CN104007090A - Portable elementary composition analysis device based on laser-induced breakdown spectroscopy technology - Google Patents
Portable elementary composition analysis device based on laser-induced breakdown spectroscopy technology Download PDFInfo
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- CN104007090A CN104007090A CN201410225846.5A CN201410225846A CN104007090A CN 104007090 A CN104007090 A CN 104007090A CN 201410225846 A CN201410225846 A CN 201410225846A CN 104007090 A CN104007090 A CN 104007090A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- 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
- G01N21/718—Laser microanalysis, i.e. with formation of sample plasma
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2201/00—Features of devices classified in G01N21/00
- G01N2201/02—Mechanical
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- G01N2201/0221—Portable; cableless; compact; hand-held
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Abstract
The invention discloses a portable elementary composition analysis device based on a laser-induced breakdown spectroscopy technology. The portable elementary composition analysis device comprises a laser 1, an optical and control system 2 positioned at the front end of the laser 1, a piezoelectric ceramic driver 3 connected with the optical and control system 2, an optical fiber probe 4, a spectrograph A5 and a spectrograph B6 which are connected with the optical fiber probe 4, a phototube 7 positioned in an irradiation range of the laser, a time delayer 8 connected with the phototube 7, and a spectrograph B6 connected with the time delayer 8, wherein the spectrograph A5 and the spectrograph B6 are connected with an industrial personal computer mainboard 9 through a concentrating box 12; the industrial personal computer mainboard 9 is connected with a display 10; the industrial personal computer mainboard 9 is connected with the time delayer 8; the portable elementary composition analysis device also comprises a voltage converter 13; the voltage converter 13 is connected with a power supply 11, the industrial personal computer mainboard 9 and the time delayer 8; all the parts are integrated in a portable suitcase. The elementary composition analysis with outdoor online in-situ detection requirements can be met, the device can be automatically focused to the surface of a sample to be detected, and the type and content of elements contained in the sample are measured.
Description
Technical field
The present invention relates to field of photoelectric technology, relate in particular to a kind of Portable element composition analysis device based on Laser-induced Breakdown Spectroscopy technology.
Background technology
At present, the spectral technique that the composition of material is measured mainly contains inductively coupled plasma emission spectrography (ICP-AES), atomic absorption spectrography (AAS) (AAS), gas chromatography (GC), mass spectroscopy (MS) etc., these technology have some limitation, ICP-AES method, AAS method and MS method need to be carried out pre-service to sample, GC method is more difficult to the accurate qualitative and quantitative analysis of non-pure sample product, the operating difficulties of MS method.When using above-mentioned technology to analyze the contained elemental composition of material, first need to collect sample and fetch sample, and then analyzing, not thering is the ability of real-time online in situ detection.
Laser-induced Breakdown Spectroscopy technology (Laser Induced Breakdown Spectroscopy), be called for short LIBS, made up above-mentioned shortcoming completely, sample is without pre-service, can complete the qualitative and quantitative analysis of the contained element of complex material, simple to operate, there is the ability of online in site measurement.In addition LIBS measurement range is wide, can measure all elements on the periodic table of elements; Measuring speed is fast, has batch testing ability; Solid, liquid, gas, suspended particle all can be measured, and have heterogeneous mensuration ability.Owing to having above-mentioned advantage, LIBS can be widely used in fields such as metallurgical analysis, environmental monitoring, geologic prospecting, on-line monitoring, national defence.
At present, adopt the instrument of LIBS technology to mainly contain two kinds, desk-top LIBS instrument and portable LIBS instrument.Desk-top LIBS appliance requires takes sample to laboratory measurement, can not bring into play the advantage of the online in site measurement of LIBS technology.And the structure of portable LIBS instrument is more flexible, more can adapt to the harsh requirement of online in site measurement to apparatus structure dirigibility.Therefore, the exploitation of this portable LIBS instrument has more wide application space.
Summary of the invention
The present invention aims to provide a kind of Portable element composition analysis device based on Laser-induced Breakdown Spectroscopy technology, can meet the elemental composition analytical equipment of outdoor online in situ detection demand, this device can automatic focus arrive testing sample surface, completes the measurement of the contained element contamination of sample.
