CN103900998A - Accurate target point positioning laser-induced breakdown spectroscopy (LIBS) elemental analyzer and method thereof - Google Patents
Accurate target point positioning laser-induced breakdown spectroscopy (LIBS) elemental analyzer and method thereof Download PDFInfo
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- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
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Abstract
The invention relates to an elemental analyzer, and in particular relates to a laser-induced breakdown spectroscopy (LIBS) elemental analyzer. An accurate target point positioning laser-induced breakdown spectroscopy elemental analyzer is mainly characterized by comprising a pulse laser, wherein a laser beam is conducted onto an analysis sample inside a sample room through a laser transmission system; an accurate target point positioning system is arranged on the sample room; a target sample emission spectrum is connected with a spectrograph through a transmission optical fiber of the accurate target point positioning system. The elemental analyzer has the advantages that the whole suit of LIBS analyzer consists of a laser system, a light guide system, a positioning system and the sample room which are independent, so that the elemental analyzer can be taken as one piece of equipment and also can be used by conveniently replacing laser sources with different parameters, or an in-situ sample can be directly analyzed without using the sample room; the application range of the analyzer is enlarged, and the practicability and the commercialization of an instrument are promoted. The accurate target point positioning system can realize the micron dimension positioning of three-dimensional space and the automatic correction of target points, so that the accuracy of measurement and analysis results of the analysis instrument is improved, and the sensibility of analytical elements of the instrument is promoted.
Description
Technical field
The present invention relates to elemental analyser, particularly the elemental analyser of Laser-induced Breakdown Spectroscopy method.
Background technology
Ultimate analysis has a wide range of applications demand in every field such as metallurgy, food security, environmental monitoring, space explorations.Conventional ultimate analysis means comprise x-ray fluorescence analyzer, inductively-coupled plasma spectrometer, icp ms, atomic absorption spectrophotometer (AAS), laser ablation inductively coupled plasma mass spectrometry etc.But traditional ultimate analysis instrument needs to sample more, and sample is carried out just can analyzing after pre-service, some analytical approach all has larger restriction to sample form, institute's analytical element kind etc.
Laser-induced Breakdown Spectroscopy (LIBS) technology is to utilize light laser to focus on sample surfaces to form plasma, carrys out the analysis means of elemental composition in analytic sample by the characteristic spectral line in measurement plasma emission spectroscopy.Aspect the qualitative and quantitative analysis applied research of the trace element in the samples such as metal, liquid, gas of the method, carry out extensive work.Compared with traditional analysis, still be to need hardly preparation in the feature of developing LIBS technology maximum, little to sample destruction, the features such as sensitivity height, and because this analytical approach only has contacting of light beam and target target, thereby can realize multielement, original position analysis.
Because LIBS technology is to form plasma as basis taking laser ablation analytic sample, and after laser plasma parameters, intensity of emission spectra and laser ablation target material, the fractionating effect of its component etc. is all closely related with laser power density.For specific lasing light emitter, its pulse width, optical maser wavelength are all fixing, and present laser technology can realize the high stability (shake <3%) of pulsed laser energy, therefore the factor, power density after Laser Focusing being had the greatest impact is accurately to control the distance of condenser lens to sample surfaces; For surface irregularity or irregular sample, if can revise in time the distance of lens to analysis site, can increase substantially LIBS skill element analysis precision, further reduce the detectability of element.
At present, can provide in the world the leading firm of commercialization LIBS equipment to have the company such as French IVEA, Britain Applied Photonics.Wherein on the products such as the EasyLIBS of IVEA company, adopt two bundle semiconductor lasers to carry out target spot location, and by camera collection hot spot, judged the design of target spot by naked eyes.For hand-held LIBS equipment carries out express-analysis, this design can meet express-analysis demand.But the target spot for irregular sample is accurately located, improve constituent content analysis precision and duplicate measurements etc. in sample, this device also has certain limitation.In many moneys LIBS of Applied Photonics company product, although applied the design of some taper surface optical element layouts, but in its design, pulse laser transmits along axis, design has reduced Laser Transmission structure like this, but also reduce the controllability of Laser Transmission, and proposed strict demand for the size of laser instrument and LIBS device, be unfavorable for changing the lasing light emitter of different parameters.Just distribute according to pyramidal structure at its optical element, be not fixed on the conical surface, steadiness weakens.In this design, camera is not installed in axis, and does not also adopt three beams of laser location, and therefore, this design is accurately located for the target spot of carrying out irregular sample and element distribution measuring still has limitation.And in this LIBS equipment, there is not environmental gas designs of nozzles yet, limited the application of its ultimate analysis under fundamental research and particular surroundings gas yet.
