there also is provided on the optical axis of laser and for detecting that the laser energy of recording laser energy is monitored in real time in real time
System;
Described first laser is climbed system after laser energy real-time monitoring system outgoing into light path;
Described second laser focuses to plasma after laser energy real-time monitoring system outgoing.
3. multi-mode laser induced breakdown spectroscopy device as claimed in claim 1, it is characterised in that described signal acquisition and
Processing system includes:
Optical fiber collection system, for collecting the characteristic spectral line that plasma cooling is sent;
Beam splitting system, for carrying out light splitting to characteristic spectral line;
ICCD detectors, for the optical signal of beam splitting system to be converted into electric signal;
Sample surface imaging system, for monitoring first laser impact sample position, obtains the spatial information of sampled point;
Computer, according to the spatial information of described electric signal and sampled point, distributed intelligence of the display elements in sample surfaces.
4. multi-mode laser induced breakdown spectroscopy device as claimed in claim 3, it is characterised in that described beam splitting system is
Echelle spectrometer.
5. multi-mode laser induced breakdown spectroscopy device as claimed in claim 4, it is characterised in that described sample surface into
As system includes:
For from surface to illumination sample LED light source for illuminating,
Beam splitter on LED light source for illuminating optical axis,
CCD camera and imaging lens, the sample surfaces image information for gathering beam splitter reflection.
6. multi-mode laser induced breakdown spectroscopy device as claimed in claim 1, it is characterised in that described delay time generator
Double-impulse solid laser is controlled to adjust Q triggered times and xenon lamp to open the triggered time, delay time generator sets dipulse solid to swash
The triggered time of light device tune Q signal 150 ± 20 μ s after the triggering of xenon lamp signal.
7. multi-mode laser induced breakdown spectroscopy device as claimed in claim 1, it is characterised in that described sample stage includes
Electric displacement platform with four-degree-of-freedom, the lifter plate being movably arranged on electric displacement platform and the objective table being slidably fitted on electric displacement platform;
The lifter plate impacts sample after being provided with transparent constraint window, laser light constraint window;
The lower section of the lifter plate is provided with restraining plate, and the restraining plate is placed in distribution Constrained chamber on the surface of sample, restraining plate,
The constraint chamber is used for the plasma for constraining sample excitation.
8. multi-mode laser induced breakdown spectroscopy device as claimed in claim 7, it is characterised in that set on described lifter plate
There is light-transmitting opening, covered with light-passing board at the light-transmitting opening, the light-transmitting opening constitutes described constraint window with light-passing board.
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EP3510376B1 (en) * | 2016-09-08 | 2024-02-14 | FOSS Analytical A/S | Method for performing laser induced breakdown spectroscopy |
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CN113916787B (en) * | 2021-10-19 | 2023-05-26 | 西安电子科技大学 | Multimode laser-induced breakdown spectroscopy device |
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Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US8310671B1 (en) * | 2010-09-29 | 2012-11-13 | The United States Of America As Represented By The Administrator Of National Aeronautics And Space Administration | Interference-free optical detection for Raman spectroscopy |
CN102841078A (en) * | 2012-09-10 | 2012-12-26 | 北京宝瑞光电科技有限公司 | Integrated laser-induced enhanced plasma spectrum acquisition system |
CN103529000A (en) * | 2013-10-17 | 2014-01-22 | 中国科学院西安光学精密机械研究所 | Single-light-source dual-wavelength laser-induced breakdown spectroscopy measurement device and method |
CN203894165U (en) * | 2014-06-09 | 2014-10-22 | 江西农业大学 | Collinear double-pulse laser-induced breakdown spectroscopy (LIBS) technology-based device for rapidly detecting benzopyrene content in edible oil |
CN104142316A (en) * | 2014-08-15 | 2014-11-12 | 中国科学院上海技术物理研究所 | Pre-ablation and reheating combined triple-pulse LIBS (laser-induced breakdown spectroscopy) detection system |
CN204214778U (en) * | 2014-11-17 | 2015-03-18 | 浙江大学 | A kind of multi-mode laser induced breakdown spectroscopy device |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2011006156A2 (en) * | 2009-07-10 | 2011-01-13 | University Of Florida Research Foundation, Inc. | Method and apparatus to laser ablation-laser induced breakdown spectroscopy |
US20120314214A1 (en) * | 2011-06-07 | 2012-12-13 | Alexander Dennis R | Laser Induced Breakdown Spectroscopy Having Enhanced Signal-to-Noise Ratio |
-
2014
- 2014-11-17 CN CN201410653808.XA patent/CN104406942B/en active Active
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US8310671B1 (en) * | 2010-09-29 | 2012-11-13 | The United States Of America As Represented By The Administrator Of National Aeronautics And Space Administration | Interference-free optical detection for Raman spectroscopy |
CN102841078A (en) * | 2012-09-10 | 2012-12-26 | 北京宝瑞光电科技有限公司 | Integrated laser-induced enhanced plasma spectrum acquisition system |
CN103529000A (en) * | 2013-10-17 | 2014-01-22 | 中国科学院西安光学精密机械研究所 | Single-light-source dual-wavelength laser-induced breakdown spectroscopy measurement device and method |
CN203894165U (en) * | 2014-06-09 | 2014-10-22 | 江西农业大学 | Collinear double-pulse laser-induced breakdown spectroscopy (LIBS) technology-based device for rapidly detecting benzopyrene content in edible oil |
CN104142316A (en) * | 2014-08-15 | 2014-11-12 | 中国科学院上海技术物理研究所 | Pre-ablation and reheating combined triple-pulse LIBS (laser-induced breakdown spectroscopy) detection system |
CN204214778U (en) * | 2014-11-17 | 2015-03-18 | 浙江大学 | A kind of multi-mode laser induced breakdown spectroscopy device |
Non-Patent Citations (1)
Title |
---|
Dual-Pulse LIBS Using a Pre-ablation Spark for Enhanced Ablation and Emission;DIMITRA N. STRATIS et al.;《APPLIED SPECTROSCOPY》;20001231;第54卷(第9期);1271 * |
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