For achieving the above object, the present invention realizes by the following technical solutions:
Portable element composition analysis device based on Laser-induced Breakdown Spectroscopy technology disclosed by the invention, comprise laser instrument, be positioned at optics and the control system of laser instrument front end, the piezoelectric ceramic actuator being connected with optics and control system, fibre-optical probe, the spectrometer A being connected with fibre-optical probe and spectrometer B, be positioned at the photoelectric tube of laser illumination scope, the chronotron being connected with photoelectric tube, the spectrometer B being connected with chronotron, described spectrometer A, spectrometer B connects industrial control computer mainboard by cable concentrator, described industrial control computer mainboard connects display, industrial control computer mainboard connects chronotron, also comprise electric pressure converter, described electric pressure converter connects power supply, industrial control computer mainboard and chronotron, above-mentioned parts are all integrated in a Portable suitcase.
Further, described optics and control system comprise main optical path, dual-wavelength laser autofocus system, control system;
Described main optical path comprises the first collimating mirror 26, the first catoptron 25, focus lamp 14, and the laser that described laser instrument sends is successively by the first collimating mirror 26, the first catoptron 25, the first focus lamp 14, and the position of described focus lamp 14 is adjustable;
Described dual-wavelength laser autofocus system comprises focus lamp 14, the second catoptron 15, the second collimating mirror 16, CCD detects screen 17, the 3rd catoptron 18, laser instrument 1, frequency-doubling crystal 20, tooth bar 21, gear 22, micro-step motor 23, slide block 24, the axes intersect of the base of described the 3rd catoptron 18 and the second collimating mirror 16, angle between the axis of its reflecting surface and the second collimating mirror 16 is 45 ゜, described CCD detects screen 17 and is in the focus of the second collimating mirror 16 about the mirror position of the second catoptron 18, the laser head of described laser instrument 1 is in the focus place of the second collimating mirror 16, described frequency-doubling crystal 20 is fixed on slide block 24, and described slide block 24 moves on slide rail by tooth bar 21, gear 22, micro-step motor 23.
Further, the position of described focus lamp 14 is adjusted by piezoelectric ceramic actuator 3, described piezoelectric ceramic actuator 3 is comprised of following mechanism: the first current-carrying plate 33 is fixed on mount pad 34, piezoelectric ceramics lamella 32 be fixed between the first current-carrying plate 33 and the second current-carrying plate 31 and with the first current-carrying plate 33 and the second current-carrying plate 31 close contacts, described the second current-carrying plate 31 and second slide block 30 one end are connected, described second slide block 30 other ends connect slip cap 29, described focus lamp 14 is fixed on and is connected on slip cap 29 by gib screw 28, second slide block 30 other ends are one end of linking springs 27 also, the described other end that connects spring 27 is fixed on the chute suitable with the second slide block 30.
Preferably, described piezoelectric ceramics lamella 32 is by least 2 bonding formation of piezoelectric ceramic piece.
Further, described fibre-optical probe 4 adopts bifurcation fiber, and one has 8 groups, is evenly distributed on the surrounding of the first focus lamp 14, and the angle between the axis of fibre-optical probe 4 and the axis of focus lamp 14 is 60 ゜, and its axial location can be coordinated and be regulated by closely-pitched spiral.
Further, the sensitization mouth of described photoelectric tube 7 is placed near the laser head of laser instrument 1.The position of photoelectric tube 7 can regulate.
Further, described display 10 is with rotating mechanism.
Further, the delay time of described chronotron 8 passes through serial port setting.
Energy automatic focus of the present invention, test specification is wide, and test speed is fast, and volume is little, quality light, carrying convenience, can vehicle-mountedly to open air, carry out in-situ investigation.
