CN116223481A - Multi-element multi-spectral line spectrum enhanced laser-induced breakdown spectroscopy measurement method - Google Patents
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Abstract
The invention provides a multi-element multispectral spectrum enhanced laser-induced breakdown spectroscopy measurement method, belongs to the technical field of substance element component detection, and solves the problems in the existing LIBS technology spectrum enhancement mode; the method comprises the following steps: s1, generating a super-continuous light source by using femtosecond laser; s2, ablating a target sample by using pulse laser, and generating plasma on the surface of the target sample; s3, enabling the super-continuous light source to act on the plasma to excite particles with different energy levels of different elements in the plasma; s4, collecting and measuring the emission spectrum of the excited particles in the plasma to obtain the element composition of the target sample; the invention utilizes the characteristics of super-continuous wide spectrum and high peak power of femto-second white light to act on plasma, fully plays a role in selectively exciting different energy level population particles of different elements by different frequency components, realizes enhancement of multispectral signals, and remarkably improves the detection sensitivity of LIBS technology on the multiple elements.
Description
Technical Field
The invention belongs to the technical field of detection of material element components, and is applied to the technical process of laser-induced breakdown spectroscopy, in particular to a multi-element multispectral spectrum enhanced laser-induced breakdown spectroscopy measurement method.
Background
The Laser Induced Breakdown Spectroscopy (LIBS) technology is a method for detecting elemental components of a substance based on laser spectroscopy, which focuses high-energy laser on the surface of a sample to induce plasma, and then collects and analyzes atomic, ionic and molecular spectra radiated in the plasma cooling process to determine the elemental components of the substance. LIBS technology has the advantages of no need of sample preparation, real-time online, micro-damage, multi-element analysis, remote non-contact analysis and the like, and is widely applied to the fields of environmental monitoring, food safety, address exploration, energy, construction, metallurgy and the like.
When the LIBS technology is applied to the analysis of substance components, the LIBS technology still faces the problems of weak spectral line intensity, matrix effect, poor repeatability caused by unstable plasmas and the like due to element content intersection; the detection limit of LIBS technology is usually mg/kg (ppm) which is far higher than the detection limit ug/kg (ppb) of inductively coupled plasma emission spectrometry (ICP-OES) and the detection limit ng/kg (ppt) of inductively coupled plasma mass spectrometry (ICP-MS); in addition, the LIBS technique also has a larger error during the measurement than the other two techniques due to the matrix effect and the self-absorption effect. However, the ICP-OES technology and ICP-MS technology require complex sample preparation and cumbersome analytical procedures, and do not have the capability of in-situ analysis; the LIBS technology has the advantages of no need of sample preparation, high spectrum acquisition speed and the like, and plays an important role in on-site substance element detection. For example, in the on-site detection of heavy metal elements in a water body, the requirement on the detection limit of the elements is in ppm level, so that the LIBS technology can meet the on-site detection requirement of Fe, cu, cr, pb and other elements; however, the detection limit requires elements such as Cd and Hg in the ppb level, and thus higher detection sensitivity is required. Therefore, in order to further improve the analysis capability of the LIBS technology and expand the application field of the LIBS technology, it is necessary to improve the signal strength of the LIBS technology on the premise of exerting the advantages of rapid and real-time analysis of the LIBS technology, thereby enhancing the sensitivity of the LIBS technology in element detection. As for the method for enhancing the LIBS sensitivity, there are two methods in the prior art:
the double-pulse LIBS technique is the most commonly used LIBS sensitivity enhancement. In conventional double pulse LIBS measurements, a second laser beam is typically used to preheat the plasma to ablate the region or reheat the plasma plume, the plasma absorbing the laser energy primarily in the form of reverse bremsstrahlung; thus, this technique is less efficient for characteristic emission spectrum signal enhancement while being prone to strong continuous background noise.
