CN115684329A - Multi-wavelength laser coaxial micro-area in-situ ablation sample injection system - Google Patents

Multi-wavelength laser coaxial micro-area in-situ ablation sample injection system Download PDF

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Publication number
CN115684329A
CN115684329A CN202211311017.XA CN202211311017A CN115684329A CN 115684329 A CN115684329 A CN 115684329A CN 202211311017 A CN202211311017 A CN 202211311017A CN 115684329 A CN115684329 A CN 115684329A
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laser
ablation
sample
area
situ
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CN202211311017.XA
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吕涛
尼洋
范博文
刘勇胜
陈力飞
陈海红
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China University of Geosciences
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China University of Geosciences
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Abstract

The invention discloses a multi-wavelength laser coaxial micro-area in-situ ablation sample injection system, wherein a multi-wavelength laser of the system is provided with a plurality of light outlets for outputting a plurality of paths of lasers with different wavelengths; a beam expander is arranged in front of each light outlet, and the expanded multi-path laser passes through a beam splitter or a reflector and the beam splitter and then is superposed on the same optical axis and is focused by a focusing mirror; the denudation pool is positioned on the three-dimensional moving platform and is internally provided with a sample; the three-dimensional moving platform and the camera are both connected with the machine vision control module, and the machine vision control module controls the three-dimensional moving platform to move to realize that the laser focus is arranged at the selected position on the surface of the sample so as to complete the automatic focusing of the ablation laser, the free selection and the automatic adjustment of the ablation point position; the carrier gas device is communicated with the denudation pool to realize aerosol particle transmission. The invention can make the multi-light path laser realize the output of multiple wavelengths by a single light path, and realize the automatic focusing ablation and the micro-area in-situ ablation sample injection of the sample.

