CN109884034B - Method and device for detecting femtosecond plasma grating induced breakdown spectrum - Google Patents
Method and device for detecting femtosecond plasma grating induced breakdown spectrum Download PDFInfo
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Abstract
The invention relates to the technical field of element detection, in particular to a femtosecond plasma grating induced breakdown spectrum detection method and a femtosecond plasma grating induced breakdown spectrum detection device. The method combines the plasma grating in ultrafast optics with Laser Induced Breakdown Spectroscopy (LIBS), not only retains the incomparable advantages of LIBS technology such as real-time, high speed, micro-loss and full-element analysis, but also overcomes the limitation of single beam femtosecond optical fiber clamping power to a certain extent, improves the free electron density, thereby improving the element signal intensity and the detection sensitivity.
Description
Technical Field
The invention relates to the technical field of element detection, in particular to a method and a device for detecting femtosecond plasma grating induced breakdown spectroscopy.
Background
In recent years, the demand for detecting common sample elements is increasing, for example, heavy metal elements in water and soil are detected to monitor and control heavy metal pollution, and various elements in organic matters such as vegetables and tea are detected to evaluate the influence of the elements on human bodies.
Conventional analytical testing of substances typically employs sampling followed by analysis by laboratory chemical reagent processing and spectroscopic instrumentation. Although the methods have high detection accuracy, the traditional method has a long detection period and cannot perform quick and instant detection, and secondary pollution is easily caused by treatment of chemical reagents in the detection process. Recently, a series of novel detection technical methods such as a hyperspectral analysis technology, an electrochemical analysis method, a biological analysis method, a terahertz analysis method and the like combined with latest research results still have the problems of complex pretreatment, incapability of rapidly obtaining results in real time, easiness in causing secondary pollution and the like. It is very important to be able to simply pretreat and rapidly analyze the heavy metal content of the soil in real time.
Laser-Induced Breakdown Spectroscopy (LIBS) is a emerging spectrum detection technology in recent years, and compared with other spectrum technologies, the LIBS has incomparable advantages of simple sample pretreatment, real-time performance, rapidness, micro-loss, full-element analysis and the like, so that the LIBS is widely concerned and is widely applied to the fields of metallurgical analysis, environmental monitoring, geological exploration, online monitoring, national defense and the like. The method can be used for sample monitoring to perform laser-induced breakdown spectroscopy analysis only by simply processing a sample or even without processing, but has the problem of low detection sensitivity.
The traditional laser-induced breakdown spectroscopy system adopts single-beam nanosecond pulse laser or femtosecond pulse laser as a source to excite a substance. Strong reverse bremsstrahlung exists at the initial stage of plasma evolution generated by nanosecond pulse laser excitation, so that a fluorescence spectrum has strong continuous background noise, and a target signal spectrum can be covered; the influence of strong continuous spectrum can be solved by the delayed acquisition signal, but the target signal spectrum is weakened, and the final detection sensitivity is reduced; the femtosecond pulse laser excitation has no strong background spectrum, but the balance of the Kerr self-focusing effect and the plasma self-defocusing effect in the pulse laser drawing process is adopted, so that the formed optical fiber has a certain clamping power, the intensity of the signal spectrum cannot be effectively improved along with the improvement of the laser intensity due to the focusing on the surface of a sample, and the improvement of the detection sensitivity is limited. How to avoid strong background spectrum without sacrificing signal spectrum intensity and how to effectively improve the free electron density at the laser focus is the key point to improve element detection sensitivity.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention aims to provide a femtosecond plasma grating induced breakdown spectroscopy detection method, which combines the ultrafast optical plasma grating with Laser Induced Breakdown Spectroscopy (LIBS), not only retains the incomparable advantages of LIBS technology such as real-time, rapidness, micro-loss and full-element analysis, but also overcomes the limitation of single-beam femtosecond fiber clamping power to a certain extent, and improves the free electron density, thereby improving the element signal intensity and the detection sensitivity.
