CN113281257A - Laser-induced breakdown spectroscopy element analysis system - Google Patents

Laser-induced breakdown spectroscopy element analysis system Download PDF

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Publication number
CN113281257A
CN113281257A CN202110616046.6A CN202110616046A CN113281257A CN 113281257 A CN113281257 A CN 113281257A CN 202110616046 A CN202110616046 A CN 202110616046A CN 113281257 A CN113281257 A CN 113281257A
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laser
signal
sample
induced breakdown
breakdown spectroscopy
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黄莎莎
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Spectrum Times Beijing Technology Co ltd
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Spectrum Times Beijing Technology Co ltd
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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
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • 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
    • G01N21/73Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches

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  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
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Abstract

The invention relates to the technical field of laser-induced breakdown spectroscopy, in particular to a laser-induced breakdown spectroscopy elemental analysis system which comprises a sample chamber, wherein a sampling platform, a spectrometer, a laser, a condenser lens, a camera, a scanning device, an integrated blowing device, an illuminating device and a computer are arranged in the sample chamber, the laser comprises a main laser and an auxiliary laser which are orthogonally arranged, the main laser vertically bombards the surface of a sample, the auxiliary laser horizontally bombards an ablation plume section excited by the main laser from the side surface to obviously enhance a radiation signal of plasma, the condenser lens is used for focusing pulses emitted by the laser, and compared with a single-pulse LIBS system, the laser-induced breakdown spectroscopy elemental analysis system supports a user to flexibly adjust different wavelengths and powers to use the laser through a measurement process management unit, and adjusts parameters such as interval time and focus position of double pulses, is very suitable for LIBS mechanism research and the requirement of industrial application.

