CN218847971U - Filter paper enrichment and high-voltage discharge combined laser-induced breakdown spectroscopy analysis system - Google Patents
Filter paper enrichment and high-voltage discharge combined laser-induced breakdown spectroscopy analysis system Download PDFInfo
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- CN218847971U CN218847971U CN202222594357.XU CN202222594357U CN218847971U CN 218847971 U CN218847971 U CN 218847971U CN 202222594357 U CN202222594357 U CN 202222594357U CN 218847971 U CN218847971 U CN 218847971U
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Abstract
The utility model relates to a filter paper enrichment and high-voltage discharge laser induced breakdown spectroscopy analysis system; the problems that plasma is easy to have quenching phenomenon and the spectrum intensity is low due to the fact that a direct measurement method is adopted for LIBS detection of a liquid sample in the prior art are solved; and the method of converting liquid into solid is adopted, so that the problem of coffee ring effect is easily caused; the system comprises a laser ablation module, a spectrum acquisition module, a discharge module and a data analyzer; the laser ablation module comprises a laser, a reflecting mirror, a dichroic mirror and a first converging lens, wherein the reflecting mirror, the dichroic mirror and the first converging lens are sequentially arranged along a light path; the spectrum acquisition module comprises a second converging lens, an optical fiber detector and a spectrum analyzer, wherein the second converging lens and the optical fiber detector are sequentially arranged on a reflection light path of an emergent surface of the dichroic mirror, and the spectrum analyzer is connected with the optical fiber detector; the discharging module comprises a direct current power supply, a charging circuit and a discharging circuit, the discharging circuit is arranged above the filter paper, the charging circuit is connected with the direct current power supply, and the discharging circuit is connected with the charging circuit; the data analyzer is connected with the spectrum analyzer.
Description
Technical Field
The utility model relates to a spectral analysis system, concretely relates to filter paper enrichment combines high-voltage discharge laser induction to puncture spectral analysis system.
Background
The Laser-Induced Breakdown Spectroscopy (LIBS) is a novel element analysis technology based on atomic emission Spectroscopy, and has the advantages of rapidness, in-situ, multi-element real-time online detection, no need of complex pretreatment on a sample and the like, so that the Laser-Induced Breakdown Spectroscopy (LIBS) has important application value in the aspects of qualitative identification and quantitative detection.
The LIBS can realize the all-round detection of gas, liquid and solid, and is widely applied to the fields of geological exploration, cultural relic identification, archaeology, deep-space and deep-sea exploration, environment detection and the like at present. However, for qualitative and quantitative analysis of trace elements in a liquid sample, compared with other detection technologies, the LIBS technology has the defects of low spectral intensity, large signal fluctuation, poor detection sensitivity and high detection limit, which become bottlenecks that restrict the development of LIBS technology, and thus is highly valued by vast LIBS researchers.
At present, aiming at the detection of a liquid sample, the LIBS technology usually has two ideas:
1) Direct measurement of liquid samples: directly generating plasma inside the liquid sample by using single or multiple pulses, and realizing qualitative and quantitative analysis by collecting spectral information of the plasma;
2) Conversion of the liquid to a solid: after a liquid sample is converted into a solid sample by methods of electrochemical deposition, graphene sheet adsorption, freezing and the like, high-energy laser is used for exciting plasma, and detection and analysis of elements in the liquid are realized.
Although the two methods realize the LIBS detection of the liquid sample to a certain extent, certain problems still exist:
in the first scheme, when a liquid sample is directly measured, quenching phenomenon easily occurs to plasma, and the spectral intensity is low, so that the analysis capability of the LIBS technology is limited; meanwhile, the laser irradiates the liquid to generate liquid level sputtering, so that the optical system is easily polluted;
in the second scheme, a long-time sample pretreatment process is often needed, a coffee ring effect is easily generated, the precision and the sensitivity of quantitative analysis of the LIBS technology are influenced, and the first scheme is against the first purpose of the LIBS, namely rapidness, real-time performance and high efficiency.
