CN115791756A - Laser-induced breakdown spectroscopy device for measuring full spectrum at one time - Google Patents
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Abstract
The invention relates to a laser-induced breakdown spectroscopy device for measuring a full spectrum at one time. The invention relates to a laser-induced breakdown spectroscopy device for measuring a full spectrum at one time. The method comprises the following steps: the device comprises a light generation module, a focusing lens, an optical fiber coupling module, a spectrometer, a galvanometer, a 4f lens group and an area array detector; the vibrating mirror is arranged at the exit slit and used for periodically adjusting the exit angle of the laser-induced breakdown spectrum signal; the front focal plane of the 4f lens group is coincided with the initial position of the galvanometer, the rotating shaft of the galvanometer is on the front focal plane, and the rear focal plane of the 4f lens group is coincided with the plane of the area array detector; the area array detector is arranged opposite to the galvanometer and used for receiving the laser induced spectrum signals of all the wave bands after light splitting at the same time and transmitting the received signals to the computing and processing equipment. The invention has the advantages that the full-spectrum laser-induced breakdown spectroscopy signals are obtained by one-time measurement, and a data source is provided for researching the signal variation trend of the same wavelength in the induction process.
Description
Technical Field
The invention relates to the field of laser detection devices, in particular to the field of laser-induced breakdown spectroscopy devices.
Background
Laser Induced Breakdown Spectroscopy (LIBS) is a technique because it can excite a sample in any state into plasma, and because almost all elements emit characteristic spectral lines after being excited into plasma, we can analyze the composition elements and the element ratios of the sample to be detected according to the distribution and the amplitude of the characteristic spectral lines.
Some existing laser induced breakdown spectroscopy devices include a device for acquiring a spectrum by using a photomultiplier tube or an ICCD, and acquiring a time-resolved spectrum by gating a shutter time, so as to acquire a laser induced breakdown spectrum generated by a sample, but have some disadvantages, such as: there are some devices such as the contrast patent "CN 108152268A-LIBS spectroscopic detection system based on striped tubes" that use striped tubes plus ICCD to achieve time-resolved laser-induced breakdown spectroscopy. However, the cost of the streak tube and the ICCD is very expensive, which is not favorable for industrial production.
There are also devices that use a scanning galvanometer to direct light of different wavelengths that are separated by a grating onto a photomultiplier tube so that the different temporal intensities of the photomultiplier tube correspond to the intensities of the different wavelengths. However, the data obtained in this way is intensity information of different wavelengths in different time periods, and the change state of the amplitude and frequency of each excitation light in the excitation process cannot be collected, so that data support cannot be provided for further analysis of the internal elements of the sample.
Disclosure of Invention
Based on this, the present invention provides a laser induced breakdown spectroscopy apparatus for measuring a full spectrum at one time, which has the advantages of simple structure, low industrial cost, high sensitivity, and complete and continuous obtained excitation light signals.
The invention provides a laser-induced breakdown spectroscopy device for measuring a full spectrum at one time, which comprises:
the device comprises a laser generation module, a focusing lens, an optical fiber coupling module, a spectrometer, a galvanometer, a 4f lens group and an area array detector;
the laser generating module is used for generating single-pulse laser;
the focusing lens is used for focusing the laser generated by the laser generating module on the sample to be detected;
the optical fiber coupling module comprises a receiving probe, an optical fiber and a transmitting probe, wherein the receiving probe is used for collecting laser-induced breakdown spectrum signals emitted by a sample excitation surface, the optical fiber is used for transmitting the laser-induced breakdown spectrum signals to the transmitting probe, and the transmitting probe is used for emitting the laser-induced breakdown spectrum signals into the spectrometer through an incidence slit;
the spectrometer comprises a collimating lens, a grating and a focusing lens, wherein the collimating lens is used for collimating the laser-induced breakdown spectrum signal, the grating is used for splitting the collimated laser-induced breakdown spectrum signal, the split laser-induced breakdown spectrum signal is separated in a spatial domain at different angles according to the light wave length, and the focusing lens is used for focusing the laser-induced breakdown spectrum signal split by the grating to an emergent slit of the spectrometer;
the vibrating mirror is arranged at the emergent slit and used for periodically adjusting the emergent angle of the laser-induced breakdown spectrum signal;
the front focal plane of the 4f lens group is superposed with the initial position of the galvanometer, the rotating shaft of the galvanometer is arranged on the front focal plane, and the rear focal plane of the 4f lens group is superposed with the plane of the area array detector;
the area array detector is arranged opposite to the vibrating mirror and is used for simultaneously receiving the laser-induced spectrum signals of all the wave bands after light splitting and transmitting the received signals to the computing and processing equipment.
