CN112557375A - Inverted laser-induced breakdown spectroscopy device - Google Patents

Inverted laser-induced breakdown spectroscopy device Download PDF

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Publication number
CN112557375A
CN112557375A CN202011258079.XA CN202011258079A CN112557375A CN 112557375 A CN112557375 A CN 112557375A CN 202011258079 A CN202011258079 A CN 202011258079A CN 112557375 A CN112557375 A CN 112557375A
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China
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laser
sample
adapter plate
induced breakdown
breakdown spectroscopy
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CN202011258079.XA
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Chinese (zh)
Inventor
李嘉铭
张宁
覃禹智
张博元
许志颖
李创锴
赵楠
张庆茂
郭亮
马琼雄
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South China Normal University
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South China Normal University
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/71Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
    • G01N21/718Laser microanalysis, i.e. with formation of sample plasma
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03Cuvette constructions
    • G01N21/0303Optical path conditioning in cuvettes, e.g. windows; adapted optical elements or systems; path modifying or adjustment

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
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  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
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  • Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Optics & Photonics (AREA)
  • Plasma & Fusion (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)

Abstract

The embodiment of the invention provides an inverted laser-induced breakdown spectroscopy device, which comprises a mobile platform, vertical supporting frames and a switching plate, wherein the mobile platform is connected with the two vertical supporting frames, the two vertical supporting frames can be adjusted to a certain distance relative to the mobile platform, the switching plate is connected to the vertical supporting frames and is fixed relative to the two vertical supporting frames, and a small hole is formed in the middle of the switching plate for placing a sample on the switching plate; laser generated by a pulse laser is focused on a sample from bottom to top through a converging lens, and the side of the sample to be detected is placed downwards, so that secondary focusing is not needed no matter the thickness of the sample, the detection efficiency is greatly improved, and automatic detection can be realized; the structure is simple, various adjustments can be made according to the specific light path of the optical system, focusing is only needed once on repeated sample detection, and the efficiency of sample detection is greatly improved.