SUMMERY OF THE UTILITY MODEL
The utility model aims to solve the problems that the plasma is easy to have quenching phenomenon, the spectrum intensity is low, the analysis capability of the LIBS technology is limited and the optical system is easy to be polluted because the LIBS detection of the liquid sample adopts a direct measurement method in the prior art; and the method of converting liquid into solid is adopted, so that the coffee ring effect is easy to generate, and the accuracy and the sensitivity of quantitative analysis of the LIBS technology are influenced, and the system for analyzing the breakdown spectrum by combining filter paper enrichment with high-voltage discharge laser induction is provided.
The utility model adopts the technical proposal that:
a filter paper enrichment and high-voltage discharge laser-induced breakdown spectroscopy analysis system is characterized in that:
the device comprises a laser ablation module, a spectrum acquisition module, a discharge module and a data analyzer;
the laser ablation module comprises a laser, a reflecting mirror, a dichroic mirror and a first converging lens; the reflector is positioned on an emergent light path of the laser, the laser reflected by the reflector is incident on an incident surface of the dichroic mirror and is transmitted to the first converging lens through the dichroic mirror, and emergent light of the first converging lens is vertically incident on filter paper for enriching a liquid sample to excite and generate liquid sample plasma; a spectral signal generated by the liquid sample plasma is reflected by the dichroic mirror after passing through the first converging lens;
the spectrum acquisition module comprises a second convergent lens, an optical fiber detector and a spectrum analyzer connected with the optical fiber detector, wherein the second convergent lens and the optical fiber detector are sequentially arranged on a dichroic mirror reflection light path; the spectral signals reflected by the dichroic mirror are converged by a second converging lens and then enter an optical fiber detector, and the optical fiber detector transmits the optical signals to a spectrum analyzer through optical signals;
the discharging module comprises a direct-current power supply, a charging circuit and a discharging circuit, the discharging circuit is arranged above the filter paper, the charging circuit is connected with the direct-current power supply and used for realizing charging, and the discharging circuit is connected with the charging circuit and used for discharging;
the data analyzer is connected with the spectrum analyzer and used for receiving the spectrum signals collected by the spectrum analyzer and generating a plasma spectrogram.
Further, the charging circuit comprises an inductor, a diode and a capacitor;
one end of the inductor is connected with the grounding end of the direct current power supply, the other end of the inductor is connected with the cathode of the diode, the anode of the diode is connected with the cathode of the capacitor, and the anode of the capacitor is connected with the anode of the direct current power supply;
the discharge circuit is connected with two ends of the capacitor.
Further, the discharge circuit includes a discharge cathode and a discharge anode;
the discharge cathode is connected with the negative electrode of the capacitor, and the discharge anode is connected with the positive electrode of the capacitor;
the discharge cathode and the discharge anode are oppositely arranged in parallel to the filter paper; the distance between the discharge cathode and the discharge anode is 3-6mm, and the vertical distance between the discharge cathode and the discharge anode and the surface of the filter paper is 2-3mm.
Further, in order to reduce the measurement error, a three-dimensional translation stage is also included;
the filter paper is arranged on the three-dimensional translation table, and the discharge cathode and the discharge anode are fixed on the three-dimensional translation table.
Further, the inductance is 5-40mH, and the capacitance is 10-100nF;
the output voltage of the direct current power supply is 1000-5000V.
Furthermore, the energy of the laser is 10-100mJ, and the focal point of the laser is arranged 2-6mm below the filter paper vertically.
The utility model has the advantages that:
1. the utility model discloses in, adopt the module of discharging through the setting, can realize the excitation of discharging to the secondary of plasma, can strengthen the spectral signal intensity of plasma greatly.
2. The utility model discloses in, utilize the method of filter paper enrichment sample, need not to carry out complicated preliminary treatment to the sample, can reduce the influence of the base member effect of liquid to plasma spectral signal, improve the quantitative analysis accuracy.
3. The utility model discloses in, the experimental apparatus total cost is low, and the light path is simple, need not complicated light path calibration.
4. The utility model discloses in, through adopting charging circuit to carry out the advantage of charging in advance to lie in: direct contact between a direct current power supply and a discharge loop can be avoided; and the capacitor stores electric energy, which is more beneficial to stabilizing secondary excitation plasma.