The invention also aims to provide a femtosecond plasma grating induced breakdown spectroscopy detection device, which converts femtosecond pulses into plasma gratings to act on a sample to be detected and induce stronger plasma fluorescence, thereby improving detection sensitivity.
The purpose of the invention is realized by the following technical scheme: a femtosecond plasma grating induced breakdown spectrum detection method is characterized in that emitted femtosecond pulse laser sequentially undergoes beam splitting, time domain synchronization and focusing to form a plasma grating with a space period modulation, and the plasma grating induced breakdown spectrum is adopted to detect a sample to be detected.
Preferably, the method comprises the following steps: (1) the laser emission module emits femtosecond pulse laser, and the femtosecond pulse laser is subjected to beam splitting by the beam splitting module to obtain beam-split pulse laser;
(2) the beam-splitting pulse laser obtained in the step (1) forms a plurality of beams of synchronous pulse laser after passing through a time domain synchronization module;
(3) the multiple beams of synchronous pulse laser obtained in the step (2) form multiple beams of synchronous optical fibers after passing through a focusing module, and the multiple beams of synchronous optical fibers are crossed in space to form a plasma grating with space period modulation;
(4) and (4) the plasma grating obtained in the step (3) acts on a sample to be detected to form a plasma fluorescence spectrum, and the plasma fluorescence spectrum is collected and detected by a spectrum collection module. In the method, femtosecond pulse laser emitted by a laser emitting module sequentially forms a plurality of beams of synchronous light wires after beam splitting, time domain synchronization and focusing, the plurality of beams of synchronous light wires are crossed in space to form a plasma grating with space period modulation, the plasma grating is acted on the surface of a sample to be detected to generate plasma cluster fluorescence containing atoms, ions or electrons of a substance to be detected, the plasma cluster fluorescence is collected and detected by a spectrum collecting module, and a spectrum signal is enhanced, so that the detection sensitivity is improved. The femtosecond laser pulse peak power in the plasma grating breaks through the limitation of the conventional femtosecond optical filament peak power clamping, generates space period modulation femtosecond laser pulse with high peak power density, acts on a sample to be detected, obtains the peak power density which is at least one magnitude higher than that of the conventional femtosecond optical filament, acts on the surface of the sample to be detected, and induces stronger plasma fluorescence. The method of the invention can overcome the adverse effect of the matrix effect on the plasma spectrum, and can realize the calibration of the concentration of the ions to be measured without a standard sample. In addition, the influence of the fluorescence background of the femtosecond plasma grating is small (the characteristic of femtosecond light, the pulse width is small), and the signal-to-noise ratio of the femtosecond plasma grating induced breakdown spectrum is high.
The multiple beams of synchronous optical fibers after time domain synchronization and focusing are crossed and interacted in space to form a plasma grating with space period modulation, which is the prior art and is not repeated again.
Preferably, in the step (1), the number of the split pulse lasers generated after the splitting is at least two.
The plasma grating comprises at least two beams of synchronous optical fibers, and the plurality of plasma gratings form a plasma grating cascade. The beam splitting module can be a plurality of modules, and the beam splitting is carried out for a plurality of times. Specifically, the femtosecond pulse laser emitted by the laser emission module is subjected to beam splitting at least once to obtain two beams of beam-split pulse laser, the two beams of beam-split pulse laser form two beams of synchronous optical fibers after time domain synchronization and focusing, and the two beams of synchronous optical fibers are crossed in space to form a plasma grating with space period modulation; the two beams of beam splitting pulse lasers can also be subjected to beam splitting for multiple times to obtain multiple beams of beam splitting pulse lasers, multiple beams of synchronous optical fibers are formed after passing through the focusing module, the multiple beams of synchronous optical fibers are crossed in space to form multiple plasma gratings modulated in a space period, and the multiple plasma gratings form a plasma grating cascade.
Preferably, in the step (4), a gas atmosphere is provided at a contact position of the plasma grating and the sample to be measured.