Description

Inverted laser-induced breakdown spectroscopy device
Technical Field
The embodiment of the invention relates to the technical field of laser, in particular to an inverted laser-induced breakdown spectroscopy device.
Background
In Laser Induced Breakdown Spectroscopy (LIBS) technology, Laser pulses are focused onto a sample surface by optical elements such as mirrors and focusing mirrors. The high-energy laser pulse is focused on a sample, the sample is induced to generate plasma, after the laser pulse disappears, the plasma is gradually cooled and expands to the external environment, and a spectrum for representing the component information of the sample is emitted. The emission spectrum of the plasma is collected by using a photoelectric detector and a spectrometer, and the element type and content information of the sample to be detected can be obtained by analyzing the wavelength and intensity distribution of the emission spectrum lines and combining a quantitative analysis model. The LIBS technology is used as a new atomic emission spectroscopy technology, the detection process is simple and quick, and the LIBS technology can be used for simultaneously analyzing multiple elements on line and is widely applied to the fields of environment, coal, metallurgy, biology, geology and the like.
The LIBS device system mainly comprises a laser, an optical transmission system, a signal detection system, a PC and the like. The optical transmission system mainly realizes the optimized shaping, beam expanding, focusing and the like of laser emergent beams. For an optical system needing focusing, the height difference of a detected sample inevitably causes the distance between a lens and the sample to be indefinite, and the optical lens system needs to be positioned and adjusted to enable the focus of the lens to be aligned with a target sample. The main disadvantage of such a device is that the focus needs to be adjusted once for changing one sample, and the repeatability and efficiency become low.
In the presently published patents, there are two types: the Chinese patent with the publication number of CN 103743718A discloses a laser spectrum analyzer combining confocal micro-Raman and laser-induced breakdown spectroscopy, wherein an incandescent lamp is adopted to illuminate a sample, CCD image processing is utilized to determine the focal plane from the sample to a micro objective lens, and the surface of the sample is imaged at a micrometer scale high resolution ratio, so that the aim of focusing is achieved; chinese patent publication No. CN 109884032 a discloses a laser-induced breakdown spectroscopy detection system and method for accurately positioning ablation points, which achieves the purpose of focusing by detecting the diameter or area of a light spot and then adjusting a sample to be detected to an optimal position according to the diameter or area of the light spot, thereby improving the accuracy of sample detection. In the above two patents, a series of system devices such as a three-dimensional moving platform controlled by a microprocessor, a CCD camera device, etc. are required, and the operation and structure are complicated and the execution speed is slow.
Disclosure of Invention
The embodiment of the invention provides an inverted laser-induced breakdown spectroscopy device which can be adjusted in various ways according to the specific optical path of an optical system, only needs to be focused once on repeated sample detection, and greatly improves the efficiency of sample detection.
The embodiment of the invention provides an inverted laser-induced breakdown spectroscopy device, which comprises:
the laser emission module is used for emitting laser pulses;
the sample stage is arranged on a light path of the laser pulse and comprises a displacement platform and an adapter plate, the adapter plate is arranged on the displacement platform, and a through hole is formed in the adapter plate; the adapter plate is used for placing a sample, and the laser pulse is injected from the lower end of the through hole and focused on a plane where the upper end of the through hole is flush with the upper surface of the adapter plate;
and the spectrum acquisition module is used for receiving the composite light emitted by the sample in the laser pulse ablation process and analyzing and processing the composite light.
Preferably, the laser emission module comprises a reflector, a focusing lens and a laser, the laser is used for generating laser pulses, the laser and the reflector are located on the same light path, and the reflector, the focusing lens and the adapter plate are sequentially located on the same light path; the focusing lens is arranged right below the through hole and parallel to the adapter plate.
Preferably, the sample stage further comprises a vertical support frame, and the adapter plate is connected to the displacement platform through the vertical support frame; the adapter plate comprises a transverse plate and a vertical plate which are vertically connected with each other, the vertical plate is connected to the vertical support frame, and a through hole is formed in the transverse plate.
Preferably, the reflector and the focusing lens are both fixed by a fixing bracket.
Preferably, the displacement platform includes a first direction movement axis and a second direction movement axis perpendicular to each other.
Preferably, the device further comprises a third direction moving axis, and the third direction moving axis is perpendicular to the plane where the first direction moving axis and the second direction moving axis are located.
Preferably, the adapter plate is detachably arranged on the vertical support frame; the vertical support frame is detachably arranged on the displacement platform.
Preferably, the vertical support is adjustable in length, or the vertical support comprises a plurality of dimensions.
Preferably, the adapter plate comprises a plurality of specifications, transverse plates of the adapter plate with the plurality of specifications are different in size, and through holes in the transverse plates of the adapter plate with different specifications are different in size.
Preferably, the spectrum acquisition module comprises a spectrum collection probe, an optical fiber, a spectrometer, a detector and a computer; one end of the spectrum collecting probe is close to the lower end of the through hole, and collects compound light emitted by the sample in the laser pulse ablation process; the other end of the laser collecting probe is connected to the spectrometer through an optical fiber, and the composite light is transmitted to the spectrometer; the spectrometer is used for dividing the composite light into monochromatic light radiation signals, converting the monochromatic light radiation signals into digital signals through the detector and sending the digital signals to the computer.
