CN104007090B - Portable element composition analysis device based on LIBS - Google Patents

Portable element composition analysis device based on LIBS Download PDF

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Publication number
CN104007090B
CN104007090B CN201410225846.5A CN201410225846A CN104007090B CN 104007090 B CN104007090 B CN 104007090B CN 201410225846 A CN201410225846 A CN 201410225846A CN 104007090 B CN104007090 B CN 104007090B
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spectrogrph
chronotron
composition analysis
laser
focus lamp
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CN104007090A (en
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段忆翔
林庆宇
王杰
刘安良
王帅
王旭
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Sichuan University
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Sichuan 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
    • G01N2201/00Features of devices classified in G01N21/00
    • G01N2201/02Mechanical
    • G01N2201/022Casings
    • G01N2201/0221Portable; cableless; compact; hand-held

Abstract

A kind of Portable element composition analysis device based on LIBS of disclosure, including laser instrument 1, it is 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 spectrogrph A5 being connected with fibre-optical probe 4 and spectrogrph B6, it is positioned at the photocell 7 of laser illumination scope, the chronotron 8 being connected with photocell 7, the spectrogrph B6 being connected with chronotron 8, spectrogrph A5, spectrogrph B6 connects industrial control computer mainboard 9 by connection box 12, industrial control computer mainboard 9 connects display 10, industrial control computer mainboard 9 connects chronotron 8, also include electric pressure converter 13, 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. the present invention can meet the elemental composition analysis of outdoor online in situ detection demand, it is possible to automatically focuses on testing sample surface, completes the measurement of element kind and content contained by sample.