The auxiliary gas in the plasma grating is subjected to multi-photon ionization to induce high-density electrons, and the type, flow rate and density of the auxiliary gas are adjusted, so that the electron density in the plasma grating is adjusted by adjusting the ionization of gas molecules. Electrons generated by the auxiliary gas multi-photon ionization are driven and accelerated by high-power-density femtosecond pulse laser in the plasma grating, and the accelerated electrons collide with gas molecules in the plasma grating to further induce avalanche ionization, so that the electron density is improved. The femtosecond laser of the plasma grating and electrons accelerated by the femtosecond laser act on a sample to be detected to excite the sample to be detected, a plasma breakdown spectrum is obtained, and a spectrum signal of the plasma breakdown spectrum is enhanced, so that the detection sensitivity is improved. The high peak power laser and the accelerated electrons in the plasma grating act on the surface of a sample to be detected, and can induce and puncture superhard materials, ultra-stable oxides, ceramic materials and the like which are difficult to excite by conventional laser ablation.
Preferably, the gas is argon or/and neon. The method selects argon or neon as the gas atmosphere, so that the spectral signal of the sample to be detected can be greatly enhanced, and the air is used as the gas atmosphere, so that the spectral signal has no enhancement effect.
Preferably, the flow rate of the gas is 2-10L/min. When the flow rate of the selected gas is 2-10L/min, the spectral signal of the sample to be detected is strong, and the spectral signal of the sample to be detected is weakened due to too small or too large gas flow rate.
Preferably, the sample to be detected is one or more of solid, liquid or gas.
The space period modulation of the plasma grating acts on the liquid surface, the ablation of the periodic modulation of the plasma grating is realized on the liquid surface, and the breakdown spectrum detection is directly induced on the liquid surface.
The high peak power laser in the plasma grating and the accelerated electrons thereof act on the surface of a sample to be detected, and can induce and puncture superhard materials, ultrastable oxides, ceramic materials and the like which are difficult to excite by conventional laser ablation.
The detection method of the invention is characterized in that the sample is induced to be broken down by the plasma grating, and the detection method is not limited by the state of the sample, and particularly has the advantages of being capable of detecting ions, inert gases, heavy metal ions, molecular ions and the like which have high ionization potential and are difficult to realize direct laser excitation, obtaining the characteristic spectrum of ion emission and having wide detection range coverage.
The other purpose of the invention is realized by the following technical scheme: the utility model provides a device that femto second plasma grating induction punctures spectrum detection, includes laser emission module, beam splitting module, time domain synchronization module, focus module, year thing module and spectrum collection module along the transmission path of laser in proper order.
The femtosecond pulse laser emitted by the laser emission module forms a plasma grating modulated in a space period after beam splitting, time domain synchronization and focusing in sequence, the obtained plasma grating acts on a sample to be detected at the object carrying module, the plasma grating induces and punctures the surface of the sample to be detected to generate plasma cluster fluorescence containing atoms, ions or electrons of a substance to be detected, and the spectrum collection module collects and focuses the fluorescence spectra to obtain a detection result.
Preferably, the laser emission module is a pulse laser emission module, and the width of the light pulse is in the femtosecond magnitude; the beam splitting module is a beam splitting sheet; the focusing module is a focusing system formed by a single-chip or a plurality of focusing lenses; the spectrum collection module consists of a fluorescence collection system and a spectrometer, and the fluorescence collection system is a single focusing lens or a 4f system; the spectrometer is a high resolution spectrometer.
