CN101696936A - Laser induced discharge reinforcement plasma spectrum detection device - Google Patents
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- CN101696936A CN101696936A CN200910154015A CN200910154015A CN101696936A CN 101696936 A CN101696936 A CN 101696936A CN 200910154015 A CN200910154015 A CN 200910154015A CN 200910154015 A CN200910154015 A CN 200910154015A CN 101696936 A CN101696936 A CN 101696936A
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- 238000001514 detection method Methods 0.000 title claims abstract description 32
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- 230000002787 reinforcement Effects 0.000 title claims abstract description 20
- 239000000523 sample Substances 0.000 claims abstract description 16
- 239000013307 optical fiber Substances 0.000 claims abstract description 7
- 238000007405 data analysis Methods 0.000 claims abstract description 4
- 238000002536 laser-induced breakdown spectroscopy Methods 0.000 abstract description 31
- 238000000034 method Methods 0.000 abstract description 21
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Abstract
The invention belongs to the technical field of plasma spectrum detection, in particular to a laser induced discharge reinforcement plasma spectrum detection device. The laser induced discharge reinforcement plasma spectrum detection device comprises an incidence unit, a signal reception unit, an object carrying platform and a data analysis unit, wherein the incidence unit comprises a YAG laser and a lens, and the signal reception unit comprises a probe, an optical fibre and a spectrograph. The laser induced discharge reinforcement plasma spectrum detection device is characterized in that the plasma detection device is provided with a signal reinforcement unit which comprises a high-voltage quick-discharge loop. The invention not only inherits various advantages of the traditional LIBS technique but also has the characteristics of stronger signal intensity, lower sample detection limit, higher stability and the like; compared with a DP-LIBS technique and an LIBS-LIF technique, the invention has simple equipment of a detection system, easy operation, lower cost and better practicability.
Description
Technical field
The invention belongs to plasma spectrum detection technique field, specifically is a kind of laser induced discharge reinforcement plasma spectrum detection device.
Background technology
(laser-induced breakdown spectroscopy, LIBS), a kind of as atomic emission spectrum is a kind of spectrum detection technique that rose gradually in recent years to Laser-induced Breakdown Spectroscopy.The LIBS technology can detect various forms of samples such as solid, liquid, powder, gas simultaneously, also is unique spectral technique that can detect multiple constituent content in any environment simultaneously.The LIBS technology also has fast, in real time, need not sample preparation, little loss, multielement and characteristics such as analyze simultaneously.At present, LIBS The Application of Technology field is extensive, comprises that traditional chemical analysis also has environmental monitoring, industrial on-line measurement, biotechnology, historical relic's protection, nuclear industry, survey of deep space, Marine Sciences, surface analysis etc.
Traditional LIBS system sends laser beam by the Nd:YAG Q-switched laser, converges in the testing sample surface through lens, makes it the surface and goes up micro substance gasification, ionization, excites, and forms high-temperature plasma; Collect the spectral line of the element of plasma emission by optical system, be coupled to spectrometer through optical fiber; Spectrometer is transferred to spectroscopic data in the computing machine and handles.
But in actual applications, LIBS detects and has the deficiency that sensitivity is lower, detection limit is too high, has limited more deep development and the application widely of this technology.For giving full play to the technical advantage of LIBS, the intensity of enhancing signal and reduction LIBS detection limit are the important development directions of LIBS technology
From improving the intensity of LIBS spectral signal, abroad some researchers have proposed the double-pulse laser shooting techniques, i.e. the DP-LIBS technology.Double-pulse laser excites and is meant that several nanoseconds to two laser pulses in succession of tens of microseconds of being separated by affact on the same position that is examined material.The dipulse technology has very big advantage than monopulse technology in spectral detection, such as: can improve laser greatly to the melting and excite of material, strengthen line strength of plasma, thereby reduce the detection limit etc. of spectral analysis.In addition, the Laser-induced Breakdown Spectroscopy technology also can effectively improve the sensitivity that trace materials detects in conjunction with laser-induced fluorescence spectroscopy technology (LIBS-LIF).But no matter be DP-LIBS technology or LIBS-LIF technology have also increased detection system greatly when improving the detection effect complicacy, for example the DP-LIBS Technology Need has two Nd:YAG Q-switched lasers and corresponding light path corollary system, adjust comparatively difficulty of the coaxial or quadrature of two bundle laser simultaneously, need the professional to operate, this makes the LIBS system increase the complicacy and the cost of its debugging in actual applications.
Summary of the invention
The present invention is directed to above-mentioned the deficiencies in the prior art, provide a kind of induced with laser-discharge reinforcement plasma spectrum detection device (laser ablation-electric discharge plasma spectroscopy, LA-EDPS).Use the plasma spectrum of this device to detect, both inherited every advantage of traditional LIBS technology, have stronger signal intensity, lower sample detection limit and the characteristics such as stability of Geng Gao again,, easy operating simple than DP-LIBS technology and LIBS-LIF technology for detection system equipment, and cost is lower, and better practicality is arranged.