Description

Portable element composition analysis device based on LIBS
Technical field
The present invention relates to field of photoelectric technology, particularly relate to a kind of Portable element composition analysis device based on LIBS.
Background technology
At present, the spectral technique that the composition of material is measured mainly has inductively coupled plasma emission spectrography (ICP-AES), atomic absorption spectrography (AAS) (AAS), gas chromatography (GC), mass spectrography (MS) etc., these technology have some limitation, ICP-AES method, AAS method and MS method need sample is carried out pretreatment, GC method is relatively difficult to the accurate qualitative and quantitative analysis of non-pure sample product, the operating difficulties of MS method. When using above-mentioned technology that elemental composition contained by material is analyzed, it is necessary first to collect sample and fetch sample, being then analyzed again, not there is the ability of real-time online in situ detection.
LIBS (LaserInducedBreakdownSpectroscopy), it is called for short LIBS, compensate for disadvantages mentioned above completely, sample is without pretreatment, the qualitative and quantitative analysis of element contained by complex material can be completed, simple to operate, there is the ability of online in site measurement. In addition LIBS measures scope extensively, can measure all elements on the periodic table of elements; Measuring speed is fast, has batch testing ability; Solid, liquid, gas, 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, geological prospecting, on-line monitoring, national defence.
At present, the instrument of LIBS technology is adopted mainly to have desk-top LIBS instrument and two kinds of portable LIBS instrument. Desk-top LIBS instrument needs to take sample to laboratory measurement, it is impossible to play the advantage of the online in site measurement of LIBS technology. And the structure comparison of portable LIBS instrument is flexible, it is suitable for the online in site measurement rigors to apparatus structure motility.Therefore, the exploitation of this portable LIBS instrument has more wide application space.
Summary of the invention
It is desirable to provide a kind of Portable element composition analysis device based on LIBS, the elemental composition analytical equipment of outdoor online in situ detection demand can be met, this device can focus on testing sample surface automatically, completes the measurement of element kind and content contained by sample.
For reaching above-mentioned purpose, the present invention realizes by the following technical solutions:
Portable element composition analysis device based on LIBS disclosed by the invention, including laser instrument, it is 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 spectrogrph A being connected with fibre-optical probe and spectrogrph B, it is positioned at the photocell of laser illumination scope, the chronotron being connected with photocell, the spectrogrph B being connected with chronotron, described spectrogrph A, spectrogrph B connects industrial control computer mainboard by connection box, described industrial control computer mainboard connects display, industrial control computer mainboard connects chronotron, also include 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 include main optical path, dual-wavelength laser autofocus system, control system;
Described main optical path includes first collimating mirror the 26, first reflecting mirror 25, focus lamp 14, and the laser that described laser instrument sends passes sequentially through first collimating mirror the 26, first reflecting mirror the 25, first focus lamp 14, and the position of described focus lamp 14 is adjustable;
Described dual-wavelength laser autofocus system includes focus lamp 14, second reflecting mirror 15, second collimating mirror 16, CCD detects screen 17, 3rd reflecting mirror 18, laser instrument 1, frequency-doubling crystal 20, tooth bar 21, gear 22, micro-step motor 23, slide block 24, the base of described 3rd reflecting mirror 18 and the axes intersect of the second collimating mirror 16, angle between the axis of its reflecting surface and the second collimating mirror 16 is 45, described CCD detection screen 17 is in the focus mirror position about the second reflecting mirror 18 of the second collimating mirror 16, the laser head of described laser instrument 1 is in the focal point of the second collimating mirror 16, described frequency-doubling crystal 20 is fixed on slide block 24, and described slide block 24 is moved 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 made up of following mechanism: the first conductive plate 33 is fixed in mounting seat 34, piezoelectric ceramics lamella 32 is fixed between the first conductive plate 33 and the second conductive plate 31 and is in close contact with the first conductive plate 33 and the second conductive plate 31, described second conductive plate 31 and second slide block 30 one end are connected, described second slide block 30 other end connects slip cap 29, described focus lamp 14 is fixed on connection slip cap 29 by fixing screw 28, second slide block 30 other end is also connected with one end of spring 27, the described other end connecing spring 27 is fixed on the chute suitable with the second slide block 30.
Preferably, described piezoelectric ceramics lamella 32 is formed by least 2 piezoelectric ceramic pieces are bonding.
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 axis and the axis of focus lamp 14 of fibre-optical probe 4 is 60, and its axial location can be regulated by closely-pitched threaded engagement.
Further, the photosensitive mouth of described photocell 7 is placed near the laser head of laser instrument 1. The position of photocell 7 can regulate.
Further, described display 10 is with rotating mechanism.
Further, the delay time of described chronotron 8 passes through serial port setting.
The present invention can focus on automatically, and test scope is wide, and test speed is fast, and volume is little, light weight, carrying convenience, vehicle-mounted can carry out in-situ investigation to open air.
Accompanying drawing explanation
Fig. 1 is principles of the invention block diagram;
Fig. 2 is the main optical path schematic diagram of the present invention;
Fig. 3 is the dual wavelength autofocus system schematic diagram of the present invention;