Summary of the invention
The object of the invention is to, for avoiding the deficiencies in the prior art, provide accurately target spot location of one, easy operating and popularization, have the Laser-induced Breakdown Spectroscopy analytical equipment compared with high analyte precision.The object of the invention is the technical equipment such as semiconductor laser location, ccd image analysis and automatically controlled accurate translation stage to combine, foundation can realize the pinpoint Laser-induced Breakdown Spectroscopy ultimate analysis of target spot instrument.
For achieving the above object, the technical scheme that the present invention takes is: the Laser-induced Breakdown Spectroscopy elemental analyser of a kind of accurate target spot location, its principal feature is to include pulsed laser and by transmission laser system, laser beam is transmitted on the analytic sample in sample chamber, target spot Precise Position System is located on sample chamber, and target sample emission spectrum is connected with spectrometer by the Transmission Fibers that is fixed on target spot Precise Position System.
The Laser-induced Breakdown Spectroscopy elemental analyser of described accurate target spot location, described transmission laser system includes on the passage of pulse laser beam transmission and is provided with the concavees lens in the first laser bundle-enlarging collimation lens combination, convex lens in ultraviolet quartz rectangular prism and the second laser bundle-enlarging collimation lens combination, in condenser lens placing chamber, be provided with Laser Focusing ultraviolet quartz lens, also be provided with characteristic wavelength completely reflecting mirror outward at condenser lens placing chamber, pulse laser beam is successively by the concavees lens in the first laser bundle-enlarging collimation lens combination, convex lens in ultraviolet quartz rectangular prism and the second laser bundle-enlarging collimation lens combination and Laser Focusing ultraviolet quartz lens are radiated on analytic sample after being reflected by characteristic wavelength completely reflecting mirror.
The Laser-induced Breakdown Spectroscopy elemental analyser of described accurate target spot location, it is that taper, outside are columniform metab that described target spot Precise Position System includes inner, be provided with camera head CCD at the center of metab, and on the conical surface of metab, be provided with the semiconductor collimation laser devices of three band focusing, transmitting collimated laser beam focuses on analytic sample surface same point, and this is on the axis of positioning table of placing analytic sample, and range pulse laser beam condenser lens distance is focal length; Plasma spectrometry collecting lens group is arranged in fiber coupler placing chamber, and the lens center of plasma spectrometry collecting lens group is concentric with the position of semiconductor collimation laser device on the conical surface, and focus point is on the surface of analytic sample; Plasma spectrometry collecting lens group connects spectrometer by the optical fiber on optical fiber flange; On the conical surface of target spot Precise Position System, be provided with the LED illuminating lamp for sample chamber intraoral illumination; Also be provided with the environmental gas nozzle that is used to sample surfaces to manufacture the environmental gas of particular types.
The Laser-induced Breakdown Spectroscopy elemental analyser of described accurate target spot location, its top, described sample chamber is connected with target spot Precise Position System, coupling part is with seal with elastometic washer, sample chamber be provided with laser wavelength protection glass for sending sample thief window; Be provided with the automatically controlled displacement platform of three-dimensional of placing analytic sample in its underpart, accurately scan with the three dimensions of realizing sample.
A using method for the Laser-induced Breakdown Spectroscopy elemental analyser of accurate target spot location, the steps include:
First in the time of apparatus installation, three collimation semiconductor lasers of initial setting up transmitting collimated laser beams focus on analytic sample surface same point, and this point is on target spot positioning base axis, and range pulse laser beam condenser lens is apart from being the focal length of lens, the hot spot of technical grade camera head CCD collection analysis collimation laser device, judge that whether three laser beam are in same point, if camera head CCD only observes a hot spot, be that analytic sample is in pulse laser focus place, can carry out Measurement and analysis, if camera head CCD observes three hot spots, interpret sample is not in laser spot place, stop measuring, and control lifting table and move until observe a hot spot, now determine laser spot, coupling fiber points to target spot and overlaps, can carry out LIBS spectral measurement and analysis, and the spectral signal that can obtain.
Because the design adopts three beams semiconductor collimated laser beam, therefore can locate irregular sample target spot, reduce LIBS and analyzed the requirement to sample flatness, and, semiconductor laser its focal spot after carefully optimizing with condenser lens can reach micron dimension, and technical grade CCD resolution micron dimension after optical system imaging, therefore, this system location has very high precision.