Concrete technical scheme of the present invention is:
Laser induced discharge reinforcement plasma spectrum detection device, comprise the incident unit formed by YAG laser instrument and lens, by signal receiving unit, objective table and data analysis unit that probe, optical fiber, spectrometer are formed, it is characterized in that described plasma pick-up unit is provided with the signal enhancement unit that the fast discharge loop of a high pressure is formed.
Described signal enhancement unit comprises direct supply, high-voltage diode, inductance, electric capacity and the discharger of being made up of two sparking electrodes, described discharger is with after electric capacity is in parallel, connect with inductance and high-voltage diode, the positive pole of described high-voltage DC power supply connects the positive pole of high-voltage diode, minus earth.
The spacing of described two sparking electrodes is 5mm~6mm, and described capacitance is 6nF, and the voltage range of direct supply is 0kv~30kv.
Described sparking electrode is a sphere pole.
Further, the spacing of two sparking electrodes is 5-6mm normally, the voltage range of direct supply be 0 to 30kv adjustable, link to each other with two sparking electrodes with inductance through high-voltage diode, the circuit minus earth, at the electrode electric capacity that to be parallel with a size for two sections be 6nF, inductance plays the protection power supply; The condition of electrode discharge is to discharge under the inducing of laser plasma, so must avoid the automatic discharge of electrode self, for fear of producing high electric field, causes point discharge, and the electrode that the present invention adopts should be spherical or arcuation.
The testing process of using pick-up unit of the present invention to carry out is as follows:
A branch of by the emission of above-mentioned YAG laser instrument, the laser beam mirror reflection that is reflected produces laser plasma by impinging perpendicularly on after the lens focus on the sample surfaces; Laser plasma outwards expands rapidly with the direction perpendicular to the surface of sample, wherein a part of electronics and ion enter the space between two sparking electrodes and the ablation points, electronics in these plasmas and ion have served as the preionization source, under the electrode voltage effect, produce avalanche and discharge, the quantity exponentially of charged ion is increased, electric energy in the electric capacity forms gas discharge along " V " shape path of " electrode-ablation points-electrode " then, produced bigger stronger electric spark, electric energy in the electric capacity is deposited in the discharge plasma, make that the population of high-energy state increases in the plasma; Therefore, the light intensity of plasma resonance is than adopting single laser excitation and even two laser excitation that very big enhancing is all arranged; The light that plasma sends is collected and is transferred to spectrometer by optical fiber, the radiant light that utilizes photodiode to accept plasma simultaneously forms a start pulse signal and comes triggered digital pulse daley generator to open spectrometer record experimental data; Spectrometer is sent experimental data into computing machine and is handled and analyze.
Description of drawings
Fig. 1 is a laser induced discharge reinforcement plasma spectrum detection device structural representation of the present invention
Fig. 2 is a signal enhancement unit circuit structure diagram of the present invention
Fig. 3 is the relative position synoptic diagram of sample of the present invention, laser beam and spark
Fig. 4 is a discharge current synoptic diagram of the present invention
Fig. 5 is the plasma effect synoptic diagram that laser beam produces separately
The plasma effect synoptic diagram that Fig. 6 produces for laser induced discharge
Fig. 7 is that laser induced discharge reinforcement plasma spectrum detects the spectral results comparison diagram under traditional SP-LIBS detection and the 11kv voltage of the present invention
Wherein, sparking electrode anode 1, sparking electrode negative electrode 2, lens 3, optical fiber 4.
Embodiment
The invention will be further described below in conjunction with accompanying drawing.
As Fig. 1, Fig. 2, shown in Figure 3, laser induced discharge reinforcement plasma spectrum detection device, comprise the incident unit formed by YAG laser instrument and lens 3, by signal receiving unit, objective table and data analysis unit that probe, optical fiber 4, spectrometer are formed, it is characterized in that described plasma pick-up unit is provided with the signal enhancement unit that the fast discharge loop of a high pressure is formed.
Described signal enhancement unit comprises direct supply, high-voltage diode, inductance, electric capacity and by globular discharge electrode anode 1, the discharger that sparking electrode negative electrode 2 is formed, described discharger is with after electric capacity is in parallel, connect with inductance and high-voltage diode, the positive pole of described high-voltage DC power supply connects the positive pole of high-voltage diode, minus earth.
The spacing of described two sparking electrodes is 5mm~6mm, and described capacitance is 6nF, and the voltage range of direct supply is 0kv~30kv.
Wherein, LASER Light Source is the Nd:YAG Q-switched laser, the long 1064nm of fundamental light wave, and pulsewidth is 10ns, and beam diameter is 6mm, and the monopulse laser energy is adjustable in the 20-300mJ scope.
Spectrometer is Avantes Spectrometer, and it is made up of ccd detector, miniature fiber grating, digit pulse delay generator, signal acquiring system and related software.The line array CCD detector has 4096 pixels to be formed, and adopts the external trigger mode to work.The opening time of CCD and time shutter are realized by spectrum software setting digit pulse delay generator.The digit pulse delay generator minimum exposure time that software can be provided with is 2ms, and minimum delay time is spaced apart 42ns.The spectral range of spectrometer is 200nm~500nm, and resolution is 0.1nm.