Description

Laser-induced breakdown spectroscopy element analysis system
Technical Field
The invention relates to the technical field of laser-induced breakdown spectroscopy, in particular to a laser-induced breakdown spectroscopy element analysis system.
Background
In many occasions, scanning imaging and content analysis of elements in a sample are required, and the traditional spectral analysis methods, such as atomic absorption spectroscopy, atomic fluorescence spectroscopy, inductively coupled plasma-atomic emission spectroscopy, inductively coupled plasma-mass spectrometry and the like, generally require pretreatment of the sample, and are slow in analysis speed; a Laser-induced Breakdown Spectroscopy (LIBS) technology based on low repetition frequency is used as an atomic spectrum analysis technology, a beam of high-energy pulse Laser is focused on the surface of a sample to be analyzed to generate high-temperature plasma, a small amount of substances stripped by the Laser are atomized and ionized in the high-temperature plasma, characteristic spectrum radiation of atoms or ions is emitted, and the analysis of the element concentration (or content) in the sample is realized by analyzing the spectrum intensity, the technology has the characteristics of no need of a complex sample pretreatment process, realization of industrial on-line and remote analysis and the like, is widely applied to element analysis of various different occasions, and can also realize scanning imaging analysis of two-dimensional element distribution of a solid sample, however, the existing LIBS technology is generally developed based on a pulse Laser with low repetition frequency (generally 10Hz), that is, even if a single sampling is performed, the frequency of acquiring data is only 10Hz, which results in slow analysis speed, and especially, it takes a long time to complete a scan imaging of a high-resolution two-dimensional element distribution, so that improvement is urgently needed.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides the laser-induced breakdown spectroscopy element analysis system which improves the plasma signal of a sample and has high detection sensitivity.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: a laser-induced breakdown spectroscopy elemental analysis system comprises a sample chamber, wherein a sampling platform, a spectrometer, a laser, a condenser lens, a camera, a scanning device, an integrated blowing device, a lighting device and a computer are arranged in the sample chamber, the laser comprises a main laser and an auxiliary laser which are orthogonally arranged, the main laser vertically bombards the surface of a sample, the auxiliary laser horizontally bombards an ablation plume section excited by the main laser from the side surface to obviously enhance the radiation signal of plasma, the condenser lens is used for focusing the pulse emitted by the laser, the spectrometer is provided with a light emitting diode, a photomultiplier and a detector, the light emitting diode is used for receiving the radiation signal of the plasma and generating an optical signal, the photomultiplier is used for receiving the optical signal generated by the light emitting diode and converting the optical signal into an electrical signal, the detector is used for detecting optical signals and electric signals and transferring the data of the optical signals or the electric signals into the spectrometer, the camera is used for observing the details of a bombarded position of a sample and the appearance change of an excited point before and after the bombardment of the laser, the scanning device is used for scanning the sample, the integrated blowing device supports a user to fill inert gas into a sample chamber so as to avoid the condition that an ultraviolet spectrum is absorbed by air, so that the detection sensitivity of the system is increased, the illuminating device is convenient for the user to observe the appearance change of the sample before and after the bombardment of the laser, the computer comprises a capacitive touch screen and a processor, the processor is provided with an account password management unit, a measurement process management unit, an imaging control unit, an in-bin illumination control unit, a gas control unit, an in-bin pressure monitoring unit and a spectrometer parameter control unit, the device comprises a spectrum data acquisition unit, an element identification unit, a database matching unit and a quantitative modeling tool.
In order to facilitate the adjustment of the sample stage, the invention has the improvement that the sampling platform comprises a manual sample stage and an electric sample stage, the sample stage is freely positioned in a three-axis manner, the adjustment precision of the stroke of the manual sample stage is 0.01mm when the stroke of the manual sample stage is +/-25 mm, and the adjustment precision of the stroke of the electric sample stage is 0.005mm when the stroke of the electric sample stage is +/-25 mm.
In order to improve the safety, the invention is improved in that a cabinet door is arranged on the sample room, a laser protection window, a locking device and a safety interlocking device are arranged on the cabinet door, the safety interlocking device comprises a locking sensor, a signal transmission device and a signal receiving device, the locking sensor is electrically connected with the locking device, the signal receiving device is positioned on a processor of a computer and is connected with the locking sensor through the signal transmission device, a hinged chain is arranged between the cabinet door and the sample room, a locking hole and a locking rod are arranged on the locking device, and the locking rod plays a role of triggering a switch and is connected with the locking sensor.