The embodiment of the invention provides an inverted laser-induced breakdown spectroscopy device, which comprises a mobile platform, vertical supporting frames and a switching plate, wherein the mobile platform is connected with the two vertical supporting frames, the two vertical supporting frames can be adjusted to a certain distance relative to the mobile platform, the switching plate is connected to the vertical supporting frames and is fixed relative to the two vertical supporting frames, and a small hole is formed in the middle of the switching plate for placing a sample on the switching plate; laser generated by a pulse laser is focused on a sample from bottom to top through a converging lens, and the side of the sample to be detected is placed downwards, so that secondary focusing is not needed no matter the thickness of the sample, the detection efficiency is greatly improved, and automatic detection can be realized; the structure is simple, various adjustments can be made according to the specific light path of the optical system, focusing is only needed once on repeated sample detection, and the efficiency of sample detection is greatly improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and those skilled in the art can also obtain other drawings according to the drawings without creative efforts.
FIG. 1 is a schematic structural diagram of an inverted laser induced breakdown spectroscopy device according to an embodiment of the invention;
FIG. 2 is a side view of a sample stage according to one embodiment of the present invention;
fig. 3 is a top view of a sample stage according to an embodiment of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the embodiment of the present application, the term "and/or" is only one kind of association relationship describing an associated object, and means that three relationships may exist, for example, a and/or B may mean: a exists alone, A and B exist simultaneously, and B exists alone.
The terms "first" and "second" in the embodiments of the present application are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the present application, the terms "comprise" and "have", as well as any variations thereof, are intended to cover a non-exclusive inclusion. For example, a system, product or apparatus that comprises a list of elements or components is not limited to only those elements or components but may alternatively include other elements or components not expressly listed or inherent to such product or apparatus. In the description of the present application, "plurality" means at least two, e.g., two, three, etc., unless explicitly specifically limited otherwise.
Reference herein to "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment can be included in at least one embodiment of the application. The appearances of the phrase in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments. It is explicitly and implicitly understood by one skilled in the art that the embodiments described herein can be combined with other embodiments.
The LIBS experimental device system mainly comprises a laser, an optical transmission system, a signal detection system, a PC and the like. The optical transmission system mainly realizes the optimized shaping, beam expanding, focusing and the like of laser emergent beams. For an optical system needing focusing, the height difference of a detected sample inevitably causes the distance between a lens and the sample to be indefinite, and the optical lens system needs to be positioned and adjusted to enable the focus of the lens to be aligned with a target sample.
In a laser-induced breakdown spectroscopy experiment, dozens or even hundreds of sets of tests are usually required, extra focusing is not required for samples with consistent thickness, and when samples with inconsistent thickness are encountered, multiple times of focusing work is required. The more samples tested, the longer the detection time required, and the less efficient it becomes. The thickness of different samples is difficult to keep consistent, and the conventional laser-induced breakdown spectroscopy experimental device is difficult to realize the detection with repeatability and automation.
Therefore, the embodiment of the invention provides an inverted laser-induced breakdown spectroscopy device, laser generated by a pulse laser is focused on a sample from bottom to top through a convergent lens, and the side of the sample to be detected is placed downwards, so that the secondary focusing is not needed no matter the thickness of the sample, the detection efficiency is greatly improved, and automatic detection can be realized; the structure is simple, various adjustments can be made according to the specific light path of the optical system, focusing is only needed once on repeated sample detection, and the efficiency of sample detection is greatly improved. The following description and description will proceed with reference being made to various embodiments.
Fig. 1 to 3 illustrate an inverted laser induced breakdown spectroscopy device according to an embodiment of the present invention, including:
the laser emission module is used for emitting laser pulses;
the sample stage is arranged on a light path of the laser pulse, the sample stage comprises a displacement platform 14 and an adapter plate 3, the adapter plate 3 is arranged on the displacement platform 14, and a through hole 12 is formed in the adapter plate 3; the adapter plate 3 is used for placing a sample 2, and the laser pulse is injected from the lower end of the through hole 12 and focused on a plane where the upper end of the through hole 12 is flush with the upper surface of the adapter plate 3;
and the spectrum acquisition module is used for receiving the composite light emitted by the sample in the laser pulse ablation process and analyzing and processing the composite light.
Specifically, as shown in fig. 1, the system further includes a control system 1, a detector 6 and a computer 8, and in order to realize automatic detection of a sample without focusing many times when different samples are replaced, the structure of the embodiment includes a laser emission module, a spectrum collection module and an inverted sample stage; a small hole is arranged in the middle of the adapter plate 3 for placing a sample thereon; the laser generated by the pulse laser 11 is focused on a sample from bottom to top through the convergent lens, and the side of the sample to be detected is placed downwards, so that the secondary focusing is not needed no matter the thickness of the sample, the detection efficiency is greatly improved, and the automatic detection can be realized; the structure is simple, various adjustments can be made according to the specific light path of the optical system, focusing is only needed once on repeated sample detection, and the efficiency of sample detection is greatly improved.