5. The utility model discloses in, set up three-dimensional translation platform, can avoid laser to cause serious ablation to the same position on sample layer to can make laser ablation get the average value to the emission spectrum of the different regions on sample layer on the different positions on sample layer through the operation of three-dimensional translation platform of control, can reduce measuring error.
6. The utility model discloses in, the energy of laser is 10-100mJ, and the advantage that laser focus set up 2-6mm department in the perpendicular below of filter paper lies in: the laser ablation efficiency is improved, and the interference of gas above a breakdown sample to plasma is avoided.
7. The utility model discloses in, the distance between the negative pole that discharges and the positive pole that discharges is 3-6mm, and the perpendicular distance that discharges negative pole and discharge positive pole and filter paper surface is 2-3 mm's advantage lies in: the coupling efficiency of the discharge energy and the plasma is improved, and secondary excitation of the plasma is facilitated, so that a plasma spectrum with higher intensity is obtained.
Drawings
Fig. 1 is a system schematic of an embodiment of the present invention;
fig. 2 is a schematic diagram of a discharge module according to an embodiment of the present invention (including filter paper, a three-dimensional translation stage, and a first converging lens);
fig. 3 is a spectrogram of a filter paper enrichment combined with a high-voltage discharge assisted LIBS technology, a spectrogram of a filter paper enrichment combined with a traditional LIBS technology, and a spectrogram of a silica-based method combined with a traditional LIBS technology, in an embodiment of the present invention.
In the figure, 1, a laser; 2. a spectrum analyzer; 3. an optical fiber detector; 5. a data analyzer; 6. a data line; 7. a first beam of laser light; 8. a mirror; 9. a dichroic mirror; 10. a first condenser lens; 11. converging the excitation laser; 12. a three-dimensional translation stage; 13. a second condenser lens; 14. collecting and collecting light; 15. a discharge cathode; 16. a discharge anode; 17. a direct current power supply; 18. an inductance; 19. a diode; 20. a capacitor; 21. an electric wire; 22. and (5) filter paper.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings and specific embodiments.
The utility model provides a filter paper enrichment and high-voltage discharge laser-induced breakdown spectroscopy analysis system, as shown in figures 1 and 2, comprising a laser ablation module, a spectrum acquisition module, a discharge module and a data analyzer 5;
the filter paper 22 enriched with the liquid sample is arranged on the laser emergent light path of the laser ablation module;
the function of each module is as follows:
the laser ablation module is used for ablating the liquid sample on the filter paper 22; the discharge module is used for enhancing the spectrum of the liquid sample through discharge, the spectrum acquisition module is used for acquiring the spectrum information of the liquid sample and sending the spectrum information to the data analyzer 5 for analysis, and the data analyzer 5 generates a spectrogram from the received spectrum information;
the arrangement mode of each module is as follows:
as shown in fig. 1, the laser ablation module includes a laser 1, a reflecting mirror 8, a dichroic mirror 9, and a first condensing lens 10; the reflecting mirror 8, the dichroic mirror 9, the first converging lens 10 and the filter paper 22 are sequentially arranged along the emergent path of the laser 1, the reflecting mirror 8 and the dichroic mirror 9 are parallel to each other, the incident surface of the dichroic mirror 9 is positioned on the emergent light path of the reflecting mirror 8, the emergent surface of the dichroic mirror 9 is positioned on the incident light path of the first converging lens 10, and the filter paper 22 is used for enriching a liquid sample;
laser emitted by the laser 1 is reflected by the reflecting mirror 8, then enters the incident surface of the dichroic mirror 9, and is transmitted to the first converging lens 10 through the dichroic mirror 9, and emergent light of the first converging lens 10 vertically enters the filter paper 22 for enriching the liquid sample, so that liquid sample plasma is excited and generated; the spectral signal generated by the liquid sample plasma is reflected by the dichroic mirror 9 after passing through the first converging lens 10.
The spectrum acquisition module comprises a second convergent lens 13, an optical fiber detector 3 and a spectrum analyzer 2 connected with the optical fiber detector 3; the second converging lens 13 and the optical fiber detector 3 are sequentially arranged along a reflection path of the emergent surface of the dichroic mirror 9, the spectral signal reflected by the dichroic mirror 9 enters the optical fiber detector 3 after being converged by the second converging lens 13, and the optical fiber detector 3 transmits the optical signal to the spectrum analyzer 2 through an optical fiber.