In order to improve the scanning effect of the sample, the invention improves that the scanning device comprises an actuating connector and a needle-type probe, the needle-type probe is connected with the actuating connector, and the actuating connector controls the needle-type probe to rotate and move up and down, so that three-dimensional scanning is realized.
In order to facilitate the transportation or discharge of gas, the integrated blowing device comprises a gas input channel and a gas output channel, electromagnetic valves are arranged on the gas input channel and the gas output channel, a signal control device is arranged on the electromagnetic valves, the signal control device comprises a signal triggering device and a signal sending device, and the signal sending device is arranged on the processor.
In order to improve the conveying effect of the gas, the invention improves that the gas input channel is provided with a blowing nozzle and is opposite to the sample table.
In order to facilitate data transmission, the spectrometer is improved by a USB interface.
(III) advantageous effects
Compared with the prior art, the invention provides a laser-induced breakdown spectroscopy element analysis system, which has the following beneficial effects:
the invention integrates a sampling sample table, a laser, a scanning device, an integrated blowing device and a lighting device, the devices can be controlled by a control unit integrated on a computer, and compared with a single-pulse LIBS system, the invention supports a user to flexibly adjust different wavelengths and powers to use the laser and adjust parameters such as interval time of double pulses, focus position and the like through a measurement process management unit, thereby being very suitable for LIBS mechanism research and industrial application requirements.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic diagram of a sample cell according to the present invention;
FIG. 3 is a diagram illustrating a computer system according to the present invention;
in the figure: 1. a sample chamber; 2. a sampling platform; 3. a computer; 4. a camera; 5. a laser; 6. a condenser lens; 7. an illumination device; 8. a scanning device; (ii) a 9. An integrated blowing device; 10. a spectrometer; 11. a main laser; 12. a slave laser; 13. a cabinet door; 14. a locking device; 15. a lock hole; 16. an articulated chain;
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-3, the present invention is a laser induced breakdown spectroscopy elemental analysis system, including a sample chamber 1, a sampling platform 2, a spectrometer 10, a laser 5, a condenser lens 6, a camera 4, a scanning device 8, an integrated blowing device 9, an illumination device 7 and a computer 3 are arranged in the sample chamber 1, the laser 5 includes a main laser 11 and a sub-laser 12, and is arranged orthogonally, the main laser 11 bombards the surface of the sample vertically, the sub-laser 12 bombards the ablation plume cross-section excited by the main laser 11 horizontally from the side, so that the radiation signal of the plasma is significantly enhanced, the condenser lens 6 is used for focusing the pulse emitted by the laser 5, the spectrometer 10 is provided with a light emitting diode, a photomultiplier and a detector, the light emitting diode is used for receiving the radiation signal of the plasma and generating an optical signal, the photomultiplier is used for receiving an optical signal generated by a light emitting diode and converting the optical signal into an electric signal, the detector is used for detecting the optical signal and the electric signal and transferring data of the optical signal or the electric signal into the spectrometer 10, the camera 4 is used for observing details of a sample at a bombarded position and changes in the appearance of an excited point before and after being bombarded by the laser 5, the scanning device 8 is used for scanning the sample, the integrated blowing device 9 supports a user to fill inert gas into the sample chamber 1 so as to avoid the condition that an ultraviolet spectrum is absorbed by air, so that the detection sensitivity of the system is increased, the lighting device 7 is convenient for the user to observe the appearance change of the sample before and after being bombarded by the laser, the computer 3 comprises a capacitive touch screen and a processor, and the processor is provided with an account password management unit, a measurement flow management unit and an imaging control unit, the device comprises an illumination control unit in the bin, a gas control unit, a gas pressure monitoring unit in the bin, a spectrometer 10 parameter control unit, a spectrum data acquisition unit, an element identification unit, a database matching unit and a quantitative modeling tool.
In this embodiment, sampling platform 2 includes manual sample platform and electronic sample platform, and is triaxial free positioning sample platform, the stroke of manual sample platform is 25mm adjustment accuracy for 0.01mm, the stroke of electronic sample platform is 25mm, and adjustment accuracy is 0.005mm, and convenience of customers places a plurality of samples and adjusts the sample position.