Furthermore, the area array detector is an area array CCD, and the whole area array CCD chip is rectangular and is composed of a plurality of pixel points.
Furthermore, 2048 pixel points are arranged in the horizontal direction of the area array CCD chip, 512 pixel points are arranged in the vertical direction of the area array CCD chip, and the size of each pixel point is 13.5 microns multiplied by 13.5 microns.
Furthermore, the laser-induced breakdown spectroscopy device for measuring the full spectrum at one time further comprises a time delay control module, wherein one end of the time delay control module is connected with the laser generation module, and the other end of the time delay control module is connected with the vibrating mirror and the area array detector, and the time delay control module is used for delaying the set time after receiving the laser output zero signal and controlling the area array detector to receive the laser-induced spectroscopy signal.
Further, the laser light source used by the laser generation module has a wavelength of 1535nm or 1570nm.
Further, the speed of the galvanometer scanning is 10000 points per second.
The invention provides a laser-induced breakdown spectroscopy device for measuring a full spectrum at one time, which is characterized in that the size of a pixel point of an area array CCD chip is planned to be matched with the size of a light spot of a laser-induced breakdown spectroscopy signal, and in combination with galvanometer scanning, different pixel points on the same line of the area array CCD chip correspond to laser-induced breakdown spectroscopy signals of exciting light with different wavelengths at the same time, so that the full-spectrum laser-induced breakdown spectroscopy signal is obtained by one-time measurement, and in the detection process corresponding to the laser-induced breakdown spectroscopy signals in the same row, the exciting light signal with the same wavelength provides a data source for the signal change trend of the same wavelength in the research induction process along with the change of the induction time, and a 1535nm or 1570nm laser light source is used for avoiding the exciting light from directly irradiating human eyes in the detection process to cause damage to the human eyes without increasing, so that an additional safety protection device is reduced.
For a better understanding and practice, the invention is described in detail below with reference to the accompanying drawings.
Drawings
FIG. 1 is a schematic diagram of an optical path of a single-measurement full-spectrum laser-induced breakdown spectroscopy apparatus according to the present invention;
FIG. 2 is a schematic diagram of an exemplary single row area array detector according to the present invention;
FIG. 3 is a schematic structural diagram of an area array detector of a one-time full-spectrum laser-induced breakdown spectroscopy apparatus according to the present invention;
FIG. 4 is a spectrum of a laser induced breakdown spectroscopy signal measured at a time delay of 0.5 μ s according to the present invention;
FIG. 5 is a spectrum of a laser induced breakdown spectroscopy signal measured at a time delay of 2 μ s according to the present invention.
Reference numerals: 10: a laser generating module; 20: a focusing lens; 31: receiving a probe; 32: an optical fiber; 33: a transmitting probe; 41: a collimating mirror; 42: a grating; 43: a focusing mirror; 50: a galvanometer; 60: a 4f lens group; 70: an area array detector; 71: and (6) pixel points.
Detailed Description
The Laser Induced Breakdown Spectroscopy (LIBS) uses ultrashort pulse laser to focus the surface of a sample to be detected to form plasma, the plasma absorbs energy to emit characteristic spectral lines, and the characteristic spectral lines are used for analyzing and determining the element composition and content ratio of the sample. Since the characteristic spectral lines of different elements are different, the obtained characteristic spectral lines are separated on a spatial domain according to different wavelengths by using a grating structure. And obtaining characteristic spectral lines with different wavelengths, combining the characteristic spectral lines with different wavelengths, and comparing the relative intensities of signals to obtain all element types and component ratios thereof in the sample to be detected at one time.
However, most of the prior art uses a scanning galvanometer to irradiate laser points with different wavelengths after being separated by a grating on a photomultiplier tube at different times, so that the signal intensities obtained by the photomultiplier tube at different times correspond to the intensities with different wavelengths. The method can be explained as that if the time interval of the acquired data is T, and the wavelength is lambda 1, lambda 2 and lambda 3, then the acquired first data is an induced breakdown spectrum signal of the exciting light with the wavelength lambda 1 at the time 0, the acquired second data is an induced breakdown spectrum signal of the exciting light with the wavelength lambda 2 at the time T, that is, the acquired intensity signals with different wavelengths at the same time are not acquired, but optical signals with different wavelengths at different times, and the time consumed in the process of generating the characteristic spectral line by laser induction is much longer than the time of acquiring data once.
Therefore, the prior device has at least the following defects:
1. the laser-induced breakdown spectra of signals with different wavelengths at the same time cannot be obtained.
2. Continuous signals of the same wavelength signal cannot be obtained.
With reference to fig. 1, aiming at the defects of the existing device, the invention provides a laser-induced breakdown spectroscopy device for measuring a full spectrum at one time, which comprises:
the system comprises a laser generation module 10, a focusing lens 20, an optical fiber 32 coupling module, a spectrometer, a galvanometer 50, a 4f lens group 60 and an area array detector 70;
the laser generating module 10 is used for generating laser.