Accompanying drawing explanation
Fig. 1 is theory diagram of the present invention;
Fig. 2 is main optical path schematic diagram of the present invention;
Fig. 3 is dual wavelength autofocus system schematic diagram of the present invention;
Fig. 4 is piezoelectric ceramic actuator cut-open view of the present invention;
In figure: 1-lasing light emitter, 2-optics and control system, 3-electroceramics driver, 4-fibre-optical probe, 5-spectrometer A, 6-spectrometer B, 7-photoelectric tube, 8-chronotron, 9-industrial control computer mainboard, 10-display, 11-power supply, 12-cable concentrator, 13-electric pressure converter, 14-focus lamp, 15-the second catoptron B, 16-the second collimating mirror, 17-CCD screen, 18-the 3rd catoptron, 20-frequency-doubling crystal, 21-tooth bar, 22-gear, 23-micro-step motor, 24-slide block, 25-the first catoptron A, 26-the first collimating mirror A, 27-spring, 28-holding screw, 29-slip cap, 30-slide block, 31-the second current-carrying plate, 32-piezoelectric ceramics lamella, 33-the first current-carrying plate, 34-mount pad.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with accompanying drawing, the present invention is further elaborated.
As shown in Figure 1, the present invention includes laser instrument 1, be positioned at the optics of laser instrument 1 front end and control system 2, the piezoelectric ceramic actuator 3 being connected with optics and control system 2, fibre-optical probe 4, the spectrometer A5 that is connected with fibre-optical probe 4 and spectrometer B6, the photoelectric tube 7 that is positioned at laser illumination scope, the chronotron 8 being connected with photoelectric tube 7, the spectrometer B6 that is connected with chronotron 8, spectrometer A5, spectrometer B6 connect industrial control computer mainboard 9 by cable concentrator 12, and the sensitization mouth of photoelectric tube 7 is placed near the laser head of laser instrument 1.The position of photoelectric tube 7 can regulate, and industrial control computer mainboard 9 connects display 10, and industrial control computer mainboard 9 connects chronotron 8, and the delay time of chronotron 8 can pass through serial port setting by industrial control computer mainboard; Also comprise electric pressure converter 13, electric pressure converter 13 connects power supply 11, industrial control computer mainboard 9 and chronotron 8; Display 10 bottoms are with rotating mechanism, and changeable angle is to meet observation needs, and above-mentioned parts are all integrated in a Portable suitcase.
Principle of work of the present invention is: the laser head alignment optical of laser instrument 1 and the laser entrance of control system 2, the laser that laser instrument 1 is got is through transmission and the convergence of optics and control system 2, arrive testing sample surface excitation plasma, the spectral line that plasma emission goes out is received by fibre-optical probe 4, by optical fiber transmission, pass spectrometer A5 and spectrometer B6, by spectrometer A5 and spectrometer B6, completed detection and the record of spectral line; The sensitization mouth of photoelectric tube 7 is placed near the laser head of laser instrument 1, and the output terminal of photoelectric tube 7 is connected with chronotron 8, and chronotron 8 is connected with spectrometer A5 again, thereby realizes the sequential control of laser instrument 1 and spectrometer A5 and spectrometer B6.Power supply 11 is connected with electric pressure converter 13, electric pressure converter 13 is connected with chronotron 8, industrial control computer mainboard 9, industrial control computer mainboard 9 is connected with cable concentrator 12, display 10, and cable concentrator 12 is all connected with two spectrometers, thereby completes power supply and the data communication of whole system.
It is 250nm-405nm that spectrometer A5 adopts bandwidth, the spectrometer that lowest resolution is 0.1nm, and the inside carries CCD detecting device.
It is 400nm-650nm that spectrometer B6 adopts bandwidth, the spectrometer that lowest resolution is 0.1nm, and the inside is also with CCD detecting device.
The photoelectric tube that the bandwidth that photoelectric tube 7 employings can be surveyed is 280nm-680nm, detection sensitivity is high, can detect extremely faint light signal.
Chronotron 8 is connected with spectrometer by BNC line.Chronotron 8, after receiving the Transistor-Transistor Logic level signal that photoelectric tube 7 transmits, postpones a period of time according to the time parameter of setting, then Transistor-Transistor Logic level signal is passed to spectrometer, spectrometer A5 is opened, image data.Can set the time delay of chronotron 8 by serial ports.