As shown in fig. 2, the discharging module includes a dc power supply 17, a charging circuit including an inductor 18, a diode 19, and a capacitor 20; one end of the inductor 18 is connected with the grounding end of the direct current power supply 17, the other end of the inductor is connected with the cathode of the diode 19, the anode of the diode 19 is connected with the cathode of the capacitor 20, and the anode of the capacitor 20 is connected with the anode of the direct current power supply 17; the discharge circuit includes a discharge cathode 15 and a discharge anode 16; the positive electrode of the direct current power supply 17 is connected with the positive electrode of the capacitor 20, the discharge cathode 15 is connected with the negative electrode of the capacitor 20 through the wire 21, the discharge anode 16 is connected with the positive electrode of the capacitor 20 through the wire 21, and the output voltage of the direct current power supply 17 is 1000-5000V;
the spectrum analyzers 2 are connected with the data analyzer 5 through data lines 6, and are used for sending the spectrum data analyzed by the spectrum analyzers 2 to the data analyzer 5 for spectrum analysis.
In this embodiment, the liquid sample is enriched by using the medium-speed filter paper 22, the microliter liquid sample is dropped into the dry filter paper 22, and after the liquid is absorbed and enriched by the filter paper 22, a sample layer is formed on the surface of the filter paper 22.
To avoid severe ablation of the same portion of the sample layer by the laser and to reduce measurement errors, the filter paper 22 is mounted on the three-dimensional translation stage 12.
The inductance 18 is 5-40mH and the capacitance 20 is 10-100nF.
The energy of the laser is 10-100mJ, and the laser focus is arranged 2-6mm below the filter paper 22.
The laser 1 adopts Nd-YAG solid laser.
The electrode material should have good conductivity and simple element types.
The utility model discloses before the test, need combine the supplementary laser induction of high-pressure discharge to filter paper enrichment method to puncture spectral analysis system and assemble, during the equipment, will discharge negative pole 15 and discharge anode 16 and install on three-dimensional translation platform 12, and be located filter paper 22 top, realize discharging negative pole 15 and discharge anode 16's control through adjusting three-dimensional translation platform 12, and discharge negative pole 15 and discharge between the anode 16 interval 3-6mm, discharge negative pole 15 and discharge anode 16 are parallel with filter paper 22, and perpendicular with the incident laser of filter paper 22, discharge negative pole 15 and discharge anode 16 and treat that the vertical distance between the filter paper 22 surface is 2-3mm.
The utility model discloses a theory of operation as follows:
the direct current power supply 17 is connected with an alternating current power supply with the voltage of 220V and the frequency of 50Hz to charge the capacitor 20;
laser passes through the reflector 8 and the dichroic mirror 9, and is focused on the surface of the filter paper 22 through the first converging lens 10 to excite and generate liquid sample plasma, the liquid sample plasma generated by laser induction contains a large number of free charges, the charges exist between the discharge cathode 15 and the discharge anode 16 as seed charges, so that the discharge cathode 15 and the discharge anode 16 are conducted, the charges stored in the capacitor 20 are injected into the liquid sample plasma to excite the liquid sample plasma again, and the spectral line intensity of the liquid sample plasma is enhanced.
The characteristic spectrum emitted by the liquid sample plasma is collected through the optical fiber detector 3, the optical fiber detector 3 is connected with the spectrum analyzer 2, the characteristic spectrum is coupled into the spectrum analyzer 2 to complete the collection of the spectrum data, and the data analyzer 5 identifies the spectrum signal obtained by measurement to realize the qualitative and quantitative analysis of the target element.