In the invention, the energy of the femtosecond pulse laser emitted by the laser emission module is set according to actual needs, the energy of the femtosecond pulse laser is generally 0.3-1.2mJ, the energy of two beams of synchronous optical fibers formed after primary beam splitting, time domain synchronization and focusing is 0.8-2mJ, and the highest energy of the optical fibers reaches 7-8mJ during actual operation. The beam splitting module is a beam splitting sheet or other beam splitting optical elements, the time domain synchronization module realizes the synchronization of pulses in a time domain by adjusting the same optical path of a plurality of beams of light, the focusing module is a focusing system formed by a single sheet or a plurality of sheets of focusing lenses and is used for forming light filaments by the light pulses, and the beam splitting module, the time domain synchronization module and the focusing module form a proper optical beam splitting focusing system, such as the combination of a rhomboid and a lens, or the combination of the beam splitting sheet, a stepping motor and the lens, and the like, so that two or more beams of synchronous light filaments are coupled with each other at a certain angle to form the plasma grating with the density period modulation. The carrier module is a carrier platform, and can control a sample to be tested on the carrier module to move along a preset track, so that the brand-new sample surface can be continuously excited. The spectrum collection module consists of a fluorescence collection system and a spectrometer, and the fluorescence collection system can be a single focusing lens or a 4f system; the spectrometer is a high resolution spectrometer.
Preferably, an auxiliary gas module is disposed between the carrier module and the focusing module. The auxiliary gas module can provide an auxiliary gas environment for exciting a sample to be detected by the plasma grating, and can adjust the type (such as argon, neon and the like), the flow speed, the density and other parameters of the auxiliary gas.
The invention has the beneficial effects that: the femtosecond pulse laser forms a plurality of beams of synchronous optical fibers after beam splitting, time domain synchronization and focusing to form a plasma grating structure with space period modulation, obtains peak power density which is at least one order of magnitude higher than that of the conventional femtosecond optical fibers, and the formed plasma grating acts on a sample to be detected to activate the sample to be detected, induce stronger plasma fluorescence and obtain a plasma breakdown fluorescence transition spectrum, thereby realizing the detection of elements in the sample.
The invention solves the problem that the traditional nanosecond LIBS system detects the high background signal at the initial stage of plasma evolution, the peak power of the femtosecond laser pulse in the plasma grating breaks through the limitation of the conventional femtosecond optical fiber peak power clamping, the femtosecond laser pulse with high peak power density modulated in a space period is generated and acts on a sample to be detected to obtain the peak power density which is at least one order of magnitude higher than that of the conventional femtosecond optical fiber, and the peak power density acts on the surface of the sample to be detected to induce stronger plasma fluorescence, so that the spectrum signal is enhanced, and the detection sensitivity is improved.
The method of the invention makes the plasma grating of the space period modulation structure act on the sample to be measured, overcomes the adverse effect of the matrix effect on the plasma spectrum, and can realize the calibration of the concentration of the ion to be measured without a standard sample. The sample to be detected can be solid, liquid or gas, the sample to be detected is induced to be broken down by the plasma grating, ions, inert gases, heavy metal ions, molecular ions and the like with high ionization potential and difficult realization of direct laser excitation can be detected, and the characteristic spectrum of ion emission is obtained.
The method combines the plasma grating in ultrafast optics with Laser Induced Breakdown Spectroscopy (LIBS), not only retains the incomparable advantages of LIBS technology such as real-time, high speed, micro-loss and full-element analysis, but also overcomes the limitation of single beam femtosecond optical fiber clamping power to a certain extent, improves the free electron density, thereby improving the element signal intensity and the detection sensitivity.
The femtosecond pulse laser emitted by a laser emitting module of the device is divided into a plurality of beam splitting pulse lasers with the same energy ratio through a beam splitting module, the beams are focused into a plurality of synchronous optical fibers through a time domain synchronous module, the plurality of synchronous optical fibers are adjusted to be intersected in space pairwise, two beams of synchronous optical fibers are adjusted to interfere through adjusting the time domain synchronous module to form a plasma grating, the plasma grating acts on the surface of a sample to be tested placed on a carrying module, and plasma transition fluorescence generated by the surface of the sample to be tested after being excited is collected through a spectrum collecting module, so that the analysis of component elements of the sample to be tested is realized.
Drawings
FIG. 1 is a schematic diagram of femtosecond plasma grating induced breakdown spectroscopy;
FIG. 2 is a schematic structural diagram of a grating-induced breakdown spectroscopy detection apparatus for gas-assisted femtosecond plasma;
FIG. 3 shows the results of testing a soil sample under the assistance of argon gas according to the present invention;
FIG. 4 shows the results of the soil sample testing under the assistance of neon gas in accordance with the present invention.