Beneficial effect of the present invention:
1) a whole set of LIBS analyser is by independently laser system, light-conducting system, positioning system and sample chamber form, both having can be used as an equipment uses, also the lasing light emitter that can change easily different parameters uses, or do not use sample chamber directly to original position sample analysis, expand the range of application of this analyser, promote practical, the commercialization of instrument.
2) can realize three-dimensional micron dimension location in conjunction with the LIBS target spot Precise Position System of the confocal location of three beams semiconductor laser, ccd image acquisition analysis system, and the automatic correction of target spot, improve the accuracy of analytical instrument Measurement and analysis result, promote the sensitivity of instrumental analysis element.
3) integrated optic path, the accurately design of location, Laser Focusing and spectra collection system, make this LIBS analytical instrument more firm, reliable, and reduce instrumentation personnel operating experiences, safeguarded the requirement of regulation technology, made instrument be easy to extensive popularization.
4) imaging to target material and hand drawing by CCD, can realize target sample element space distribution measuring;
5) in conjunction with laboratory study achievement, increase the environmental gas nozzle coaxial with target center, can create various gaseous environments, enhanced spectrum signal, raising spectral line signal to noise ratio (S/N ratio) and the interference of removal the atmospheric background etc., can meet scientific research demand and special industry application demand.
Brief description of the drawings:
Fig. 1 typical case LIBS principle of device schematic diagram;
Fig. 2 structural representation of the present invention;
The master of Fig. 3 target spot Precise Position System of the present invention embodiment 1 looks diagrammatic cross-section;
Fig. 4 target spot Precise Position System of the present invention embodiment 1 elevational schematic view;
The main diagrammatic cross-section of looking in Fig. 5 sample chamber of the present invention;
Fig. 6 sample chamber of the present invention schematic top plan view;
The master of Fig. 7 target spot Precise Position System of the present invention embodiment 3 looks schematic diagram;
Fig. 8 target spot Precise Position System of the present invention embodiment 3 elevational schematic view;
Fig. 9 testing process schematic diagram of the present invention.
In figure: 1 pulsed laser; 2 transmission laser systems; 3LIBS target spot Precise Position System; 4 sample chambers; 5 Transmission Fibers; 6 spectrometers; 7 ultraviolet quartz rectangular prisms; 8 pulse laser beams; 9 laser bundle-enlarging collimation lens combination; 10 Laser Focusing ultraviolet quartz lenss; 11 condenser lens placing chambers; 12 characteristic wavelength completely reflecting mirrors; 13 spectrum are collected coupled lens group; 14 optical fiber flanges; 15 fiber coupler placing chambers; 16 target spot location technical grade CCD; 17 environmental gas nozzles; 18 three-dimensional accurate Electrocontrolled sample platforms; 19 analytic samples; 20 plasma plumes; 21 target spot location semiconductor lasers; 22 LED light source for illuminating; 23 sample windows with laser wavelength protective window; 24 sample chamber main body frames; 25 pulse valves.
Embodiment
Be described in further detail below in conjunction with the preferred example shown in accompanying drawing:
Embodiment 1: see Fig. 2, the Laser-induced Breakdown Spectroscopy elemental analyser of a kind of accurate target spot location, its principal feature is to include pulsed laser 1 and by transmission laser system 2, laser beam is transmitted on the analytic sample 19 in sample chamber 4, target spot Precise Position System 3 is located on sample chamber 4, and target spot Precise Position System 3 is connected with spectrometer 6 by Transmission Fibers 5.Spectrometer adopts commercial fiber spectrometer or is furnished with the middle echelle spectrometer of intensifier CCD detector.
Described transmission laser system 2 includes and in the transmission channel of pulse laser beam 8, is provided with the first laser bundle-enlarging collimation lens combination concavees lens 9-1, ultraviolet quartz rectangular prism 7 and the second laser bundle-enlarging collimation lens combination convex lens 9-2, in condenser lens placing chamber 11, be provided with Laser Focusing ultraviolet quartz lens 10, outside condenser lens placing chamber 11, be also provided with characteristic wavelength completely reflecting mirror 12, pulse laser beam 8 is successively by the concavees lens 9-1 in the first laser bundle-enlarging collimation lens combination, convex lens 9-2 in ultraviolet quartz rectangular prism 7 and the second laser bundle-enlarging collimation lens combination and Laser Focusing ultraviolet quartz lens 10 are radiated on analytic sample 19 after being reflected by characteristic wavelength completely reflecting mirror 12.Pulse laser system 1 designs because employing is provided with Laser Focusing ultraviolet quartz lens 10 in condenser lens placing chamber 11, thereby can be according to different experiments needs, easily replaces with the other light sources such as psec, femtosecond laser system.