The analysis method of the system comprises the following steps:
step 1: uniformly dripping a trace amount of liquid sample on the filter paper 22 by using a dropper to realize the enrichment of the filter paper 22 on the liquid sample, thereby forming a sample layer on the surface of the filter paper 22, and horizontally placing the filter paper 22 enriched with the liquid sample on the three-dimensional translation stage 12;
step 2: turning on the laser 1, converging laser emitted by the laser 1, and then injecting the converged laser into a sample layer to excite liquid sample plasma, and then carrying out secondary discharge excitation on a sample of the generated liquid sample plasma by utilizing high-voltage direct-current discharge;
specifically, the method comprises the following steps:
2.1, the direct current power supply 17 is externally connected with an alternating current power supply with voltage of 220V and frequency of 50Hz to charge the capacitor 20, and after the charging is finished, a large amount of charges are stored in the capacitor 20;
2.2 after passing through a reflector 8, a dichroic mirror 9 and a first converging lens 10, a first beam of laser 7 emitted by a laser 1 is focused on the surface of a filter paper 22, and a liquid sample plasma is excited, at this time, a large number of free electrons and ions in the liquid sample plasma exist between a discharge cathode 15 and a discharge anode 16 as seed charges, so that a circuit is communicated and a spark discharge process is generated, a large number of charges are injected into the liquid sample plasma from a capacitor 20, reheating and excitation of the liquid sample plasma are realized, and thus the spectrum of the liquid sample plasma is greatly enhanced, as shown in fig. 3, during an experiment, in order to avoid serious ablation of the same part on the surface of the sample caused by a laser beam, a three-dimensional translation stage 12 is controlled to ablate the laser on different positions on the surface of the filter paper 22, the emission spectra of different areas on the surface of the filter paper 22 are averaged, and the measurement error of the filter paper can be reduced to a certain extent;
and step 3: as shown in fig. 1, a spectral signal generated by a liquid sample plasma returns along a primary path of a convergent excitation laser 11, is reflected by a dichroic mirror 9 after passing through a first convergent lens 10, and then passes through a second convergent lens 13 to form a convergent collected light 14, and enters an optical fiber detector 3, and the optical fiber detector 3 sends the optical signal to a spectrum analyzer 2;
the data analyzer 5 receives the spectrum signal collected by the spectrum analyzer 2, performs spectrum analysis, that is, converts the measured spectrum signal into a spectrum graph, the abscissa is the light wavelength, and the ordinate is the graph of the intensity value, and compares the wavelength and the relative intensity of each spectrum peak in the obtained spectrum graph with the wavelength and the relative intensity of each element in the standard database to obtain the element composition and the relative content of each element in the measured sample.
As shown in fig. 3, the drawings are a lubricating oil plasma spectrogram obtained by adopting filter paper enrichment and combining with a high-voltage discharge assisted LIBS technology, a lubricating oil plasma spectrogram obtained by adopting filter paper enrichment and combining with a traditional LIBS technology, and a lubricating oil plasma spectrogram obtained by adopting a silicon-based method and combining with a traditional LIBS technology, wherein an abscissa wavelegnth represents a spectral line wavelength, a unit of nm (nanometer), an ordinate intensity represents a measured spectral intensity, and a unit of a.u. (arbitrary unit) represents a relative value unit measured by an instrument. The Filter paper & D-LIBS represents that the Filter paper enrichment combines with the discharge-assisted laser-induced breakdown spectroscopy technology, the Filter paper & C-LIBS represents that the Filter paper enrichment combines with the traditional laser-induced breakdown spectroscopy technology, and the silicon substrate & C-LIBS represents that the silicon-based method combines with the traditional laser-induced breakdown spectroscopy technology; ca. W and CN respectively represent calcium element, tungsten element and carbon-nitrogen molecules.
As can be seen from fig. 3, in the conventional LIBS, compared with the silicon-based method, the filter paper enrichment can improve the spectral intensity of the plasma, and on the basis of the filter paper enrichment, the high-voltage discharge assisted LIBS can further improve the spectral intensity of the sample plasma by a large margin, and can measure more spectral lines with high ionization energy and difficult detection by the conventional LIBS technology.