Description

Multi-wavelength laser coaxial micro-area in-situ denudation sample injection system
Technical Field
The invention belongs to the field of geochemical analysis, and particularly relates to a multi-wavelength laser coaxial micro-area in-situ ablation sample injection system.
Background
The laser ablation system is an important component in the laser ablation inductively coupled plasma mass spectrometry elemental analysis technology, and can realize micro-area, in-situ and rapid elemental detection and isotope analysis by combining with the mass spectrometry technology. The laser ablation system focuses on the surface of a solid material sample through high-energy short pulse or ultrashort pulse laser, a small amount of sample is ablated, aerosol particles are formed under the condition of inert gas, and the aerosol particles are transported to an ionization device through carrier gas to finish sampling, transmission and ionization of the sample. However, some lasers can only output laser pulses with different wavelengths through a plurality of light outlets, and when lasers with different wavelengths are used, the light paths need to be adjusted frequently or a plurality of light paths need to be set up so as to meet research requirements, so that the whole laser ablation system is complicated and complex.
In the existing geochemical analysis, particularly the solid micro-area geochemical analysis technology, the combination of a laser ablation sample introduction system and a plasma mass spectrometer is relied on, and the content or the ratio of elements and isotopes of a sample can be measured. Laser wavelength in a laser ablation system is often used as an important parameter to influence the experimental result, for example, in the laser ablation inductively coupled plasma mass spectrometry elemental analysis technology, the laser wavelength influences single photon energy and the light absorption degree of a material, so that the ablation depth, the sample surface temperature, the ablation speed, aerosol composition and the like are changed, the analysis signal sensitivity during micro-area analysis is further influenced, and because the spatial positions of an ablated sample and an ablation laser light path are fixed, the operation of switching the wavelength when a multi-channel laser is used is excessively complicated, and the light path condition is easily changed to influence the test stability; denudation laser focusing needs accurate control sample height, and the micro-area analysis needs accurate location sampling point, and it is too difficult to accomplish above precision operation manually.
Disclosure of Invention
The invention aims to provide a multi-wavelength laser coaxial micro-area in-situ ablation sample injection system, which enables a multi-optical-path laser to realize single optical path output of multiple wavelengths and realizes automatic focusing ablation and micro-area in-situ ablation sample injection of a sample.
In order to realize the purpose, the technical scheme of the invention is as follows:
a multi-wavelength laser coaxial micro-area in-situ ablation sample injection system comprises a multi-wavelength laser, a beam expander, a reflector, a beam splitter, a focusing mirror, an ablation pool, a three-dimensional mobile platform, a camera, a machine vision control module and a carrier gas device;
the multi-wavelength laser is provided with a plurality of light outlets for outputting a plurality of paths of laser with different wavelengths; a beam expander is arranged in front of each light outlet, and the expanded multi-path laser is superposed on the same optical axis through two reflections of a reflector and the beam expander and is focused by a focusing mirror;
the denudation pool is positioned on the three-dimensional moving platform and is internally provided with a sample; the three-dimensional moving platform and the camera are both connected with the machine vision control module, and the machine vision control module controls the three-dimensional moving platform to move to realize that the laser focus is arranged at the selected position on the surface of the sample so as to finish the automatic focusing of the ablation laser and the in-situ ablation sampling of the micro-area;
the carrier gas device is communicated with the denudation pool to realize the micro-area in-situ denudation sample injection.
Furthermore, according to different types of solid samples corroded by users, laser pulses with different wavelengths and capable of being transmitted coaxially are selected for corrosion sampling.
Furthermore, the beam expander is a high-multiple beam expander, and the beam splitter is a high-performance long-wave transmission beam splitter, a short-wave reflection beam splitter or a short-wave transmission beam splitter and a long-wave reflection beam splitter.
Further, the machine vision control module realizes the self-focusing of the laser with different wavelengths on the surface of the sample and the automatic selection and positioning of the ablation points.
Further, the system also comprises a filter plate; the laser overlapped on the same optical axis sequentially passes through the climbing frame provided with the reflecting mirror and the focusing mirror and the glass window to be focused on the surface of the sample, and the reflected light sequentially passes through the window, the focusing mirror, the beam splitter and the filter to enter the camera.
Compared with the prior art, the invention has the following advantages and beneficial effects:
according to the invention, the combination of optical elements such as the beam expander, the beam splitter, the reflector and the like is adopted, so that lasers with different wavelengths of the laser can be coaxial, a single light path outputs multi-wavelength laser pulses, the wavelength of the ablation laser can be efficiently and conveniently switched, and the appropriate wavelength is selected according to the absorption characteristic of a material to light to improve the ablation efficiency; short pulse or ultrashort pulse laser focusing ablation, and laser self-focusing can be realized by combining a precise movable platform, a CCD camera and a machine vision control module; and the sample can be subjected to micro-area in-situ sampling and sample introduction by combining with a closed denudation pool connected with a carrier gas device, so that the chemical analysis with high resolution and high sensitivity can be realized. The system has compact structure, is fast and convenient, and is beneficial to element and isotope analysis with high resolution and high sensitivity, so that the multi-wavelength laser coaxial micro-area in-situ ablation sample injection system has important and wide application prospect in the fields of geochemistry and the like.
Drawings
FIG. 1 is a schematic structural diagram of a multi-wavelength laser coaxial micro-area in-situ ablation sample injection system of the present invention.
In the figure: 1-laser, 2-light outlet, 3-beam expander, 41-first harmonic beam splitter, 42-second harmonic beam splitter, 43-third harmonic beam splitter, 51-first reflector, 52-second reflector, 53-third reflector, 54-fourth reflector, 6-focusing mirror, 7-filter, 8-ablation pool, 9-sample, 10-three-dimensional mobile platform, 11-camera, 12-computer, 13-air inlet pipeline, 14-air outlet pipeline and 15-window.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The invention provides a set of light path coaxial output method of multi-wavelength laser and a laser micro-area in-situ ablation sample injection system, which combines multi-path output laser and can simply switch the wavelength of the ablation laser; the automatic focusing of the ablation laser and the observation and selection of the ablation position can be realized through a set of machine vision self-focusing system which comprises a movable precise platform, a CCD (charge coupled device) camera and machine vision control software on a computer; and the micro-area in-situ ablation and sample injection operation can be completed by combining a closed ablation pool connected with carrier gas. The system has compact structure, is fast and convenient, and is beneficial to element and isotope analysis with high resolution and high sensitivity.