See Fig. 3 and Fig. 4, it is taper, the outside columniform metab 3-1 of being that described target spot Precise Position System 3 includes inner, be provided with camera head CCD16 at metab 3-1 center, and on the conical surface of metab 3-1, be provided with the semiconductor collimation laser devices 21 of three band focusing, transmitting collimated laser beam focuses on the surperficial same point of analytic sample 19, and this is being placed on the axis of analytic sample 19 positioning bases 18, and range pulse laser beam condenser lens 10 distances are focal length; Plasma spectrometry collecting lens group 13 is arranged in fiber coupler placing chamber 15, and the lens center of plasma spectrometry collecting lens group 13 is concentric with the position of semiconductor collimation laser device 21 on the conical surface, and focus point is analytic sample 19 surfaces; The optical fiber 5 that plasma spectrometry scioptics group 13 focuses on optical fiber flange 14 connects spectrometer 6.Metab 3-1 is provided with environmental gas nozzle 17 and points to target sample surfaces to create required gaseous environment; On metab 3-1, be also provided with lighting source LED.
See Fig. 5 and Fig. 6, described 4 its tops, sample chamber are provided with the circular interface matching with positioning system base 3-1 size, can be connected with target spot Precise Position System 3, sample chamber is uncovered, coupling part seals with rubber ring 24-1, sample chamber 4 is provided with the window 23 with laser wavelength protection glass, for sending sample thief; Be provided with the automatically controlled displacement platform 18 of three-dimensional of placing analytic sample 19 in its underpart, analyzed sample is placed on three-dimensional automatically controlled displacement platform 18, accurately scans with the three dimensions of realizing sample.
Because the automatically controlled accurate translation stage precision of three-dimensional can reach nano levelly, and laser focal spot size is in micron dimension, obtains analytic sample pattern by CCD16, and manually draws after track while scan, can realize target sample in the analysis that distributes of element space.
The Laser-induced Breakdown Spectroscopy elemental analyser of accurate target spot of the present invention location, its accurate location survey principle is that three collimation semiconductor laser transmitting collimated laser beams focus on analytic sample surface same point, and this point is on target spot positioning base axis, and target spot range pulse laser beam condenser lens 10 distances are mated with the focal length of lens; The hot spot of technical grade CCD16 collection analysis collimation laser device 21, judge that whether three laser beam are in same point, if CCD only observes a hot spot, can carry out Measurement and analysis, if CCD observes three hot spots, interpret sample, not in laser spot place, is controlled three-dimensional electronic control translation stage correction sample position until observe a hot spot; Because the design adopts three beams semiconductor collimated laser beam, therefore can locate irregular sample target spot, reduce LIBS and analyzed the requirement to sample flatness, and, semiconductor laser its focal spot after carefully optimizing with condenser lens can reach micron dimension, and technical grade CCD resolution micron dimension after optical system imaging, therefore, this system location has very high precision.
When use, laser beam 8 enters Laser Transmission passage from 3-1 lateral wall after light-conducting arm back warp lens combination 9 expands, and quartz lens 10 in embedding condenser lens placing chamber 11 focuses on, and condenser lens position utilizes screw thread snap ring to regulate; Laser beam after focusing is radiated at the surface of analytic sample 19 after being reflected by the high reflective mirror 12 that is arranged on conical seat bottom, form plasma plume 20; Lens are consistent with the focal length of lens to sample surfaces distance; Cone bearing center mounting industrial level CCD16, for taking laser target spot luminescence of plasma image, semiconductor laser hot spot and sample topography etc.; See Fig. 4, after symmetrical 21, three the collimation laser device line focus optimizations of semiconductor collimation laser device that 3 band focusing are installed of the conical surface, form micron order hot spot and irradiate in analytic sample surface same position; Plasma spectrometry collecting lens group 13 is installed in fiber coupler placing chamber 15, lens center is concentric with the position of three beams semiconductor laser on the conical surface, and accurately point to target spot, lens combination is analyzed to spectrometer 6 by the Optical Fiber Transmission being connected on optical fiber flange 14 after plasma spectrometry is collected to focusing; Because plasma light spectrum signal has different Evolutions under varying environment gas, in native system, on the annulus of semiconductor laser position, be also provided with environmental gas nozzle 17, its direction is also accurately pointed to target spot; In addition, can know and obtain sample topography photo in order to place the convenient and CCD of sample, in this system, also configure LED illuminating lamp 22.