Fig. 4 is the piezoelectric ceramic actuator sectional view of the present invention;
In figure: 1-lasing light emitter, 2-optics and control system, 3-electroceramics driver, 4-fibre-optical probe, 5-spectrogrph A, 6-spectrogrph B, 7-photocell, 8-chronotron, 9-industrial control computer mainboard, 10-display, 11-power supply, 12-connection box, 13-electric pressure converter, 14-focus lamp, 15-the second reflecting mirror B, 16-the second collimating mirror, 17-CCD screen, 18-the 3rd reflecting mirror, 20-frequency-doubling crystal, 21-tooth bar, 22-gear, 23-micro-step motor, 24-slide block, 25-the first reflecting mirror A, 26-the first collimating mirror A, 27-spring, 28-holding screw, 29-slip cap, 30-slide block, 31-the second conductive plate, 32-piezoelectric ceramics lamella, 33-the first conductive plate, 34-mounting seat.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearly understand, 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 spectrogrph A5 that piezoelectric ceramic actuator 3 that control system 2 is connected with optics and control system 2, fibre-optical probe 4 are connected with fibre-optical probe 4 and spectrogrph B6, be positioned at the spectrogrph B6 that the chronotron 8 that the photocell 7 of laser illumination scope is connected is connected with chronotron 8 with photocell 7, spectrogrph A5, spectrogrph B6 connect industrial control computer mainboard 9 by connection box 12, and the photosensitive mouth of photocell 7 is placed near the laser head of laser instrument 1. The position of photocell 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 be passed through serial port setting by industrial control computer mainboard; Also including electric pressure converter 13, electric pressure converter 13 connects power supply 11, industrial control computer mainboard 9 and chronotron 8; With rotating mechanism bottom display 10, changeable angle is with satisfied observation needs, and above-mentioned parts are all integrated in a Portable suitcase.
The operation principle of the present invention is: the laser head of laser instrument 1 is to quasi-optics and the laser entrance controlling system 2, the laser that laser instrument 1 is got is through the transmission of optics and control system 2 and convergence, arrive testing sample surface excitation plasma, the spectral line that plasma emission goes out is received by fibre-optical probe 4, passed to spectrogrph A5 and spectrogrph B6 by optical fiber, spectrogrph A5 and spectrogrph B6 complete detection and the record of spectral line; The photosensitive mouth of photocell 7 is placed near the laser head of laser instrument 1, and the outfan of photocell 7 is connected with chronotron 8, and chronotron 8 is connected with spectrogrph A5 again, thus realizing the sequencing contro of laser instrument 1 and spectrogrph A5 and spectrogrph 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 and connection box 12, display 10 connect, and connection box 12 and two spectrogrphs are all connected with, thus completing power supply and the data communication of whole system.
Spectrogrph A5 adopts bandwidth to be 250nm-405nm, and lowest resolution is the spectrogrph of 0.1nm, and the inside carries CCD-detector.
Spectrogrph B6 adopts bandwidth to be 400nm-650nm, and lowest resolution is the spectrogrph of 0.1nm, and the inside is also with CCD-detector.
Photocell 7 adopts the photocell that bandwidth is 280nm-680nm that can survey, and detectivity is high, can detect extremely faint optical signal.
Chronotron 8 is connected with spectrogrph by BNC line. Chronotron 8 is after receiving the Transistor-Transistor Logic level signal that photocell 7 transmits, and the time parameter according to setting postpones a period of time, then Transistor-Transistor Logic level signal is passed to spectrogrph, makes spectrogrph A5 open, and gathers data. The time delay of chronotron 8 can be set by serial ports.
Industrial control computer mainboard 9 adopts the industrial control computer mainboard supporting that DC12V power supply is powered. Mainboard 9 is connected by USB line and two mother's USB mouths, and the two USB mother's mouth is stayed on shell, for copying the data of generation. The USB line of mainboard 9 is connected with the printer interface of connection box 12, powers to connection box 12, and the USB interface of mainboard 9 is connected with display 10.
Display 10 passes through hinge together with shell connection now, it is possible to rotate.
Power supply 11 adopts 12VDC power supply, and shell leaves the display lamp of power supply 11, switch and charging inlet.
Several USB interface, power interface, network interface, USB interface is had above connection box 12. Its USB port is connected with spectrogrph 5, spectrogrph 6, powers to spectrogrph.
Electric pressure converter 13 is connected with chronotron 8, industrial control computer mainboard 9. 12VDC Power convert is become 7.5VDC power supply and two kinds of power supplys of 12VDC power supply by electric pressure converter 13, and 7.5VDC power supply is powered to chronotron 8, and 12VDC power supply is powered to industrial control computer mainboard 9.
Owing to the life-span of plasma only has tens microseconds, short in the extreme, the time of plasma emission spectral line is shorter, so needing to accurately control after plasma produces, and the acquisition time of spectrogrph A5 and spectrogrph B6. When laser got by laser instrument 1, photocell 7 almost can receive optical signal at synchronization, convert optical signals into the signal of telecommunication and pass to chronotron 8, chronotron 8 can with 1ns for step-length, remove to regulate the acquisition time of spectrogrph 5 and spectrogrph 6, make there is extraordinary sequential relationship between laser instrument 1 and spectrogrph A5, spectrogrph B6.
Optics and control system 2 include main optical path, dual-wavelength laser autofocus system, control system;
As in figure 2 it is shown, main optical path includes first collimating mirror the 26, first reflecting mirror 25, focus lamp 14, the laser that laser instrument 1 sends passes sequentially through first collimating mirror the 26, first reflecting mirror the 25, first focus lamp 14, and the position of focus lamp 14 is adjustable; Wavelength is the laser of 1064nm, becomes directional light after the first collimating mirror 26, and directional light, after the first reflecting mirror 25 reflection, focuses on through focus lamp 14 again, at testing sample surface excitation plasma.