Laser-induced fluorescence assisted enhanced laser induced breakdown spectroscopy (LIBS-LIF) technology, which is a more sensitive rapid element measurement method. Unlike the double pulse LIBS technique, the LIBS-LIF technique uses a wavelength tunable laser to output a beam of wavelength tunable laser to irradiate a plasma, and when the energy of a laser photon is equal to the difference between the upper and lower energy levels of particles in the plasma, the particles at the lower energy level resonantly absorb the laser photon, transition to the upper energy level, and the particles at the upper energy level transition downward again to emit a characteristic fluorescent signal. The LIBS-LIF technology has the characteristics of high selectivity and high excitation efficiency, and can realize the great enhancement of specific spectral lines of specific elements, but the technology only enhances one element in one measurement and can excite particles with specific energy levels for the same element, so that the LIBS technology is greatly limited in high-sensitivity detection capability for multiple elements.
In view of the above problems, how to implement a LIBS measurement method with simultaneous enhancement of multi-element multispectral spectrum becomes an important problem to be solved by those skilled in the art.
Disclosure of Invention
The invention aims to overcome various problems in a spectrum enhancement mode of LIBS technology in the prior art, and therefore provides a multi-element multispectral spectrum enhanced laser-induced breakdown spectrum measurement method; according to the method, the characteristics of super-continuous wide spectrum and high peak power of the femtosecond white light are utilized, when the femtosecond super-continuous light source acts on plasma, the selective excitation of different frequency components of the super-continuous light source to the population particles with different elements and different energy levels can be fully exerted, so that the enhancement of multispectral signals is realized, and the detection sensitivity of the LIBS technology to the multiple elements is remarkably improved.
The invention adopts the following technical scheme to achieve the purpose:
a multi-element multispectral spectrum enhanced laser-induced breakdown spectroscopy measurement method comprises the following steps:
s1, generating a super-continuous light source by using femtosecond laser;
s2, ablating a target sample by using pulse laser, and generating plasma on the surface of the target sample;
s3, enabling the super-continuous light source to act on the plasma to excite particles with different energy levels of different elements in the plasma;
s4, collecting and measuring laser-induced breakdown spectra of the excited particles in the plasma to obtain element components of the target sample.
Wherein, the wavelength of a typical super-continuous light source can cover blue-violet light to near-infrared wave bands, and the generation device of the super-continuous light source comprises a femtosecond laser, a nonlinear medium and a lens.
Further, in step S1, the femtosecond laser is output by the femtosecond laser, the femtosecond laser is formed into a filament area in the nonlinear medium, and the spectrum of the femtosecond laser is broadened by the nonlinear effect, so that the supercontinuum light source is generated.
Preferably, the femtosecond laser outputs a femtosecond pulse laser beam with high peak power, and typical single pulse energy level ranges of the femtosecond pulse laser beam are: micro-focal to millifocal orders of magnitude.
Specifically, the nonlinear medium comprises a liquid, a gas, a crystal or a sheet group, wherein typical mediums comprise fused quartz crystals, sapphire, fused quartz sheet groups, water, hollow optical fibers filled with air or inert gas, and the like; nonlinear effects of nonlinear medium, including self-phase modulation, cross-phase modulation, four-wave mixing, stimulated Raman scattering, stimulated Brillouin scattering, etc., are utilized to broaden the femtosecond laser spectrum and generate a supercontinuum light source.
Specifically, the femtosecond laser is focused through a lens, and after a filament forming area is formed in a nonlinear medium, the filament forming area is collimated through the lens, so that a super-continuous light source is generated; the lens provides extremely high peak power densities for the formation of femto-second filamentization and supercontinuum light sources.
Further, in step S2, a pulse laser with high peak power is output by using a pulse laser, and the pulse width of the pulse laser is nanosecond; the pulse laser is focused and collimated by a lens in a way of high reflection mirror, and finally acts on the surface of a target sample to ablate the target sample, so that plasma plumes are generated.
The plasma generated by the high peak power pulsed laser has a particle distribution, a temporal-spatial non-uniformity of electron temperature density, and causes different elements in the plasma to be localized at a large number of different energy levels.