In this embodiment, a cabinet door 13 is disposed on the sample chamber 1, a laser protection window, a locking device 14 and a safety interlock device are disposed on the cabinet door 13, the safety interlock device includes a locking sensor, a signal transmission device and a signal receiving device, the locking sensor is electrically connected to the locking device 14, the signal receiving device is disposed on a processor of the computer 3 and connected to the locking sensor through the signal transmission device, a hinge chain 16 is disposed between the cabinet door 13 and the sample chamber 1, the locking device 14 is disposed with a locking hole 15 and a locking rod, the locking rod functions as a trigger switch and is connected to the locking sensor, through the safety interlock device, when the cabinet door 13 of the sample chamber 1 is opened, the locking rod contacts the locking sensor to trigger the locking sensor to be started, and an unlocking signal is transmitted to the signal receiving device through the signal transmission device, the processor controls the laser 5 to be in the off state, so that the safety of a user is ensured.
In this embodiment, the scanning device 8 includes an actuating connector and a needle-type probe, the needle-type probe is connected to the actuating connector, and the actuating connector controls the needle-type probe to rotate and move up and down, so as to implement three-dimensional scanning, thereby improving the scanning effect on the sample.
In this embodiment, the integrated blowing device 9 includes a gas input channel and a gas output channel, electromagnetic valves are disposed on the gas input channel and the gas output channel, signal control devices are disposed on the electromagnetic valves, the signal control devices include a signal triggering device and a signal sending device, and the signal sending device is mounted on the processor, thereby facilitating gas transportation or gas discharge.
In this embodiment, the blowing nozzle is disposed on the gas input channel and faces the sample stage, so as to improve the gas conveying effect.
In this embodiment, the spectrometer 10 is provided with a USB interface, thereby facilitating data transmission.
To sum up, the laser induced breakdown spectroscopy elemental analysis system integrates a sampling sample stage, a laser 5, a scanning device 8, an integrated blowing device 9 and a lighting device 7 when in use, the devices can be controlled by a control unit integrated on a computer 3, compared with a single-pulse LIBS system, the laser induced breakdown spectroscopy elemental analysis system supports a user to flexibly select the laser 5 with different wavelengths and powers through a measurement process management unit, and adjusts parameters such as interval time and focal position of double pulses, thereby being very suitable for LIBS mechanism research and industrial application requirements, the invention adopts a technical scheme of orthogonal double laser pulses, a main laser 11 vertically bombards the surface of a sample, an auxiliary laser 12 horizontally bombards the section of a plume excited by the main laser 11 from the side, two beams of laser ablation interact with each other to further excite the expanded plume, so that a radiation signal of plasma is obviously enhanced, the invention receives image data acquired by a camera 4 and a scanning device 8 through an imaging control unit, displays the image data through a capacitive touch screen, registers a login account and sets a login password through an account password management unit, is special for a specially-assigned person, generates a use record, prevents abnormal use of non-workers, supports a user to flexibly select different wavelengths and powers to use a laser 5 through a measurement process management unit, controls an illuminating device 7 through an illumination control unit in a cabin, controls gas transmission work or exhaust work of an integrated blowing unit through a gas control unit, monitors the pressure change in the sample chamber 1 in real time through a pressure monitoring unit in the cabin, discharges gas outwards through a gas output pipeline when the pressure in the sample chamber 1 is too high, conveniently adjusts the detection parameters of a spectrometer 10 according to different types of detection samples through a parameter control unit of the spectrometer 10, therefore, the detection accuracy of the spectrometer 10 is improved, the optical signal and the electrical signal are collected through the spectral data acquisition unit, the element identification unit analyzes the element concentration value through the output wavelength range of the optical signal or the electrical signal, the sample signal intensity with known element concentration is stored through the data matching unit, various comparison models are established by matching with the quantitative modeling tool, the element identification unit obtains the signal intensity of the sample with known element concentration value and the element concentration value or the comparison models established by the quantitative modeling tool, and respective element concentration values in different types of samples are obtained through analysis, so that the accuracy of obtaining the element concentration value in the sample is further improved, the method is suitable for performing element analysis on the samples in various types, and the method is applied to environmental science: soil, particulates, sediments; the material science: metal, slag, plastic, glass; modern agriculture: plants, grains; national defense and military: explosives, biochemical weapons; and (3) identifying the artwork: a pigment; precious stones and metallurgy: noble metals, gem and jade; forensic science: teeth, bones; a semiconductor: silicon wafers, semiconductor materials, elemental analysis in various fields, and the elemental analysis effect of the present invention is improved.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (8)