As shown in Figure 3, dual-wavelength laser autofocus system includes focus lamp 14, second reflecting mirror 15, second collimating mirror 16, CCD detects screen 17, 3rd reflecting mirror 18, frequency-doubling crystal 20, tooth bar 21, gear 22, micro-step motor 23, slide block 24, the base of described 3rd reflecting mirror 18 and the axes intersect of the second collimating mirror 16, angle between the axis of its reflecting surface and the second collimating mirror 16 is 45, described CCD detection screen 17 is in the focus mirror position about the second reflecting mirror 18 of the second collimating mirror 16, the laser head of described laser instrument 1 is in the focal point of the second collimating mirror 16,Frequency-doubling crystal 20 is fixed on slide block 24, and described slide block 24 is moved on slide rail by tooth bar 21, gear 22, micro-step motor 23.
The operation principle of dual-wavelength laser autofocus system is as follows: open laser instrument 1, the 532nm laser produced is gone half through the 3rd reflecting mirror 18 by gear, remaining half by arriving testing sample surface after second collimating mirror the 16, second reflecting mirror 15, focus lamp 14, after reflected; If focus lamp 14 has focused on, testing sample surface is just in the focus of focus lamp 14, and CCD detection screen 17 will form a luminous point; If testing sample surface is in the top of the focus of focus lamp 14, CCD detection screen 17 then can form a right semi-circle hot spot; If testing sample surface is positioned at the lower section of the focus of focus lamp 14, CCD detection screen 17 then can form a left semicircle hot spot. Control system is left semicircle or right semi-circle judges that testing sample surface is at below focus or top by detecting. And then, control system determines the distance between testing sample surface and focus according to energy analysis method, and in control information (voltage signal) output to piezoelectric ceramic actuator 3, piezoelectric ceramic actuator 3 will be controlled and extend or shorten corresponding length, complete automatic focusing. If testing sample can absorb or the light of transmission 532nm wavelength, CCD detection screen 17 just can't detect optical signal, now control system and can export a number of pulse signal to micro-step motor 23, so as to turn over special angle, engaged transmission again through gear 22 and tooth bar 21, make frequency-doubling crystal 20 move a certain distance, enter in light path. The wavelength that laser instrument 1 is got be 532nm light transmission frequency-doubling crystal 20 after reformed into the light that wavelength is 266nm, the light of 266nm will enter in light path, is repeated once said process, completes automatic focusing. Owing to absorbing or the material of light of two kinds of wavelength of transmission 532nm, 266nm is few simultaneously, this focusing system can complete the automatic focusing of majority of material. If by chance running into this material or running into inclined-plane, user switches to Manual Focus Mode, utilize the observability of 532nm laser, by changing output voltage signal ground size, while completing Manual focusing by the mode of eye observation sample surfaces hot spot ground size.
As shown in Figure 4, the position of focus lamp 14 is adjusted by piezoelectric ceramic actuator 3, piezoelectric ceramic actuator 3 is made up of following mechanism: the first conductive plate 33 is fixed in mounting seat 34, mounting seat 34 and suitcase shell are bolted and are fixed together, whole piezoelectric ceramic actuator 3 is secured on suitcase shell, piezoelectric ceramics lamella 32 is fixed between the first conductive plate 33 and the second conductive plate 31 and is in close contact with the first conductive plate 33 and the second conductive plate 31, piezoelectric ceramics lamella 32 is formed by several piezoelectric ceramic pieces are bonding, second conductive plate 31 and second slide block 30 one end are connected, second slide block 30 other end connects slip cap 29, first focus lamp 14 is fixed on connection slip cap 29 by fixing screw 28, second slide block 30 other end is also connected with one end of spring 27, the other end connecing spring 27 is fixed on the chute suitable with the second slide block 30.
Electroceramics driver 3 can come the position of vernier focusing mirror 14 according to the output signal controlling system, second conductive plate the 31, first conductive plate 33 is connected with controlling system by wire, control system is connected with CCD detection screen 17, and the optical signal on CCD detection screen 17 just can be transformed into voltage signal and be loaded on conductive plate 31 and conductive plate 33.When focusing is not fully complete, CCD detection is shielded the optical signal in face on which and is processed, after result passed to control system, control system produces corresponding voltage signal according to the signal of input and exports second and lead conductive plate 31 and first and lead on conductive plate 33, change in voltage causes the electric field intensity being added on piezoelectric ceramics lamella 32 to change, owing to piezoceramic material has inverse piezoelectric effect, piezoelectric ceramics lamella 32 can produce deformation corresponding with electric field intensity variable quantity under the electric field action of Strength Changes, second slide block 30 will promote focus lamp 14 to move corresponding distance and go to focus on.
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 axis and the axis of the first focus lamp 14 of fibre-optical probe 4 is 60, and now, the spectral line signal of most elements is all stronger. The axial location of fibre-optical probe 4 can be regulated by closely-pitched threaded engagement, and now, the spatial discrimination of LIBS signal is better.
Certainly; the present invention also can have other various embodiments; when without departing substantially from present invention spirit and essence thereof; those of ordinary skill in the art can make various corresponding change and deformation according to the present invention, but these change accordingly and deformation all should belong to the scope of the claims appended by the present invention.