In described LIBS analytical equipment, the sequential before laser instrument, spectrometer and CCD is generally by ripe pulse delay signal device, and for example the DG535 of U.S. Stamford, DG645 accurately control, and also can process by designed, designed, and its control accuracy was better than for 1 nanosecond.The business spectrometer that LIBS equipment is conventional is generally also all furnished with laser instrument trigger pip module, and utilizes software to carry out control time delay, therefore, also can realize timing synchronization between each hardware in delay by spectrometer software.
Test process of the present invention, by compact Nd:YAG laser instrument 1 as ablative light sources, laser beam is transmitted through a pair of ultraviolet quartz prism 9, and after being focused on by ultraviolet quartz lens 10, be radiated at analytic sample 19 surfaces, sample is fixed on three-dimensional electronic control translation stage 18, and according to setting track mobile example.The hot spot of the laser beam irradiation that three beams is exported by semiconductor laser 21 on sample surfaces gathered by CCD16, and judge whether with one heart, by controlling accurate electrical-controlled lifting platform, till three beams of laser Shu Tongxin, be that target spot has been located, now, pulse laser beam is concentric with three beams locating laser at sample surfaces hot spot, starts to measure.In sample motion process, CCD continues to monitor three beams semiconductor laser hot spot, and control step motor correction position simultaneously.The plasma spectrometry being produced by pulse laser ablation sample surfaces is analyzed by coupled lens group 13 coupled into optical fibres 5 input spectrum instrument 6.Time delay before spectrometer and laser instrument and CCD is by SRS company of the pulse delay signal device DG645(U.S.) accurately control.
Embodiment 2: the Laser-induced Breakdown Spectroscopy elemental analyser of a kind of accurate target spot location, be used in the irregular sample analysis such as mineral, rock, structure is identical with embodiment 1, different is to use portable power source, do not use sample chamber, directly laser beam foucing is aimed to field target sample measures and analyzes element wherein.
Conventionally LIBS spectral analysis is very responsive for laser power density, and therefore, the flatness of sample surfaces can have a great impact by LIBS analysis result.For undressed ore sample etc., the very out-of-flatness of its surface, collects coupling if can not carefully focus and optimize optical fiber, does not detect possibly any signal.But adopt of the present invention with the pinpoint LIBS analyser of target spot, can determine a plane due to 3, and the total focus of this three beams of laser and optical fiber are collected coupled lens group conllinear, therefore for irregular ore sample etc., cross as long as adjust three beams locating laser, get final product fine coupling spectrum collection system and obtain optimized spectral signal.
Embodiment 3: the Laser-induced Breakdown Spectroscopy elemental analyser of a kind of accurate target spot location, laser mass spectrometry or spectral analysis under vacuum condition.See Fig. 7 and Fig. 8, described CCD camera system 16 is located on the conical surface of metab 3-1, with vacuum seal connected mode, pulse valve 25 is located to metab 3-1 center; Select stainless steel material processing positioning base 3 ?1 simultaneously, and at the blue edge of a knife of its cylinder end face processing method, with intend being connected vacuum chamber sealing docking.The accurate target spot positioning system of the present invention can be used for laser ablation mass spectrum, the spectral analysis location under vacuum condition, and can realize the functions such as the outer original position sample ablation of vacuum chamber, the interior mass spectrophotometry of vacuum chamber.All the other structures are identical with embodiment 1.
The Laser-induced Breakdown Spectroscopy elemental analyser of 4 one kinds of accurate target spot location of embodiment, element space distribution measuring.Structure is identical with embodiment 1.Different is
On the automatically controlled displacement platform of three-dimensional of automatically controlled accurate lifting table composition, accurately scan with the three dimensions of realizing sample.Because the automatically controlled accurate translation stage precision of three-dimensional can reach nano level, and laser focal spot size is in micron dimension, obtain analytic sample pattern by CCD16, and manually gather after Image Rendering electronic control translation stage track while scan according to CCD, after reading track data by translation stage control program, move, simultaneously spectral instrument collection analysis LIBS spectral signal, can obtain the constituent content information of specific region by intensive analysis.By the scanning of zones of different, this system can realize target sample in the analysis that distributes of element space.
Embodiment 5: see Fig. 9, the using method of the Laser-induced Breakdown Spectroscopy elemental analyser of a kind of accurate target spot location, its key step is:
First in the time of apparatus installation, three collimation semiconductor lasers of initial setting up transmitting collimated laser beams focus on analytic sample surface same point, and this point is on target spot positioning base axis, and range pulse laser beam condenser lens 10 is apart from being the focal length of lens; The hot spot of technical grade CCD16 collection analysis collimation laser device 21, judge that whether three laser beam are in same point, if CCD only observes a hot spot, be that analytic sample is in pulse laser focus place, can carry out Measurement and analysis, if CCD observes three hot spots, interpret sample is not in laser spot place, stop measuring, and control lifting table and move until observe a hot spot.