Industrial control computer mainboard 9 adopts the industrial control computer mainboard of supporting DC12V Power supply.Mainboard 9 is connected with female mouthful of two USB by USB line, and the female mouth of these two USB is stayed on shell, for copying the data of generation.The USB line of mainboard 9 is connected with the printer interface of cable concentrator 12, gives cable concentrator 12 power supplies, and the VGA interface of mainboard 9 is connected with display 10.
Display 10 can rotate together with connecting now by hinge and shell.
Power supply 11 adopts 12V DC power supply, leaves pilot lamp, switch and the charging inlet of power supply 11 on shell.
Cable concentrator 12 has several USB interface, power interface, network interface, VGA interface above.Its USB mouth is connected with spectrometer 5, spectrometer 6, to spectrometer, powers.
Electric pressure converter 13 is connected with chronotron 8, industrial control computer mainboard 9.Electric pressure converter 13 converts 12V DC power supply to 7.5V DC power supply and two kinds of power supplys of 12V DC power supply, and 7.5V DC power supply is to chronotron 8 power supplies, and 12V DC power supply is to industrial control computer mainboard 9 power supplies.
Because the life-span of plasma only has tens microseconds, short in the extreme, the time of plasma emission spectral line is shorter, so need to accurately control after plasma generation the acquisition time of spectrometer A5 and spectrometer B6.When laser instrument 1 is got laser, photoelectric tube 7 almost can receive light signal at synchronization, convert light signal to electric signal and pass to chronotron 8, chronotron 8 can be take 1ns as step-length, remove to regulate the acquisition time of spectrometer 5 and spectrometer 6, making has extraordinary sequential relationship between laser instrument 1 and spectrometer A5, spectrometer B6.
Optics and control system 2 comprise main optical path, dual-wavelength laser autofocus system, control system;
As shown in Figure 2, main optical path comprises the first collimating mirror 26, the first catoptron 25, focus lamp 14, and the laser that laser instrument 1 sends is successively by the first collimating mirror 26, the first catoptron 25, the first focus lamp 14, and the position of focus lamp 14 is adjustable; Wavelength is the laser of 1064nm, after the first collimating mirror 26, becomes directional light, and directional light, after the first catoptron 25 reflections, focuses on through focus lamp 14 again, at testing sample surface excitation plasma.
As shown in Figure 3, dual-wavelength laser autofocus system comprises focus lamp 14, the second catoptron 15, the second collimating mirror 16, CCD detects screen 17, the 3rd catoptron 18, frequency-doubling crystal 20, tooth bar 21, gear 22, micro-step motor 23, slide block 24, the axes intersect of the base of described the 3rd catoptron 18 and the second collimating mirror 16, angle between the axis of its reflecting surface and the second collimating mirror 16 is 45 ゜, described CCD detects screen 17 and is in the focus of the second collimating mirror 16 about the mirror position of the second catoptron 18, the laser head of described laser instrument 1 is in the focus place of the second collimating mirror 16, frequency-doubling crystal 20 is fixed on slide block 24, and described slide block 24 moves on slide rail by tooth bar 21, gear 22, micro-step motor 23.
The principle of work of dual-wavelength laser autofocus system is as follows: open laser instrument 1, the 532nm laser producing is gone half through the 3rd catoptron 18 by gear, remaining half be by the second collimating mirror 16, the second catoptron 15, the rear arrival testing sample of focus lamp 14 surface, after be reflected; If focus lamp 14 has focused on, testing sample surface is just in time in the focus of focus lamp 14, and CCD detects on screen 17 will form a luminous point; If the top of the focus of testing sample surface in focus lamp 14, CCD detects on screen 17 can form a right semi-circle hot spot; If testing sample surface is positioned at the below of the focus of focus lamp 14, CCD detects on screen 17 can form a left semicircle hot spot.Control system is that left semicircle or right semi-circle judge that testing sample surface is in focus below or top by detection.And then, control system is determined the distance between testing sample surface and focus according to energy analysis method, and control information (voltage signal) is outputed on piezoelectric ceramic actuator 3, control piezoelectric ceramic actuator 3 and extend or shorten corresponding length, complete automatic focus.If testing sample can absorb or the light of transmission 532nm wavelength, at CCD, detect on screen 17 and just can't detect light signal, the pulse signal that now control system can be exported some is to micro-step motor 23, make it to turn over special angle, again by the engaged transmission of gear 22 and tooth bar 21, frequency-doubling crystal 20 is moved a certain distance, enter into light path.The wavelength that laser instrument 1 is got is after the light transmission frequency-doubling crystal 20 of 532nm, just to have become the light that wavelength is 266nm, and the light of 266nm will enter in light path, repeats one time said process, completes automatic focus.Due to absorb simultaneously or the material of the light of transmission 532nm, two kinds of wavelength of 266nm few, this focusing system can complete the automatic focus of most materials.If by chance run into this material or run into inclined-plane, user switches to Manual focusing pattern, utilize the observability of 532nm laser, one side by changing output voltage signal ground size, complete Manual focusing Yi Bian observe the big or small mode in sample surfaces hot spot ground with eyes.