Claims (7)

1. based on the Portable element composition analysis device of LIBS, it is characterized in that: include laser instrument (1), it is positioned at the optics of laser instrument (1) front end and controls system (2), the piezoelectric ceramic actuator (3) being connected with optics and control system (2), fibre-optical probe (4), the spectrogrph A (5) being connected with fibre-optical probe (4) and spectrogrph B (6), it is positioned at the photocell (7) of laser illumination scope, the chronotron (8) being connected with photocell (7), the spectrogrph B (6) being connected with chronotron (8), described spectrogrph A (5), spectrogrph B (6) connects industrial control computer mainboard (9) by connection box (12), described industrial control computer mainboard (9) connects display (10), industrial control computer mainboard (9) connects chronotron (8), also include 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,
Described optics and control system (2) include main optical path, dual-wavelength laser autofocus system, control system;
Described main optical path includes the first collimating mirror (26), the first reflecting mirror (25), focus lamp (14), the laser that described laser instrument (1) sends passes sequentially through the first collimating mirror (26), the first reflecting mirror (25), the first focus lamp (14), and the position of described focus lamp (14) is adjustable;
Described dual-wavelength laser autofocus system includes focus lamp (14), second reflecting mirror (15), second collimating mirror (16), CCD detection screen (17), 3rd reflecting mirror (18), frequency-doubling crystal (20), tooth bar (21), gear (22), micro-step motor (23), slide block (24), the base of described 3rd reflecting mirror (18) and the axes intersect of the second collimating mirror (16), angle between the axis of its reflecting surface and the second collimating mirror (16) is 45, described CCD detection screen (17) is in the focus mirror position about the second reflecting mirror (18) of the second collimating mirror (16), the laser head of described laser instrument (1) is in the focal point of the second collimating mirror (16), described frequency-doubling crystal (20) is fixed on slide block (24), and described slide block (24) is moved on slide rail by tooth bar (21), gear (22), micro-step motor (23).
2. the Portable element composition analysis device based on LIBS according to claim 1, 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 made up of following mechanism: the first conductive plate (33) is fixed in mounting seat (34), piezoelectric ceramics lamella (32) is fixed between the first conductive plate (33) and the second conductive plate (31) and is in close contact with the first conductive plate (33) and the second conductive plate (31), described second conductive plate (31) is connected with the second slide block (30) one end, described second slide block (30) other end connects slip cap (29), described focus lamp (14) is fixed in connection slip cap (29) by fixing screw (28), second slide block (30) other end is also connected with one end of spring (27), the described other end connecing spring (27) is fixed on the chute suitable with the second slide block (30).
3. the Portable element composition analysis device based on LIBS according to claim 2, it is characterised in that: described piezoelectric ceramics lamella (32) is formed by least 2 piezoelectric ceramic pieces are bonding.
4. the Portable element composition analysis device based on LIBS according to claim 1, it is characterized in that: described fibre-optical probe (4) has 8 groups, all adopt bifurcation fiber, they are evenly distributed on the surrounding of the first focus lamp (14), angle between axis and the axis of focus lamp (14) of fibre-optical probe (4) is 60, and its axial location can be regulated by closely-pitched threaded engagement.
5. the Portable element composition analysis device based on LIBS according to claim 1, it is characterized in that: the photosensitive mouth of described photocell (7) is placed near the laser head of laser instrument (1), the position of photocell (7) can regulate.
6. the Portable element composition analysis device based on LIBS according to claim 1, it is characterised in that: described display (10) is with rotating mechanism.
7. the Portable element composition analysis device based on LIBS according to claim 1, it is characterised in that: the delay time of described chronotron (8) passes through serial port setting.
CN201410225846.5A 2014-05-27 2014-05-27 Portable element composition analysis device based on LIBS Active CN104007090B (en)

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