The foregoing is only preferred embodiment of the present invention, in order to limit the present invention, within the spirit and principles in the present invention not all, any amendment of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (5)
1. the Laser-induced Breakdown Spectroscopy elemental analyser of an accurate target spot location, it is characterized in that including pulsed laser is transmitted to laser beam on the analytic sample in sample chamber by transmission laser system, target spot Precise Position System is located on sample chamber, and target sample emission spectrum is connected with spectrometer by the Transmission Fibers that is fixed on target spot Precise Position System.
2. the Laser-induced Breakdown Spectroscopy elemental analyser of accurate target spot as claimed in claim 1 location, transmission laser system described in it is characterized in that includes on the passage of pulse laser beam transmission and is provided with the concavees lens in the first laser bundle-enlarging collimation lens combination, convex lens in ultraviolet quartz rectangular prism and the second laser bundle-enlarging collimation lens combination, in condenser lens placing chamber, be provided with Laser Focusing ultraviolet quartz lens, also be provided with characteristic wavelength completely reflecting mirror outward at condenser lens placing chamber, pulse laser beam is successively by the concavees lens in the first laser bundle-enlarging collimation lens combination, convex lens in ultraviolet quartz rectangular prism and the second laser bundle-enlarging collimation lens combination and Laser Focusing ultraviolet quartz lens are radiated on analytic sample after being reflected by characteristic wavelength completely reflecting mirror.
3. the Laser-induced Breakdown Spectroscopy elemental analyser of accurate target spot as claimed in claim 1 location, it is characterized in that it is that taper, outside are columniform metab that described target spot Precise Position System includes inner, be provided with camera head CCD at the center of metab, and on the conical surface of metab, be provided with the semiconductor collimation laser devices of three band focusing, transmitting collimated laser beam focuses on analytic sample surface same point, and this is on the axis of positioning table of placing analytic sample, and range pulse laser beam condenser lens distance is focal length; Plasma spectrometry collecting lens group is arranged in fiber coupler placing chamber, and the lens center of plasma spectrometry collecting lens group is concentric with the position of semiconductor collimation laser device on the conical surface, and focus point is on the surface of analytic sample; Plasma spectrometry collecting lens group connects spectrometer by the optical fiber on optical fiber flange; On the conical surface of target spot Precise Position System, be provided with the LED illuminating lamp for sample chamber intraoral illumination; Also be provided with the environmental gas nozzle that is used to sample surfaces to manufacture the environmental gas of particular types.
4. the Laser-induced Breakdown Spectroscopy elemental analyser of accurate target spot as claimed in claim 1 location, it is characterized in that described its top, sample chamber is connected with target spot Precise Position System, coupling part is with seal with elastometic washer, sample chamber be provided with laser wavelength protection glass for sending sample thief window; Be provided with the automatically controlled displacement platform of three-dimensional of placing analytic sample in its underpart, accurately scan with the three dimensions of realizing sample.