Preferably, the movement of the target is controlled by a stepper motor so that the pulsed laser acts at different locations on the surface of the target.
Furthermore, the output delay time of the femtosecond laser and the pulse laser is controlled by utilizing the digital signal delay generator, so that the supercontinuum light source delays to act on plasmas generated by the pulse laser, and the supercontinuum light source excites particles with different energy levels in the plasmas in different plasma states.
Specifically, in step S4, the excited and enhanced plasma emission spectrum is collected by the spectrum collecting lens group, then coupled into the optical fiber probe, transmitted to the spectrometer through the optical fiber, and the spectrometer performs the spectroscopic processing on the collected spectrum, and stores the spectrum data into the computer.
Preferably, the spectrometer acquisition time and the delay time between the femtosecond laser and the pulsed laser are controlled by a digital signal delay generator.
In summary, by adopting the technical scheme, the invention has the following beneficial effects:
the method has the characteristic of multi-element multi-spectral line enhancement, and is very important for real-time and high-sensitivity detection of the LIBS technology in the fields of sewage heavy metal detection, nuclear material evidence collection, atmospheric aerosol component monitoring, food and drug safety and the like; through different frequency components of the super-continuous light source in a wide spectrum range, resonance excitation is carried out on various elements, atoms, ions and molecules with different energy levels in the laser plasma, the intensity of various particle emission lines is enhanced, and further the spectrum detection sensitivity is improved.
The invention uses the digital signal delay generator to make the super-continuous light source interact with particles in different evolution periods of the plasma by controlling the action time, so as to excite the particles such as atoms, ions, molecules and the like which are populated on different energy levels in the plasma plume, thereby improving the efficiency of the super-continuous light source to enhance the emission spectrum.
In the traditional double-pulse laser-induced breakdown spectroscopy measurement, the mode of absorbing laser energy by plasma is mainly reverse bremsstrahlung radiation absorption, and atoms, ions and molecules moving at high speed in the plasma collide with each other under the action of a laser light field to obtain energy; in the measurement of the super-continuous enhanced laser-induced breakdown spectroscopy, when photon energy of different frequencies contained in the super-continuous light source is equal to the difference between upper and lower energy levels of atoms, ions, molecules and the like in the plasma, particles of the plasma selectively absorb different frequency components of the super-continuous light source, and the selective absorption belongs to resonance absorption, and the efficiency is far higher than that of reverse bremsstrahlung radiation absorption.
The method is also characterized by being different from a resonance-enhanced laser-induced fluorescence-assisted laser-induced breakdown spectroscopy method; the femtosecond super-continuous light source with wide spectrum and high peak power covers a plurality of resonance excitation lines of multiple elements, and when the light source interacts with plasma, particles which are distributed in different energy levels in the plasma are excited simultaneously, so that the light source has the characteristic of multi-element multi-spectral line spectrum enhancement.
Drawings
FIG. 1 is a schematic diagram of the structural principle of the present invention;
FIG. 2 is a data diagram of a super-continuum light source produced by the method of the present invention;
FIG. 3 is a graph of a supercontinuum enhanced differential spectrum of a gypsum sample obtained by the method of the present invention;
FIG. 4 is a graph of Al element quantitative analysis of an alloy steel standard sample obtained by the method of the invention;
FIG. 5 is a graph of Nb element quantitative analysis of an alloy steel standard sample obtained by the method of the invention.
The meaning of the symbols in the drawings is specifically as follows:
1-pulse laser, 2-pulse laser beam, 3-high reflection mirror, 4-lens, 5-target sample, 6-plasma, 7-femtosecond laser, 8-femtosecond laser beam, 9-nonlinear medium, 10-super continuous light source, 11-spectrum collection lens group, 12-fiber probe, 13-fiber, 14-spectrometer, 15-digital signal delay generator and 16-computer.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments of the present invention. The components of the embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the invention, as presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The detailed steps of the method of the present invention are described by the hardware structure shown in fig. 1, please refer to the structure in fig. 1 at the same time, and the method for measuring the multi-element multi-spectral line spectrum enhanced laser-induced breakdown spectrum disclosed by the present invention comprises the following steps:
s1, generating a super-continuous light source by using femtosecond laser.