The reference signs are: 1. a laser emission module; 2. a beam splitting module; 3. a time domain synchronization module; 4. a focusing module; 5. a carrier module; 6. an auxiliary gas module; 7. a spectrum collection module; 8. and (5) testing the sample to be tested.
Detailed Description
For the understanding of those skilled in the art, the present invention will be further described with reference to the following examples and accompanying fig. 1, and the description of the embodiments is not intended to limit the present invention.
Example 1
The method comprises the following steps of splitting a femtosecond laser pulse with single pulse energy of 1.6mJ and repetition frequency of 1kHz by a beam splitting sheet in a ratio of 1:1, adjusting optical paths of two beams of pulses to be synchronous, then forming a light wire by the same focusing lens, adjusting spaces to intersect to form a plasma grating, acting the grating on the surface of a soil sample pressed sheet, blowing argon gas in an acting area for testing, and testing an air environment for comparison; meanwhile, the light pulses under the same conditions are not subjected to beam splitting interference, and the direct single-beam filamentation is tested under the action of the air environment to serve as comparison.
FIG. 3 shows the detection results of the present invention under several conditions, as shown in the same femtosecond pulse, the signal intensity of the action excitation test after the beam splitting, wire drawing and synchronous interference is much stronger than the test result of the single beam optical fiber action, and is enhanced by about 8 times; the signal intensity of the argon blowing test in the action area is improved by 2-3 times compared with the test result in the air environment.
Example 2
The method comprises the following steps that femtosecond laser pulse with single pulse energy of 2.3mJ and repetition frequency of 1kHz is split by a beam splitting sheet with a ratio of 1:1, then optical paths of two beams of pulse are adjusted to be synchronous, then the two beams of pulse pass through the same focusing lens to form a light wire, adjusting spaces are intersected to form a plasma grating, the grating acts on the surface of a soil sample tabletting, neon is blown in an acting area to perform testing, and an air environment is also tested to serve as comparison; meanwhile, the light pulses under the same conditions are not subjected to beam splitting interference, and the direct single-beam filamentation is tested under the action of the air environment to serve as comparison.
FIG. 4 shows the detection results of the present invention under the above conditions, where the same femtosecond pulse is shown in the figure, and the signal intensity of the action excitation test after the beam splitting, wire drawing and synchronous interference is much stronger than the test result of the single beam action, which is enhanced by about 7 times; the signal intensity of the argon blowing test in the action area is improved by 2 times compared with the test result in the air environment.
Example 3
As shown in fig. 2, a femtosecond plasma grating induced breakdown spectrum detection device structure includes a laser emission module 1, a beam splitting module 2, a time domain synchronization module 3, a focusing module 4, a carrying module 5, an auxiliary gas module 6, and a spectrum collection module 7, wherein an emergent light of the laser emission module 1 is divided into two laser beams with an energy ratio of 1:1 through the beam splitting module 2, passes through the optical path synchronization module 3 and is focused into a filament by the focusing module 4, the two laser beams are adjusted to intersect in space, the two laser beams are adjusted to have the same optical path by adjusting the optical path synchronization module 3 and then interfere to form a plasma grating, the plasma grating acts on the surface of a sample 8 to be detected placed on the carrying module 5, different types of gas environments are provided for an acting region through the auxiliary gas module 6, and plasma transition fluorescence generated by exciting the surface of the sample 8 to be detected is collected through the spectrum collection module 7, and realizing the analysis of the component elements of the tested sample.
The above-described embodiments are preferred implementations of the present invention, and the present invention may be implemented in other ways without departing from the spirit of the present invention.