5. a using method for the Laser-induced Breakdown Spectroscopy elemental analyser of accurate target spot location, the steps include:
First in the time of apparatus installation, three collimation semiconductor lasers of initial setting up transmitting collimated laser beams focus on analytic sample surface same point, and this point is on target spot positioning base axis, and range pulse laser beam condenser lens is apart from being the focal length of lens, the hot spot of technical grade camera head CCD collection analysis collimation laser device, judge that whether three laser beam are in same point, if camera head CCD only observes a hot spot, be that analytic sample is in pulse laser focus place, can carry out Measurement and analysis, if camera head CCD observes three hot spots, interpret sample is not in laser spot place, stop measuring, and control lifting table and move until observe a hot spot, now, determine laser spot, coupling fiber points to target spot and overlaps, can carry out LIBS spectral measurement and analysis, and the spectral signal that can obtain.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410107046.3A CN103900998B (en) | 2014-03-21 | The LIBS elemental analyser of accurate target spot location and method thereof |
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|---|---|---|---|---|
| CN104677885A (en) * | 2015-03-17 | 2015-06-03 | 北京理工大学 | High-spatial-resolution laser differential confocal spectrum-mass spectrum microscopic imaging method and device |
| CN105044052A (en) * | 2015-09-07 | 2015-11-11 | 中国科学院近代物理研究所 | Laser spectrum analysis method and device for elements in liquid |
| CN105115944A (en) * | 2015-09-07 | 2015-12-02 | 北京科技大学 | Automatic focusing method and system for detecting LIBS material compositions |
| CN105866104A (en) * | 2016-05-16 | 2016-08-17 | 浙江大学 | Sample stage filled with protecting gas for detecting laser-induced breakdown spectrum as well as detection system and detection method |
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Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002001191A2 (en) * | 2000-06-29 | 2002-01-03 | Pharma Laser Inc. | System and method for performing a laser-induced breakdown spectroscopy analysis |
| WO2004039530A2 (en) * | 2002-10-25 | 2004-05-13 | Universität Kassel | Adaptive, feedback-controlled material processing using ultra-short laser pulses |
| JP2010019626A (en) * | 2008-07-09 | 2010-01-28 | Toshiba Corp | Element analyzer and element analysis method |
| CN102221539A (en) * | 2011-03-29 | 2011-10-19 | 钢铁研究总院 | Laser-induced breakdown spectrum in-situ analyzer |
| CN102364329A (en) * | 2011-09-19 | 2012-02-29 | 华东师范大学 | Automatic collection system of laser-induced breakdown spectroscopy |
| CN102519918A (en) * | 2011-12-08 | 2012-06-27 | 大连理工大学 | Method for rapid detection of waste oil based on laser-induced breakdown spectroscopy |
| CN102692399A (en) * | 2012-05-25 | 2012-09-26 | 四川大学 | Small multifunctional sample room for LIBS (laser-induced breakdown spectroscopy) |
| CN102841078A (en) * | 2012-09-10 | 2012-12-26 | 北京宝瑞光电科技有限公司 | Integrated laser-induced enhanced plasma spectrum acquisition system |
| CN103175808A (en) * | 2013-03-14 | 2013-06-26 | 中国科学院西安光学精密机械研究所 | Laser-induced breakdown spectroscopy analysis system and laser-induced breakdown spectroscopy analysis method |
| CN203824908U (en) * | 2014-03-21 | 2014-09-10 | 中国科学院近代物理研究所 | Laser-induced breakdown spectroscopy elemental analyzer capable of positioning target spots accurately |
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002001191A2 (en) * | 2000-06-29 | 2002-01-03 | Pharma Laser Inc. | System and method for performing a laser-induced breakdown spectroscopy analysis |
| WO2004039530A2 (en) * | 2002-10-25 | 2004-05-13 | Universität Kassel | Adaptive, feedback-controlled material processing using ultra-short laser pulses |
| WO2004039530A3 (en) * | 2002-10-25 | 2004-11-18 | Univ Kassel | Adaptive, feedback-controlled material processing using ultra-short laser pulses |
| JP2010019626A (en) * | 2008-07-09 | 2010-01-28 | Toshiba Corp | Element analyzer and element analysis method |
| CN102221539A (en) * | 2011-03-29 | 2011-10-19 | 钢铁研究总院 | Laser-induced breakdown spectrum in-situ analyzer |
| CN102364329A (en) * | 2011-09-19 | 2012-02-29 | 华东师范大学 | Automatic collection system of laser-induced breakdown spectroscopy |
| CN102519918A (en) * | 2011-12-08 | 2012-06-27 | 大连理工大学 | Method for rapid detection of waste oil based on laser-induced breakdown spectroscopy |
| CN102692399A (en) * | 2012-05-25 | 2012-09-26 | 四川大学 | Small multifunctional sample room for LIBS (laser-induced breakdown spectroscopy) |