As shown in Figure 4, the position of focus lamp 14 is adjusted by piezoelectric ceramic actuator 3, piezoelectric ceramic actuator 3 is comprised of following mechanism: the first current-carrying plate 33 is fixed on mount pad 34, mount pad 34 is bolted and is fixed together with suitcase shell, whole piezoelectric ceramic actuator 3 is just fixed on suitcase shell, piezoelectric ceramics lamella 32 be fixed between the first current-carrying plate 33 and the second current-carrying plate 31 and with the first current-carrying plate 33 and the second current-carrying plate 31 close contacts, piezoelectric ceramics lamella 32 forms by several piezoelectric ceramic pieces are bonding, the second current-carrying plate 31 and second slide block 30 one end are connected, second slide block 30 other ends connect slip cap 29, the first focus lamp 14 is fixed on and is connected on slip cap 29 by gib screw 28, second slide block 30 other ends are one end of linking springs 27 also, the other end that connects spring 27 is fixed on the chute suitable with the second slide block 30.
Electroceramics driver 3 can come according to the output signal of control system the position of vernier focusing mirror 14, the second current-carrying plate 31, the first current-carrying plate 33 are connected with control system by wire, control system detects screen 17 with CCD and is connected, and the light signal on CCD detection screen 17 just can be transformed into voltage signal and be loaded on current-carrying plate 31 and current-carrying plate 33.When having focused on, CCD detects screen the light signal above it is processed, after result is passed to control system, control system produces corresponding voltage signal according to the signal of input and outputs to second and lead current-carrying plate 31 and first and lead on current-carrying plate 33, change in voltage causes that the electric field intensity being added on piezoelectric ceramics lamella 32 changes, because piezoceramic material has inverse piezoelectric effect, piezoelectric ceramics lamella 32 can produce and the corresponding deformation of electric field intensity variable quantity under the electric field action of Strength Changes, the second slide block 30 will promote focus lamp 14 and move corresponding distance and gone focusing.
Fibre-optical probe 4 one has 8 groups, all adopts bifurcation fiber, and they are evenly distributed on the surrounding of the first focus lamp 14, and the angle between the axis of fibre-optical probe 4 and the axis of the first focus lamp 14 is 60 ゜, and now, the spectral line signal of most elements is all more intense.The axial location of fibre-optical probe 4 can be coordinated and be regulated by closely-pitched spiral, and now, the spatial discrimination of LIBS signal is better.
Certainly; the present invention also can have other various embodiments; in the situation that not deviating from spirit of the present invention and essence thereof; those of ordinary skill in the art can make according to the present invention various corresponding changes and distortion, but these corresponding changes and distortion all should belong to the protection domain of the appended claim of the present invention.
Claims (8)
1. the Portable element composition analysis device based on Laser-induced Breakdown Spectroscopy technology, it is characterized in that: comprise laser instrument 1, be positioned at optics and the control system 2 of laser instrument 1 front end, the piezoelectric ceramic actuator 3 being connected with optics and control system 2, fibre-optical probe 4, the spectrometer A5 being connected with fibre-optical probe 4 and spectrometer B6, be positioned at the photoelectric tube 7 of laser illumination scope, the chronotron 8 being connected with photoelectric tube 7, the spectrometer B6 being connected with chronotron 8, described spectrometer A5, spectrometer B6 connects industrial control computer mainboard 9 by cable concentrator 12, described industrial control computer mainboard 9 connects display 10, industrial control computer mainboard 9 connects chronotron 8, also comprise electric pressure converter 13, described electric pressure converter 13 connects power supply 11, industrial control computer mainboard 9 and chronotron 8, above-mentioned parts are all integrated in a Portable suitcase.