On the basis of the above embodiment, the laser emission module includes a reflecting mirror 10, a focusing lens 9 and a laser 11, the laser 11 is used for generating laser pulses, the laser 11 and the reflecting mirror 10 are located on the same light path, and the reflecting mirror 10, the focusing lens 9 and the adapter plate 3 are sequentially located on the same light path; the focusing lens 9 is arranged right below the through hole 12, and the focusing lens 9 is parallel to the adapter plate 3.
Specifically, the laser 11 is an Nd laser 11 which can generate laser pulse induced plasma; YAG laser emitted from Nd is incident on a reflector 10 and reflected to a focusing lens 9, wherein the light-emitting hole of a laser 11 is on the same line with the reflector 10, the laser reflected by the reflector 10 is perpendicular to the line, and the laser finally converges at the focal point of the lens through the focusing lens 9.
On the basis of the above embodiments, the sample stage further includes a vertical support frame 13, and the adapter plate 3 is connected to the displacement platform 14 through the vertical support frame 13; the adapter plate 3 comprises a transverse plate and a vertical plate which are vertically connected with each other, the vertical plate is connected to the vertical support frame 13, and a through hole 12 is formed in the transverse plate.
On the basis of the above embodiments, the reflecting mirror 10 and the focusing lens 9 are both fixed by a fixing bracket.
On the basis of the above embodiments, the displacement platform 14 includes a first direction displacement axis and a second direction displacement axis perpendicular to each other.
Specifically, the mobile platform is provided with two knobs, the mobile platform can be translated in two directions of x-y manually or under the control of a computer, the travel distance of the two directions of x and y is 50mm, when the mobile platform is controlled by the computer, the mobile platform can be set to have the moving speed of 10mm/s along the x axis, the moving speed of 6mm/s along the y axis, and the acceleration is set to be 5mm/s ^ 2.
In addition to the above embodiments, as another preferable embodiment, a third direction moving axis may be added, and the third direction moving axis is perpendicular to the plane where the first direction moving axis and the second direction moving axis are located.
Specifically, a z-axis adjusting displacement table capable of moving up and down along the z-axis direction is placed on the moving platform, the displacement table can be used for fine adjustment of the system up and down, and the fine adjustment distance at each time is in millimeter level.
On the basis of the above embodiments, the adapter plate 3 is detachably disposed on the vertical support frame 13; the vertical support frame 13 is detachably arranged on the displacement platform 14.
On the basis of the above embodiments, the length of the vertical holder 13 is adjustable, or the vertical holder 13 includes a plurality of sizes. The height of the vertical support 13 of the sample stage can be selected according to the height of the sample to be measured.
Specifically, the vertical supports 13 include two vertical supports 13 fixed on the movable platform, and the edge lines of the two vertical supports 13 are parallel and perpendicular to the movable platform 14. The height of the two vertical supporting frames 13 is 300mm, the horizontal adjustable distance is 34mm-63mm, and the adjustment range is wide.
The vertical support frame 13 is connected to the adapter plate 3. The height of the adapter plate 3 can be adjusted according to the position near the focus of the optical system, and the small hole of the adapter plate 3 is a circle with the diameter of 34 mm. And different adapter plates 3 can be selected according to the general size of the detected sample, the structure is simple, and the practicability is strong.
On the basis of the above embodiments, the adapter plate 3 includes a plurality of specifications, the transverse plates of the adapter plate 3 of the plurality of specifications have different sizes, and the through holes 12 in the transverse plates of the adapter plate 3 of different specifications have different sizes. The adapter plate 3 in the sample stage can be selected according to the size of most samples to be measured.
YAG laser 11 through a reflector 10 to a converging lens, and then from the converging lens to the lens focus, from the bottom to the top focused on the sample to be measured.
On the basis of the above embodiments, the spectrum acquisition module includes a spectrum collection probe 7, an optical fiber 4, a spectrometer 5, a detector and a computer; one end of the spectrum collecting probe 7 is close to the lower end of the through hole 12, and collects the composite light emitted by the sample in the laser pulse ablation process; the other end of the laser collecting probe is connected to the spectrometer 5 through an optical fiber 4, and the composite light is transmitted to the spectrometer 5; the spectrometer 5 is used for dividing the composite light into monochromatic light radiation signals, converting the monochromatic light radiation signals into digital signals through the detector and sending the digital signals to the computer.
In summary, the inverted laser-induced breakdown spectroscopy apparatus provided in the embodiment of the present invention includes a mobile platform, two vertical supports 13, and an adaptor plate 3, wherein the mobile platform is connected to the two vertical supports 13, the two vertical supports 13 can adjust a certain distance with respect to the mobile platform, the adaptor plate 3 is connected to the vertical supports 13, the position of the adaptor plate is fixed with respect to the two vertical supports 13, and a small hole is formed in the middle of the adaptor plate 3 for placing a sample thereon; the laser generated by the pulse laser 11 is focused on a sample from bottom to top through the convergent lens, and the side of the sample to be detected is placed downwards, so that the secondary focusing is not needed no matter the thickness of the sample, the detection efficiency is greatly improved, and the automatic detection can be realized; the structure is simple, various adjustments can be made according to the specific light path of the optical system, focusing is only needed once on repeated sample detection, and the efficiency of sample detection is greatly improved.
The embodiments of the present invention can be arbitrarily combined to achieve different technical effects.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (10)