The femtosecond laser is utilized to output the femtosecond laser, the femtosecond laser is formed into a filament area in a nonlinear medium, and the spectrum of the femtosecond laser is widened through nonlinear effect, so that a super-continuous light source is generated.
The femtosecond laser outputs a femtosecond pulse laser beam with high peak power, and typical single pulse energy level range of the femtosecond pulse laser beam is: micro-focal to millifocal orders of magnitude.
Nonlinear media include liquids, gases, crystals or flakes, with typical media including fused silica crystals, sapphire, fused silica flakes, water, air or inert gas filled hollow fiber, and the like; nonlinear effects of nonlinear medium, including self-phase modulation, cross-phase modulation, four-wave mixing, stimulated Raman scattering, stimulated Brillouin scattering, etc., are utilized to broaden the femtosecond laser spectrum and generate a supercontinuum light source.
Focusing the femtosecond laser through a lens, forming a filament forming area in a nonlinear medium, and then collimating through the lens to generate a super-continuous light source; the lens provides extremely high peak power densities for the formation of femto-second filamentization and supercontinuum light sources.
In this embodiment, as shown in fig. 1, a femtosecond laser 7 outputs a femtosecond laser beam 8, a filament forming region is formed in a nonlinear medium 9 through a lens 4, and a spectrum is broadened by using the nonlinear effect of the nonlinear medium to generate a supercontinuum light source 10; the supercontinuum light source 10 is collimated by the lens 4.
S2, ablating the target sample by using pulse laser, and generating plasma on the surface of the target sample.
Outputting pulse laser with high peak power by using a pulse laser, wherein the pulse width of the pulse laser is nanosecond; the pulse laser is focused and collimated by a lens in a way of high reflection mirror, and finally acts on the surface of a target sample to ablate the target sample, so that plasma plumes are generated.
The plasma generated by the high peak power pulsed laser has a particle distribution, a temporal-spatial non-uniformity of electron temperature density, and causes different elements in the plasma to be localized at a large number of different energy levels.
And controlling the movement of the target sample by using a stepping motor, so that the pulse laser acts on different positions of the surface of the target sample.
In this embodiment, as shown in fig. 1, a high peak power pulse laser beam 2 output from a pulse laser 1 is reflected by a high reflection mirror 3, focused by a lens 4 onto the surface of a target 5, and ablates the surface of the target 5 to generate plasma 6.
In this embodiment, the pulse laser 1 employs Q-switched Nd: YAG nanosecond pulse laser, the wavelength of the output pulse laser beam 2 is 1064nm, the pulse width is 7ns, and the repetition rate is 10Hz.
The movement of the target 5 is controlled by the stepping motor, so that the pulse laser beam 2 can be prevented from repeatedly ablating the same position of the target 5, thereby avoiding damaging the target 5 and improving the repeatability of the emission signal of the plasma 6.
S3, enabling the super-continuous light source to act on the plasma to excite particles with different energy levels of different elements in the plasma.
As shown in fig. 1, the output delay time of the femtosecond laser and the pulse laser is controlled by a digital signal delay generator 15, so that the supercontinuum light source 10 delays acting on the plasma 6 generated by the pulse laser, and the supercontinuum light source 10 excites particles with different energy levels in the plasma 6 in different plasma states; in this embodiment, when the supercontinuum light source 10 is collimated by the lens 4, it acts on the region of the plasma 6 with a small spot size, delayed by a certain time with respect to the pulsed laser beam 2.
S4, collecting and measuring laser-induced breakdown spectra of the excited particles in the plasma to obtain element components of the target sample.