Claims (6)
1. The utility model provides a filter paper enrichment combines high-voltage discharge laser-induced breakdown spectroscopy analysis system which characterized in that:
the device comprises a laser ablation module, a spectrum acquisition module, a discharge module and a data analyzer (5);
the laser ablation module comprises a laser (1), a reflecting mirror (8), a dichroic mirror (9) and a first converging lens (10); the reflector (8) is positioned on an emergent light path of the laser (1), laser reflected by the reflector (8) is incident on an incident surface of the dichroic mirror (9) and is transmitted to the first converging lens (10) through the dichroic mirror (9), emergent light of the first converging lens (10) is vertically incident on filter paper (22) for enriching a liquid sample, and the liquid sample is excited to generate plasma; a spectral signal generated by the liquid sample plasma is reflected by a dichroic mirror (9) after passing through a first converging lens (10);
the spectrum acquisition module comprises a second convergent lens (13), an optical fiber detector (3) and a spectrum analyzer (2) which is connected with the optical fiber detector (3), wherein the second convergent lens (13) and the optical fiber detector (3) are sequentially arranged on a reflection light path of the dichroic mirror (9); the spectral signals reflected by the dichroic mirror (9) are converged by a second converging lens (13) and then enter the optical fiber detector (3), and the optical fiber detector (3) transmits the optical signals to the spectrum analyzer (2) through optical fibers;
the discharging module comprises a direct current power supply (17), a charging circuit and a discharging circuit, the discharging circuit is arranged above the filter paper (22), the charging circuit is connected with the direct current power supply (17) and used for realizing charging, and the discharging circuit is connected with the charging circuit and used for discharging;
the data analyzer (5) is connected with the spectrum analyzer (2) and used for receiving the spectrum signals collected by the spectrum analyzer (2) and generating a plasma spectrogram.
2. The filter paper enrichment and high-voltage discharge laser-induced breakdown spectroscopy analysis system according to claim 1, wherein the filter paper enrichment and high-voltage discharge laser-induced breakdown spectroscopy analysis system comprises:
the charging circuit comprises an inductor (18), a diode (19) and a capacitor (20);
one end of the inductor (18) is connected with the grounding end of the direct current power supply (17), the other end of the inductor is connected with the cathode of the diode (19), the anode of the diode (19) is connected with the cathode of the capacitor (20), and the anode of the capacitor (20) is connected with the anode of the direct current power supply (17);
the discharge circuit is connected to both ends of a capacitor (20).
3. The filter paper enrichment-combined high voltage discharge laser-induced breakdown spectroscopy analysis system as claimed in claim 2, wherein:
the discharge circuit comprises a discharge cathode (15) and a discharge anode (16);
the discharge cathode (15) is connected with the negative electrode of the capacitor (20), and the discharge anode (16) is connected with the positive electrode of the capacitor (20);
the discharge cathode (15) and the discharge anode (16) are oppositely arranged in parallel with the filter paper (22); the distance between the discharge cathode (15) and the discharge anode (16) is 3-6mm, and the vertical distance between the discharge cathode (15) and the discharge anode (16) and the surface of the filter paper (22) is 2-3mm.
4. The filter paper enrichment and high-voltage discharge laser-induced breakdown spectroscopy analysis system according to claim 3, wherein the filter paper enrichment and high-voltage discharge laser-induced breakdown spectroscopy analysis system comprises:
further comprising a three-dimensional translation stage (12);
the filter paper (22) is arranged on the three-dimensional translation table (12), and the discharge cathode (15) and the discharge anode (16) are fixed on the three-dimensional translation table (12).
5. The filter paper enrichment-combined high voltage discharge laser-induced breakdown spectroscopy analysis system as claimed in claim 4, wherein:
the inductor (18) is 5-40mH, and the capacitor (20) is 10-100nF;
the output voltage of the direct current power supply (17) is 1000-5000V.
6. The filter paper enrichment-combined high voltage discharge laser-induced breakdown spectroscopy analysis system according to any one of claims 1 to 5, wherein:
the energy of the laser is 10-100mJ, and the laser focus is arranged at a position 2-6mm vertically below the filter paper (22).
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117445520A (en) * | 2023-12-26 | 2024-01-26 | 成都艾立本科技有限公司 | Composite nanostructure for LIBS analysis, analysis method and application |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117445520A (en) * | 2023-12-26 | 2024-01-26 | 成都艾立本科技有限公司 | Composite nanostructure for LIBS analysis, analysis method and application |
| CN117445520B (en) * | 2023-12-26 | 2024-03-19 | 成都艾立本科技有限公司 | Composite nanostructure for LIBS analysis, analysis method and application |
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