| CN102841078A (en) * | 2012-09-10 | 2012-12-26 | 北京宝瑞光电科技有限公司 | Integrated laser-induced enhanced plasma spectrum acquisition system |
| CN103175808A (en) * | 2013-03-14 | 2013-06-26 | 中国科学院西安光学精密机械研究所 | Laser-induced breakdown spectroscopy analysis system and laser-induced breakdown spectroscopy analysis method |
| CN203824908U (en) * | 2014-03-21 | 2014-09-10 | 中国科学院近代物理研究所 | Laser-induced breakdown spectroscopy elemental analyzer capable of positioning target spots accurately |
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| CN107110769A (en) * | 2014-12-31 | 2017-08-29 | 赛默科技便携式分析仪器有限公司 | LIBS sample chamber |
| CN104677885A (en) * | 2015-03-17 | 2015-06-03 | 北京理工大学 | High-spatial-resolution laser differential confocal spectrum-mass spectrum microscopic imaging method and device |
| CN104677885B (en) * | 2015-03-17 | 2017-09-05 | 北京理工大学 | High-space resolution laser differential confocal spectrum mass spectrum micro imaging method and device |
| CN105044052A (en) * | 2015-09-07 | 2015-11-11 | 中国科学院近代物理研究所 | Laser spectrum analysis method and device for elements in liquid |
| CN105115944A (en) * | 2015-09-07 | 2015-12-02 | 北京科技大学 | Automatic focusing method and system for detecting LIBS material compositions |
| CN105115944B (en) * | 2015-09-07 | 2017-12-29 | 北京科技大学 | A kind of auto focusing method and system for LIBS material composition detections |
| CN105866104B (en) * | 2016-05-16 | 2019-05-07 | 浙江大学 | It is a kind of to fill the sample stage for protecting the laser induced breakdown spectroscopy of gas to detect and detection system and detection method |
| CN105866104A (en) * | 2016-05-16 | 2016-08-17 | 浙江大学 | Sample stage filled with protecting gas for detecting laser-induced breakdown spectrum as well as detection system and detection method |
| CN106442471A (en) * | 2016-10-28 | 2017-02-22 | 段忆翔 | Remote measuring device based on LIBS (laser-induced breakdown spectroscopy) technology |
| CN106289199A (en) * | 2016-11-08 | 2017-01-04 | 佛山科学技术学院 | A kind of location aligner |
| CN106334973A (en) * | 2016-11-08 | 2017-01-18 | 佛山科学技术学院 | Optical positioning alignment instrument |
| CN107064032A (en) * | 2017-04-12 | 2017-08-18 | 江苏农牧科技职业学院 | A kind of liquid concentration measuring device and method |
| CN107727615A (en) * | 2017-10-13 | 2018-02-23 | 中国科学院上海技术物理研究所 | PARTICLE TRANSPORT FROM component associated with light quality spectrum under a kind of planet open environment |
| CN110196245A (en) * | 2018-02-26 | 2019-09-03 | 成都艾立本科技有限公司 | A kind of laser induced breakdown spectroscopy detection system |
| CN108723012A (en) * | 2018-07-18 | 2018-11-02 | 深圳市汇泽激光科技有限公司 | A kind of integrated laser cleaning electro-optical system |
| CN110749546A (en) * | 2018-07-24 | 2020-02-04 | 国合通用测试评价认证股份公司 | Device for accurately positioning laser-induced breakdown spectroscopy focusing position |
| CN109164070A (en) * | 2018-08-21 | 2019-01-08 | 天津科技大学 | LIBS detection system and method for powdered rubber |
| CN109991209B (en) * | 2019-04-09 | 2021-08-24 | 广东博智林机器人有限公司 | Method for identifying taste based on laser-induced breakdown spectroscopy and electronic tongue |
| CN109991209A (en) * | 2019-04-09 | 2019-07-09 | 广东博智林机器人有限公司 | Method and electronic tongues based on laser induced breakdown spectroscopy identification taste |
| CN110261368A (en) * | 2019-08-02 | 2019-09-20 | 平顶山学院 | Sample detection case for laser induced breakdown spectroscopy analysis |
| CN110261368B (en) * | 2019-08-02 | 2023-11-28 | 平顶山学院 | Sample detection box for laser-induced breakdown spectroscopy |
| WO2021159861A1 (en) * | 2020-02-10 | 2021-08-19 | 浙江迪谱诊断技术有限公司 | Laser coaxial ion excitation device |
| CN111413191A (en) * | 2020-03-02 | 2020-07-14 | 中国计量科学研究院 | Sample release system for alkali metal gas cell and control method thereof |
| CN112129742A (en) * | 2020-09-10 | 2020-12-25 | 刘舆帅 | Coal element detector |
| CN112496860B (en) * | 2020-11-27 | 2022-12-06 | 广东佩斯智能装备有限公司 | Method for monitoring service life of turning tool in real time |
| CN112496860A (en) * | 2020-11-27 | 2021-03-16 | 张海强 | Method for monitoring service life of turning tool in real time |
| CN113658845A (en) * | 2021-07-14 | 2021-11-16 | 安图实验仪器(郑州)有限公司 | Laser spot position positioning method suitable for mass spectrometer |
| 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 |
| CN114384011A (en) * | 2021-12-03 | 2022-04-22 | 西安交通大学 | Pulse laser automatic focusing device and method for laser-induced plasma spectrum |
| CN114384011B (en) * | 2021-12-03 | 2023-07-21 | 西安交通大学 | Pulse laser automatic focusing device and method for laser-induced plasma spectrum |
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