In this embodiment, as shown in fig. 1, the excited and enhanced plasma emission spectrum is collected by the spectrum collecting lens group 11, then coupled into the optical fiber probe 12, transmitted to the spectrometer 14 through the optical fiber 13, and the spectrometer 14 performs the spectroscopic processing on the collected spectrum, and stores the spectrum data in the computer 16.
The pulse laser 1, the femtosecond laser 7 and the spectrometer 14 are all connected with a digital signal delay generator 15; the digital signal delay generator 15 is used for controlling the acquisition time of the spectrometer 14 and the delay time between the femtosecond laser and the pulse laser, so that the interference degree of background radiation to the light measurement caused by the influence of the femtosecond laser and the pulse laser is reduced.
In this embodiment, more specifically, it is: the femtosecond laser 7 adopts a titanium gemstone femtosecond laser, the central wavelength of the output femtosecond laser beam 8 is 800nm, the repetition frequency is 10Hz, the pulse width is less than 100fs, and the single pulse energy is about 1mJ; the nonlinear medium 9 is a fused quartz crystal.
Example 2
Based on the embodiment 1, the method of the embodiment 1 is adopted in the embodiment, and the effect brought by enhancing the multi-spectral line intensities of Ca, na and other elements in the gypsum spectrum by utilizing a supercontinuum enhancement mode is introduced.
In the embodiment, a 1064nm nanosecond laser generated by a pulse laser is utilized to ablate plasma on the surface of gypsum, then a titanium gemstone femtosecond laser and a fused quartz crystal serving as a nonlinear medium are utilized to generate a super-continuous light source, and after beam splitting by a beam splitter, the visible light component in the super-continuous light source is reserved.
Fig. 2 shows the spectrum of the supercontinuum light source obtained by the method of this embodiment, the spectrum range is 380-680 nm, wherein the long-wave spectrum is limited by the bandwidth of the beam splitter, and the actual output wavelength can reach the infrared band. The super-continuous light source covers a plurality of excitation lines of Ca, na and other elements. The femtosecond super-continuous light source is controlled to act on the plasma by a digital signal delay generator (specifically DG 645) under the delay of 0.5-5 us, particles with different energy levels of Ca and Na elements in the plasma are re-excited, and the spectrum of the gypsum sample under the enhancement of the super-continuous light source is differentiated to obtain a differential spectrum of the gypsum sample shown in figure 3.
As can be seen from FIG. 3, the molecular spectrum intensities of Ca II 396.7nm, ca I422.7 nm, na I588.9 nm, na I589.6 nm and the like are improved under different delays. The result shows that the method in the embodiment 1 of the invention used in the embodiment can not only improve the intensity of spectral lines of different elements, but also enhance a plurality of emission spectral lines of the same element.
Example 3
Based on the embodiment 1, the method of the embodiment 1 is adopted in the embodiment, and the effect of improving the sensitivity of the LIBS quantitative analysis of the alloy steel standard sample by using the super-continuous light source is introduced.
The method process of the invention is adopted in the embodiment to quantitatively analyze the trace elements in the 5 groups of alloy steel standard samples. Also using 1064nm Nd generated by a pulsed laser: YAG nanosecond laser is used as an excitation source of plasma; the super-continuous light source formed by the femtosecond laser generated by the femtosecond laser is used as microelement atoms in alloy steel plasma to be re-excited, the pulse interval of two laser beams is optimized to be 1us by utilizing a digital signal delay generator, and a spectrometer delays the acquisition of a spectrum by 0.5us relative to the super-continuous light source, so that quantitative analysis is carried out on the acquired spectrum.
FIG. 4 shows the results of quantitative analysis of Al element obtained by the method of the present invention, wherein SC-LIBS represents the results of laser-induced breakdown spectroscopy measurement after super-continuous enhancement of the method; compared with the traditional LIBS technology, under the action of the super-continuous light source, the slope of the calibration curve of the Al element of the SC-LIBS is obviously improved, and the detection limit is improved from 47ppm to 34ppm.
FIG. 5 shows the result of quantitative analysis of Nb element obtained by the method of the present invention, and likewise, the detection limit of Nb element is raised from 143ppm to 90ppm under the action of a super-continuous light source.