1. An inverted laser induced breakdown spectroscopy device, comprising:
the laser emission module is used for emitting laser pulses;
the sample stage comprises a displacement platform and an adapter plate, the adapter plate is arranged on the displacement platform, the adapter plate is arranged on a light path of laser pulse, and a through hole is formed in the adapter plate; the adapter plate is used for placing a sample, and the laser pulse is injected from the lower end of the through hole and focused on a plane where the upper end of the through hole is flush with the upper surface of the adapter plate;
and the spectrum acquisition module is used for receiving the composite light emitted by the sample in the laser pulse ablation process and analyzing and processing the composite light.
2. The inverted laser-induced breakdown spectroscopy apparatus of claim 1, wherein the laser emitting module comprises a mirror, a focusing lens, and a laser, the laser is configured to generate laser pulses, the laser and the mirror are located on a same optical path, and the mirror, the focusing lens, and the adapter plate are sequentially located on a same optical path; the focusing lens is arranged right below the through hole and parallel to the adapter plate.
3. The inverted laser induced breakdown spectroscopy device of claim 1, wherein the sample stage further comprises a vertical support frame, and the adapter plate is connected to the displacement platform through the vertical support frame; the adapter plate comprises a transverse plate and a vertical plate which are vertically connected with each other, the vertical plate is connected to the vertical support frame, and a through hole is formed in the transverse plate.
4. The inverted laser induced breakdown spectroscopy device of claim 2, wherein the mirror and the focusing lens are both fixed by a fixed bracket.
5. The inverted laser induced breakdown spectroscopy apparatus of claim 1, wherein the displacement stage comprises a first direction movement axis and a second direction movement axis perpendicular to each other.
6. The inverted laser induced breakdown spectroscopy device of claim 5, further comprising a third axis of motion perpendicular to the plane of the first and second axes of motion.
7. The inverted laser induced breakdown spectroscopy device of claim 3, wherein the adapter plate is removably mounted to the vertical support; the vertical support frame is detachably arranged on the displacement platform.
8. The inverted laser induced breakdown spectroscopy device of claim 7, wherein the vertical support is adjustable in length or comprises a plurality of dimensions.
9. The inverted LIBS device of claim 7, wherein the interposer comprises a plurality of sizes, the cross plates of the interposer of the plurality of sizes are different in size, and the through holes of the cross plates of the interposer of different sizes are different in size.
10. The inverted laser induced breakdown spectroscopy device of claim 1, wherein the spectrum acquisition module comprises a spectrum collection probe, an optical fiber, a spectrometer, a detector and a computer; one end of the spectrum collecting probe is close to the lower end of the through hole, and collects compound light emitted by the sample in the laser pulse ablation process; the other end of the laser collecting probe is connected to the spectrometer through an optical fiber, and the composite light is transmitted to the spectrometer; the spectrometer is used for dividing the composite light into monochromatic light radiation signals, converting the monochromatic light radiation signals into digital signals through the detector, accumulating and amplifying the digital signals and then sending the digital signals to the computer so as to process the digital signals through the computer.
CN202011258079.XA 2020-11-12 2020-11-12 Inverted laser-induced breakdown spectroscopy device Pending CN112557375A (en)

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CN113970540A (en) * 2021-09-09 2022-01-25 华南师范大学 Element isotope analysis system and method based on laser-induced plasma
CN114235517A (en) * 2021-11-16 2022-03-25 北京科技大学 Method for automatically removing oxide layer of LIBS stokehole sample by nine-point surrounding
CN115389487A (en) * 2022-08-08 2022-11-25 苏州星帆华镭光电科技有限公司 Method for detecting components and concentration thereof in object

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CN102661935A (en) * 2012-05-15 2012-09-12 广东电网公司电力科学研究院 LIBS (Laser-induced Breakdown Spectroscopy) belt type powdery material detector
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Publication number Priority date Publication date Assignee Title
CN113970540A (en) * 2021-09-09 2022-01-25 华南师范大学 Element isotope analysis system and method based on laser-induced plasma
CN113970540B (en) * 2021-09-09 2023-07-04 华南师范大学 Elemental isotope analysis system and method based on laser-induced plasma
CN114235517A (en) * 2021-11-16 2022-03-25 北京科技大学 Method for automatically removing oxide layer of LIBS stokehole sample by nine-point surrounding
CN115389487A (en) * 2022-08-08 2022-11-25 苏州星帆华镭光电科技有限公司 Method for detecting components and concentration thereof in object

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