Claims (6)
1. A femtosecond plasma grating induced breakdown spectroscopy detection method is characterized in that: the method comprises the following steps of sequentially carrying out beam splitting, time domain synchronization and focusing on emitted femtosecond pulse laser to form a plasma grating with a space period modulation function, and detecting a sample to be detected by adopting a plasma grating induced breakdown spectrum; the method comprises the following steps:
(1) the laser emission module emits femtosecond pulse laser, and the femtosecond pulse laser is subjected to beam splitting by the beam splitting module to obtain beam-split pulse laser;
(2) the beam-splitting pulse laser obtained in the step (1) forms a plurality of beams of synchronous pulse laser after passing through a time domain synchronization module;
(3) the multiple beams of synchronous pulse laser obtained in the step (2) form multiple beams of synchronous optical fibers after passing through a focusing module, and the multiple beams of synchronous optical fibers are crossed in space to form a plasma grating with space period modulation;
(4) the plasma grating obtained in the step (3) acts on a sample to be detected to form a plasma fluorescence spectrum, and the plasma fluorescence spectrum is collected and detected by a spectrum collection module;
in the step (4), a gas atmosphere is arranged at the contact position of the plasma grating and the sample to be detected, and the gas is argon or/and neon.
2. The femtosecond plasma grating induced breakdown spectroscopy detection method according to claim 1, wherein the method comprises the following steps: in the step (1), the number of the split pulse lasers generated after the splitting is at least two.
3. The femtosecond plasma grating induced breakdown spectroscopy detection method according to claim 1, wherein the method comprises the following steps: the flow rate of the gas is 2-10L/min.
4. The femtosecond plasma grating induced breakdown spectroscopy detection method according to claim 1, wherein the method comprises the following steps: the sample to be detected is one or more of solid, liquid or gas.
5. The utility model provides a device that femto second plasma grating induction punctures spectrum detection which characterized in that: the laser system sequentially comprises a laser emitting module, a beam splitting module, a time domain synchronization module, a focusing module, a carrying module and a spectrum collecting module along the emitting path of laser; the laser emission module emits femtosecond pulse laser, the femtosecond pulse laser is split by the beam splitting module to obtain beam splitting pulse laser, the beam splitting pulse laser forms a plurality of beams of synchronous pulse laser after passing through the time domain synchronous module, the plurality of beams of synchronous pulse laser form a plurality of beams of synchronous optical fibers after passing through the focusing module, the plurality of beams of synchronous optical fibers are crossed in space to form a plasma grating with space period modulation, the plasma grating acts on a sample to be detected, and a plasma fluorescence spectrum is formed and is collected and detected by the spectrum collection module; the object carrying module and the focusing module are provided with an auxiliary gas module therebetween, so that a gas atmosphere is arranged at the contact position of the plasma grating and a sample to be detected, and the gas is argon or/and neon.
6. The femtosecond plasma grating induced breakdown spectroscopy device according to claim 5, wherein: the laser emission module is a pulse laser emission module, and the width of light pulse is femtosecond magnitude; the beam splitting module is a beam splitting sheet; the focusing module is a focusing system formed by a single-chip or a plurality of focusing lenses; the spectrum collection module consists of a fluorescence collection system and a spectrometer, and the fluorescence collection system is a single focusing lens or a 4f system; the spectrometer is a high resolution spectrometer.
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| CN113960015A (en) * | 2021-09-30 | 2022-01-21 | 华东师范大学重庆研究院 | Multi-pulse induced spectroscopy method and device based on femtosecond plasma grating |
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| CN105181679A (en) * | 2015-09-08 | 2015-12-23 | 天津科技大学 | Device for detecting the content of heavy metal Cr element in soil by laser-induced breakdown spectroscopy |
| CN105784680A (en) * | 2016-03-10 | 2016-07-20 | 北京理工大学 | Method for enhancing plasma spectrum of fused silica induced by femtosecond laser double pulses |
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| CN105181679A (en) * | 2015-09-08 | 2015-12-23 | 天津科技大学 | Device for detecting the content of heavy metal Cr element in soil by laser-induced breakdown spectroscopy |
| CN105784680A (en) * | 2016-03-10 | 2016-07-20 | 北京理工大学 | Method for enhancing plasma spectrum of fused silica induced by femtosecond laser double pulses |
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