The experimental results of the above embodiments show that the sensitivity of LIBS technology to detection of various elements can be improved by adopting the method of the invention; therefore, the method successfully improves the LIBS signal strength on the premise of exerting the advantages of the LIBS technology of rapid and real-time analysis, and does not bring about the problems and defects existing in the existing enhancement mode.
Claims (10)
1. The multi-element multi-spectral line spectrum enhanced laser-induced breakdown spectroscopy measurement method is characterized by comprising the following steps of:
s1, generating a super-continuous light source by using femtosecond laser;
s2, ablating a target sample by using pulse laser, and generating plasma on the surface of the target sample;
s3, enabling the super-continuous light source to act on the plasma to excite particles with different energy levels of different elements in the plasma;
s4, collecting and measuring the emission spectrum of the excited particles in the plasma to obtain the element composition of the target sample.
2. The multi-element multispectral spectrally enhanced laser-induced breakdown spectroscopy method of claim 1, wherein: in step S1, a femtosecond laser is output by a femtosecond laser, the femtosecond laser is formed into a filament area in a nonlinear medium, and the spectrum of the femtosecond laser is broadened by a nonlinear effect, thereby generating a supercontinuum light source.
3. The multi-element multispectral spectrally enhanced laser-induced breakdown spectroscopy method of claim 2, wherein: the femtosecond laser outputs a femtosecond pulse laser beam with high peak power, and typical single pulse energy level ranges of the femtosecond pulse laser beam are: micro-focal to millifocal orders of magnitude.
4. The multi-element multispectral spectrally enhanced laser-induced breakdown spectroscopy method of claim 2, wherein: the nonlinear medium comprises a liquid, gas, crystal, or sheet set; the nonlinear effects include self-phase modulation, cross-phase modulation, four-wave mixing, stimulated raman scattering, and stimulated brillouin scattering.
5. The multi-element multispectral spectrally enhanced laser-induced breakdown spectroscopy method of claim 2, wherein: the femtosecond laser is focused by a lens, and after a filament forming area is formed in a nonlinear medium, the filament forming area is collimated by the lens, so that a super-continuous light source is generated.
6. The multi-element multispectral spectrally enhanced laser-induced breakdown spectroscopy method of claim 1, wherein: in the step S2, a pulse laser with high peak power is output by using a pulse laser, and the pulse width of the pulse laser is nanosecond; the pulse laser is focused and collimated by a lens in a way of high reflection mirror, and finally acts on the surface of a target sample to ablate the target sample, so that plasma plumes are generated.
7. The multi-element multispectral spectrally enhanced laser-induced breakdown spectroscopy method of claim 6, wherein: and controlling the movement of the target sample by using a stepping motor, so that the pulse laser acts on different positions of the surface of the target sample.
8. The multi-element multispectral spectrally enhanced laser-induced breakdown spectroscopy method of claim 1, wherein: the output delay time of the femtosecond laser and the pulse laser is controlled by utilizing a digital signal delay generator, so that the supercontinuum light source delays to act on plasmas generated by the pulse laser, and particles with different energy levels in the plasmas are excited by the supercontinuum light source under different plasma states.
9. The multi-element multispectral spectrally enhanced laser-induced breakdown spectroscopy method of claim 8, wherein: in step S4, the excited and enhanced plasma emission spectrum is collected by the spectrum collecting lens group, then coupled into the optical fiber probe, transmitted to the spectrometer through the optical fiber, subjected to spectral processing by the spectrometer, and stored in the computer.
10. The multi-element multispectral spectrally enhanced laser-induced breakdown spectroscopy method of claim 9, wherein: and controlling the acquisition time of the spectrometer and the delay time between the femtosecond laser and the pulse laser by using a digital signal delay generator.
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| CN117269008B (en) * | 2023-09-22 | 2024-05-03 | 哈尔滨工业大学 | High-concentration soot volume fraction measuring device and method based on laser preheating |
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