The in-situ ablation sample injection system with the coaxial multi-wavelength laser light path can realize the coaxiality of short pulse or ultrashort pulse lasers with different multi-wavelengths according to specific conditions and requirements, and complete the in-situ sampling and sample injection of micro-areas. The invention firstly uses high-power beam expanders to expand the beams of different light outlets of the laser, then uses a reflector and a harmonic beam expander to reflect twice to enable different laser paths to be superposed, and can enable the laser pulse paths with different wavelengths to be on the same optical axis by selecting a proper beam expander and adjusting the reflecting angle; then, the laser path is climbed by a reflector, and then the laser is focused by a focusing mirror; the CCD camera is combined with machine vision control software to enable the precise three-dimensional moving platform to automatically adjust the spatial position of the sample, so that the laser focus is placed at the selected position of the upper surface of the sample to complete the in-situ ablation sampling of the micro-area; and then the aerosol generated by the denudation can be transmitted to complete the whole sample introduction process through a closed denudation pool and a carrier gas device. The laser optical path system only needs to combine standard optical elements such as a beam expander, a beam splitter, a reflector and the like, so that the multi-optical-path laser realizes single-optical-path output of various wavelengths, realizes automatic focusing denudation and micro-area in-situ denudation sample injection of a sample, is beneficial to analysis of elements and isotopes with high resolution and high sensitivity, and has the advantages of convenience in assembly and adjustment, simple structure, wide applicability and good repeatability.
The invention has important function in the fields of geochemistry analysis and the like, and can complete the micro-area in-situ denudation, sampling and sample introduction operation of the required multi-wavelength laser to the sample. On one hand, laser wavelength as an important parameter influences the sampling performance of laser ablation, including the size and distribution of particles (aerosol) of an ablation product, an ablation threshold, an ablation depth, an ablation speed and the like on the same base material, and some common short pulse or ultrashort pulse lasers respectively output lasers with different wavelengths through different frequency doubling optical paths, so that a single optical path is difficult to pass the lasers with different wavelengths, and the problem that lasers with different wavelengths cannot be coaxially output in scientific research application is complicated and difficult to switch the ablation lasers with different wavelengths; on the other hand, the ablation system based on short pulse or ultrashort pulse laser as the light source is an important component of the micro-area in-situ element analysis technology, the invention combines a whole set of system consisting of short pulse (or ultrashort pulse) laser ablation, a movable precise platform, a CCD camera, machine vision control software and a closed ablation pool connected with carrier gas, can realize laser self-focusing and automatically complete the micro-area in-situ sampling and sample introduction functions, and has important function and wide application prospect in the fields of geochemical analysis and the like.
As shown in fig. 1, the wavelengths output by the short pulse and ultrashort pulse laser 1 under different frequency doubling conditions are different from infrared, visible to ultraviolet, such as 1064nm, 1030nm, 800nm, 532nm, 515nm, 400nm, 355nm, 193nm, etc., and the present invention is applicable (only suitable elements are selected). With the common Nd: YAG nanosecond laser for example, three light outlets 2 respectively output three lasers with different wavelengths: the frequency tripled 355nm laser, the fundamental frequency 1064nm laser and the frequency doubled 532nm laser are respectively expanded by using standard high-power beam expanders 3 corresponding to the wavelengths of the lasers, and the expanded 355nm laser, 1064nm laser and 532nm laser are output. After beam expansion, 532nm laser passes through the first harmonic beam splitter 41 and the second harmonic beam splitter 42 and is continuously output to a subsequent optical path; after beam expansion, 355nm laser turns a light path through the first reflector 51, then turns the light path through the first harmonic beam splitter 41, and is coaxial with a 532nm laser light path; after beam expansion, 1064nm laser is turned through the second reflector 52, and then turned through the second harmonic beam expander 42, and is coaxial with the 532nm laser path. By controlling the working state of the laser, 355nm laser, 532nm laser or 1064nm laser can be respectively output in the same channel; then 355nm, 532nm and 1064nm laser beams are reflected by a third reflecting mirror 53 and a fourth reflecting mirror 54 to realize optical path climbing, and then are reflected by a third harmonic beam splitter 43 to vertically and downwards pass through a focusing mirror 6 to be focused on the surface of a sample 9 to complete denudation.
A sample 9 is placed in a closed cavity of an ablation pool 8 on a precise three-dimensional moving platform 10, the bottom of the ablation pool 8 is fixed with the precise three-dimensional moving platform 10, and a window 15 is arranged on the ablation pool 8 and is loaded with optical glass (such as calcium fluoride glass) so that laser can pass through the window; the reflected light upwards penetrates through the window 15 and the third harmonic beam splitter 33, and then laser is filtered out through the filtering wave plate 7, so that the CCD camera 11 can obtain a high-definition image in the denudation pool 8; the CCD camera 11 transmits the image data to the computer 12, and the machine vision software recognizes and transmits a control signal to the precise three-dimensional moving platform 10, so that the precise focusing of the laser on the surface of the sample is automatically realized. And meanwhile, the denudated position is accurately positioned, and the micro-area in-situ sampling of the sample is realized. An air inlet and an air outlet are arranged on two sides of the denudation pool and are respectively communicated with an air inlet pipeline 13 and an air outlet pipeline 14 so as to realize aerosol transmission after sampling, namely sample introduction operation.
In summary, the invention adopts the combination of the beam expander, the beam splitter, the reflector and other optical elements to coaxially align the lasers with different wavelengths, so that the single optical path outputs multi-wavelength laser pulses, the wavelength of the ablation laser can be efficiently and conveniently switched, and the appropriate wavelength is selected to improve the ablation efficiency according to the absorption characteristic of the material to the light; short pulse or ultrashort pulse laser focusing ablation, and laser self-focusing can be realized by combining a precise movable platform, a CCD camera and machine vision control software; and the sample can be subjected to micro-area in-situ sampling and sample introduction by combining with a closed denudation pool connected with carrier gas, so that the high-resolution and high-sensitivity chemical analysis can be realized. The invention can realize the functions of fast switching of laser wavelength, self-focusing of ablation laser, in-situ sampling of micro-areas and sample introduction with low cost, fast and conveniently.
It will be understood by those skilled in the art that the foregoing is only an exemplary embodiment of the present invention, and is not intended to limit the invention to the particular forms disclosed, since various modifications, substitutions and improvements within the spirit and scope of the invention are possible and within the scope of the appended claims.