Below adopt national standard material pedotheque GBW07421 to compare detection, use for convenience and reduce error, laboratory sample is handled: the pedotheque of 5g is put into the plastic hoop of crossing with washed with de-ionized water, soil is pressed into disk with sheeter.
The energy of laser adopts 30mJ, and the repetition frequency of laser is 0.33Hz, and laser spot is positioned at the following 0.5mm of sample surfaces, and electrode is 2mm to the distance of sample room, and two distance between electrodes are 6mm.The relative position of sample, electrode and laser beam is seen Fig. 3.The voltage at electrode two ends is 11kV.Typical fast discharge current synoptic diagram when Fig. 4 is 11KV voltage, oscillating discharge cycle submicrosecond magnitude (about 0.5 microsecond), discharge times 6 microsecond.Use electronic two-dimension translational platform as objective table in experimentation, target spot is relatively stable when having guaranteed each the bombardment, to help the stable of spectral signal.
With laser induced discharge reinforcement plasma body spectrum new method and traditional SP-LIBS method continuous bombardment of pedotheque asked average for 20 times respectively according to above-mentioned condition, the data of gained are sent into computer analysis.Analysis result is as follows:
Fig. 7 adopts the pedotheque spectral results comparison diagram that induced with laser-discharge reinforcement plasma body spectrum new method and technology obtain under pedotheque spectrum that traditional SP-LIBS technology obtains and the 11kV voltage.Can find to adopt the resulting spectral line of new detection method to be greatly improved on intensity than the spectral line that classic method obtains in the comparison of two figure: traditional SP-LIBS spectral intensity coordinate range is half of the technical program.
As can be known from Table 1, in the spectrum except the stronger spectral line of several intensity, the intensity of most of spectral line, no matter be the spectral line of metallic element or the spectral line of nonmetalloid, with traditional SP-LIBS method relatively, line strength that induced with laser-discharge reinforcement plasma body spectrum new method obtains all is the former more than 20 times of gained line strength.Some more weak spectral lines in the SP-LIBS spectrum wherein use the multiple that line strength increases after the new method can reach 80 to 114 times.When the signal intensity that detects had tangible enhancing, also as can be seen, the plasma plume that produces than the classic method new method obviously became big from the comparison of Fig. 5 and Fig. 6, and brightness obviously improves.In addition, some micro-spectral lines are arranged, as As (286.04nm), Co (345.35nm), because their content is very low, the content of As is 9.4ppm in sample GBW07421, the content of Co is 9.2ppm, does not find its spectral line and can find in induced with laser-discharge spectrum in SP-LIBS spectrum.
Aspect spectral signal stable, induced with laser-discharge reinforcement plasma body spectrum new method and technology also obviously are better than traditional SP-LIBS method.
Use relative standard deviation (RSD) to weigh the stability of spectral signal in this example.In the individual spectroscopic data of bombardment, to get 20 data and be one group and average to be defined as and be one-shot measurement, the continuous coverage 20 times that uses the same method finally forms 20 spectroscopic datas.At last these 20 data are asked relative standard deviation.In table 1, the relative standard deviation of using traditional SP-LIBS method gained spectral line all is higher than 6%, and the relative standard deviation overwhelming majority of spectral line has been reduced to 2-3% after the method for employing induced with laser-discharge.
Generally speaking, induced with laser provided by the invention-discharge enhanced spectrum checkout equipment, do not needing to roll up under complex apparatus input and the prerequisite simple to operate, realized having higher signal intensity, lower sample detection limit and better signal stabilization than traditional SP-LIBS technology, this method has important use and is worth in the trace of reality or trace element detect.
Line strength of the some elements of table 1 and relative standard deviation
Claims (4)
1. laser induced discharge reinforcement plasma spectrum detection device, comprise the incident unit formed by YAG laser instrument and lens, by signal receiving unit, objective table and data analysis unit that probe, optical fiber, spectrometer are formed, it is characterized in that described plasma pick-up unit is provided with the signal enhancement unit that the fast discharge loop of a high pressure is formed.
2. laser induced discharge reinforcement plasma spectrum detection device according to claim 1, it is characterized in that described signal enhancement unit comprises direct supply, high-voltage diode, inductance, electric capacity and the discharger of being made up of two sparking electrodes, described discharger is with after electric capacity is in parallel, connect with inductance and high-voltage diode, the positive pole of described high-voltage DC power supply connects the positive pole of high-voltage diode, minus earth.
3. laser induced discharge reinforcement plasma spectrum detection device according to claim 2, the spacing that it is characterized in that described two sparking electrodes is 5mm~6mm, and described capacitance is 6nF, and the voltage range of direct supply is 0kv~30kv.
4. according to claim 2 or 3 described laser induced discharge reinforcement plasma spectrum detection devices, it is characterized in that described sparking electrode is a sphere pole.
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