1. The laser-induced breakdown spectroscopy elemental analysis system is characterized by comprising a sample chamber (1), wherein a sampling platform (2), a spectrometer (10), a laser (5), a condenser lens (6), a camera (4), a scanning device (8), an integrated blowing device (9), an illuminating device (7) and a computer (3) are arranged in the sample chamber (1), the laser (5) comprises a main laser (11) and an auxiliary laser (12) which are arranged orthogonally, the main laser (11) vertically bombards the surface of a sample, the auxiliary laser (12) horizontally bombards an ablation plume section excited by the main laser (11) from the side surface to obviously enhance a radiation signal of plasma, the condenser lens (6) is used for focusing a pulse emitted by the laser (5), and a light emitting diode is arranged on the spectrometer (10), The plasma detection system comprises a light-emitting diode and a detector, wherein the light-emitting diode is used for receiving a radiation signal of plasma and generating an optical signal, the photomultiplier is used for receiving the optical signal generated by the light-emitting diode and converting the optical signal into an electric signal, the detector is used for detecting the optical signal and the electric signal and transferring the data of the optical signal or the electric signal into a spectrometer (10), a camera (4) is used for observing the details of a sample at a bombarded position and the shape change of an excited point before and after bombardment by a laser (5), a scanning device (8) is used for scanning the sample, an integrated blowing device (9) supports a user to fill inert gas into a sample chamber (1) so as to avoid the condition that an ultraviolet spectrum line is absorbed by air, the detection sensitivity of the system is increased, and the illumination device (7) is convenient for the user to observe the shape change of the sample before and after laser, the computer (3) comprises a capacitive touch screen and a processor, wherein an account password management unit, a measurement flow management unit, an imaging control unit, an in-bin lighting control unit, a gas control unit, an in-bin gas pressure monitoring unit, a spectrometer (10) parameter control unit, a spectral data acquisition unit, an element identification unit, a database matching unit and a quantitative modeling tool are arranged on the processor.
2. The laser-induced breakdown spectroscopy elemental analysis system of claim 1, wherein the sampling platform (2) comprises a manual sample stage and an electric sample stage, and the sample stage is freely positioned for three axes, wherein the stroke of the manual sample stage is ± 25mm with an adjustment accuracy of 0.01mm, and the stroke of the electric sample stage is ± 25mm with an adjustment accuracy of 0.005 mm.
3. The laser-induced breakdown spectroscopy elemental analysis system of claim 1, wherein a cabinet door (13) is disposed on the sample chamber (1), a laser protection window, a locking device (14) and a safety interlock device are disposed on the cabinet door (13), the safety interlock device comprises a locking sensor, a signal transmission device and a signal receiving device, the locking sensor is electrically connected to the locking device (14), and the signal receiving device is disposed on a processor of the computer (3) and connected to the locking sensor through the signal transmission device.
4. The laser-induced breakdown spectroscopy elemental analysis system of claim 1, wherein the scanning device (8) comprises an actuating connector and a needle-punch probe, the needle-punch probe is connected with the actuating connector, and the actuating connector controls the needle-punch probe to rotate and move up and down, so that three-dimensional scanning is realized.
5. The laser-induced breakdown spectroscopy elemental analysis system of claim 1, wherein the integrated gas blowing device (9) comprises a gas input channel and a gas output channel, electromagnetic valves are arranged on the gas input channel and the gas output channel, signal control devices are arranged on the electromagnetic valves, the signal control devices comprise signal triggering devices and signal sending devices, and the signal sending devices are installed on the processor.
6. The laser-induced breakdown spectroscopy elemental analysis system of claim 6, wherein the gas input channel is provided with a blowing nozzle and faces the sample stage.
7. The laser-induced breakdown spectroscopy elemental analysis system of claim 3, wherein the cabinet door (13) is connected to the sample chamber (1) by a hinge (16), the locking device (14) is provided with a locking hole (15) and a locking bar, and the locking bar functions as a trigger switch and is connected to the locking sensor.
8. The laser-induced breakdown spectroscopy elemental analysis system of claim 3, wherein the spectrometer (10) is provided with a USB interface.
CN202110616046.6A 2021-06-02 2021-06-02 Laser-induced breakdown spectroscopy element analysis system Pending CN113281257A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN104406942A (en) * 2014-11-17 2015-03-11 浙江大学 Multi-mode laser-induced breakdown spectroscopy device
US20150346103A1 (en) * 2014-05-29 2015-12-03 Bwt Property, Inc. Laser Induced Breakdown Spectroscopy (LIBS) Apparatus and Method for Performing Spectral Imaging of a Sample Surface
CN107064111A (en) * 2017-05-15 2017-08-18 华南理工大学 Gao Zhongying laser lift-off spark induced breakdown spectroscopy elemental analysis system and method
CN109239055A (en) * 2018-10-16 2019-01-18 山西大学 Homocentric multipath chamber enhances the highly sensitive detection device of laser induced breakdown spectroscopy and method

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
US20150346103A1 (en) * 2014-05-29 2015-12-03 Bwt Property, Inc. Laser Induced Breakdown Spectroscopy (LIBS) Apparatus and Method for Performing Spectral Imaging of a Sample Surface
CN104406942A (en) * 2014-11-17 2015-03-11 浙江大学 Multi-mode laser-induced breakdown spectroscopy device
CN107064111A (en) * 2017-05-15 2017-08-18 华南理工大学 Gao Zhongying laser lift-off spark induced breakdown spectroscopy elemental analysis system and method
CN109239055A (en) * 2018-10-16 2019-01-18 山西大学 Homocentric multipath chamber enhances the highly sensitive detection device of laser induced breakdown spectroscopy and method

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