2. the Portable element composition analysis device based on Laser-induced Breakdown Spectroscopy technology according to claim 1, is characterized in that: described optics and control system 2 comprise main optical path, dual-wavelength laser autofocus system, control system;
Described main optical path comprises the first collimating mirror 26, the first catoptron 25, focus lamp 14, and the laser that described laser instrument 1 sends is successively by the first collimating mirror 26, the first catoptron 25, the first focus lamp 14, and the position of described focus lamp 14 is adjustable;
Described dual-wavelength laser autofocus system comprises focus lamp 14, the second catoptron 15, the second collimating mirror 16, CCD detects screen 17, the 3rd catoptron 18, frequency-doubling crystal 20, tooth bar 21, gear 22, micro-step motor 23, slide block 24, the axes intersect of the base of described the 3rd catoptron 18 and the second collimating mirror 16, angle between the axis of its reflecting surface and the second collimating mirror 16 is 45 ゜, described CCD detects screen 17 and is in the focus of the second collimating mirror 16 about the mirror position of the second catoptron 18, the laser head of described laser instrument 1 is in the focus place of the second collimating mirror 16, described frequency-doubling crystal 20 is fixed on slide block 24, and described slide block 24 moves on slide rail by tooth bar 21, gear 22, micro-step motor 23.
3. the Portable element composition analysis device based on Laser-induced Breakdown Spectroscopy technology according to claim 2, it is characterized in that: the position of described focus lamp 14 is adjusted by piezoelectric ceramic actuator 3, described piezoelectric ceramic actuator 3 is comprised of following mechanism: the first current-carrying plate 33 is fixed on mount pad 34, piezoelectric ceramics lamella 32 be fixed between the first current-carrying plate 33 and the second current-carrying plate 31 and with the first current-carrying plate 33 and the second current-carrying plate 31 close contacts, described the second current-carrying plate 31 and second slide block 30 one end are connected, described second slide block 30 other ends connect slip cap 29, described focus lamp 14 is fixed on and is connected on slip cap 29 by gib screw 28, second slide block 30 other ends are one end of linking springs 27 also, the described other end that connects spring 27 is fixed on the chute suitable with the second slide block 30.
4. the Portable element composition analysis device based on Laser-induced Breakdown Spectroscopy technology according to claim 3, is characterized in that: described piezoelectric ceramics lamella 32 is by least 2 bonding formation of piezoelectric ceramic piece.
5. the Portable element composition analysis device based on Laser-induced Breakdown Spectroscopy technology according to claim 2, it is characterized in that: described fibre-optical probe 4 one has 8 groups, all adopt bifurcation fiber, they are evenly distributed on the surrounding of the first focus lamp 14, angle between the axis of the axis of fibre-optical probe 4 and focus lamp 14 is 60 ゜, and its axial location can be coordinated and be regulated by closely-pitched spiral.
6. the Portable element composition analysis device based on Laser-induced Breakdown Spectroscopy technology according to claim 1, is characterized in that: the sensitization mouth of described photoelectric tube 7 is placed near the laser head of laser instrument 1, and the position of photoelectric tube 7 can regulate.
7. the Portable element composition analysis device based on Laser-induced Breakdown Spectroscopy technology according to claim 1, is characterized in that: described display 10 is with rotating mechanism.
8. the Portable element composition analysis device based on Laser-induced Breakdown Spectroscopy technology according to claim 1, is characterized in that: the delay time of described chronotron 8 passes through serial port setting.
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| CN104655595A (en) * | 2015-02-11 | 2015-05-27 | 北京农业智能装备技术研究中心 | Analysis system and analysis method of laser induced breakdown spectroscopy |
| CN105092539A (en) * | 2014-12-17 | 2015-11-25 | 天津陆海石油设备系统工程有限责任公司 | Laser-induced breakdown spectrum analyzer |
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