Claims (5)

1. A multi-wavelength laser coaxial micro-area in-situ ablation sample injection system is characterized by comprising a multi-wavelength laser, a beam expander, a reflector, a beam splitter, a focusing mirror, an ablation pool, a three-dimensional mobile platform, a camera, a machine vision control module and a carrier gas device;
the multi-wavelength laser is provided with a plurality of light outlets for outputting a plurality of paths of laser with different wavelengths; a beam expander is arranged in front of each light outlet, and the expanded multi-path laser is superposed on the same optical axis through a beam splitter or a reflector and the beam splitter and is focused by a focusing mirror;
the denudation pool is positioned on the three-dimensional moving platform and is internally provided with a sample; the three-dimensional mobile platform and the camera are connected with the machine vision control module, the machine vision control module controls the three-dimensional mobile platform to move to realize that the laser focus is arranged at the selected position on the surface of the sample, and the ablation point is freely selected and positioned to finish the automatic focusing of the ablation laser and the in-situ ablation sampling of the micro-area;
the carrier gas device is communicated with the denudation pool to realize the in-situ denudation sample injection of the micro-area.
2. The multi-wavelength laser coaxial micro-area in-situ ablation sample injection system according to claim 1, wherein ablation sampling is performed by selecting laser pulses with different wavelengths and capable of coaxial transmission according to different types of solid samples ablated by a user.
3. The multi-wavelength laser coaxial micro-area in-situ ablation sample injection system according to claim 1, wherein the beam expander is a high-multiple beam expander, and the beam splitter is a high-performance long-wave transmission, short-wave reflection or short-wave transmission, long-wave reflection beam splitter.
4. The multi-wavelength laser coaxial micro-area in-situ ablation sample injection system according to claim 1, wherein the machine vision control module realizes self-focusing of different wavelength lasers on the surface of a sample and automatic selection and positioning of ablation points.
5. The multi-wavelength laser coaxial micro-area in-situ ablation sample injection system according to claim 1, further comprising a filter; the laser overlapped on the same optical axis sequentially passes through the climbing frame provided with the reflecting mirror and the focusing mirror and the glass window to be focused on the surface of the sample, and the reflected light sequentially passes through the window, the focusing mirror, the beam splitter and the filter to enter the camera.
CN202211311017.XA 2022-10-25 2022-10-25 Multi-wavelength laser coaxial micro-area in-situ ablation sample injection system Pending CN115684329A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117110020A (en) * 2023-10-24 2023-11-24 中国地质大学(武汉) Automatic online solution laser ablation pond

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117110020A (en) * 2023-10-24 2023-11-24 中国地质大学(武汉) Automatic online solution laser ablation pond
CN117110020B (en) * 2023-10-24 2024-02-02 中国地质大学(武汉) Automatic online solution laser ablation pond

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