The focusing lens 20 is arranged between the laser generating module 10 and the sample, and the focusing lens 20 focuses the laser on the sample to be detected; the focusing lens 20 can further focus the laser light to a focal point, the LIBS focuses a beam of pulsed laser light on the surface of the sample, and when the laser irradiance exceeds the breakdown threshold of the sample, the particles, molecules and atoms in the laser ablation area can undergo multi-photon ionization to generate initial free electrons. The initial free electrons continue to absorb photons and accelerate, collide with atoms and ionize to generate new free electrons, which repeat the behavior of the initial free electrons to ionize the atoms continuously, so that avalanche effect occurs to generate laser-induced plasma, and the focusing lens 20 is used to increase the irradiance at the focal position to several to tens of GW/cm 2 So that the initial temperature of the plasma is 10 DEG 4 ～10 5 And between K, plasma is quickly formed on the surface of the sample to be detected.
The optical fiber 32 coupling module comprises a receiving probe 31, an optical fiber 32 and a transmitting probe 33, wherein the receiving probe 31 is used for collecting laser-induced breakdown spectrum signals emitted from the excitation surface of the sample, the optical fiber 32 is used for transmitting the laser-induced breakdown spectrum signals, the transmitting probe 33 is arranged at an entrance slit of the spectrometer, and the laser-induced breakdown spectrum signals enter the spectrometer module through the entrance slit.
The optical signal is disturbed by atmospheric molecules when propagating in the air, so that on one hand, the optical signal generates large loss, and on the other hand, the optical signal is scattered in all directions. The optical fiber 32 coupling module is used for communication of optical signals, the receiving probe 31 is used for receiving the signals, the optical fiber 32 is used for transmitting the signals, and the transmitting probe 33 is used for transmitting the optical signals to an incident slit of the spectrometer. The excitation light enters the receiving probe 31 and is transmitted to the exit slit through the optical fiber 32, and the excitation light is mixed light with different wavelengths.
The spectrometer comprises a collimating lens 41, a grating 42 and a focusing lens 43, wherein the collimating lens 41 is used for collimating the laser-induced spectrum signal, the grating 42 is used for splitting the light of different wave bands of the collimated laser-induced spectrum signal, the focusing lens 43 is used for focusing the laser-induced spectrum signal split by the grating 42 to an emergent slit, and the emergent angles of different light waves in the laser-induced spectrum signal split by the grating 42 are related to the wavelength of the light waves, so that the laser-induced spectrum signal is separated.
The focus of the collimating lens 41 coincides with the entrance slit, all the light emitted from the entrance slit becomes parallel light after passing through the collimating lens 41, the parallel light enters the grating 42 to realize spatial separation of the light with different wavelengths, and finally the separated light is converged through the focusing lens 43, so that the separated light can pass through the exit slit.
The surface of the galvanometer 50 is a reflector, the galvanometer 50 is arranged at the exit slit, the rotating shaft is superposed with the exit slit, and the galvanometer 50 is used for periodically adjusting the exit angle of the laser-induced spectrum signal. The rotation axis of the galvanometer 50 coincides with the exit slit, and when the incident light direction is not changed, the galvanometer 50 is rotated, the normal direction changes, which is equivalent to the incident angle, and according to the law of reflection, the incident angle is equal to the exit angle, the angle of the exit light changes, and the use frequency of the galvanometer 50 is 10000HZ.
The rotating shaft of the galvanometer 50 is arranged on the front focal plane of the 4f lens group 60 and is superposed with the focus of the front focal plane, and the rear focal plane of the 4f lens group 60 is superposed with the plane of the area array detector 70; the spectrum signal passes through the 4f lens group 60, the size of the light spot is reduced, and the light spots with different wavelengths are focused to the photosensitive units on the same line of the area array CCD.
The area array detector 70 is arranged opposite to the galvanometer 50, and the area array detector 70 receives the laser induced spectrum signal and transmits the signal to the computer. The photosensitive units of the CCD perform photoelectric conversion within the illumination time, and the accumulated charge amount of each unit is different along with the illumination intensity. During the period of no illumination, the signals of all the photosensitive units are read out in sequence. When the signals are read out, all the signals in each row in the area array move to the next row, and the signals at the lowest row enter a horizontal shift register after being moved out of the light sensitive area. At this time, the signals in the horizontal shift register are sequentially shifted out to the computing processing equipment, and continuous laser induced spectrum signals are obtained.
In another preferred embodiment, referring to fig. 3 in conjunction with fig. 2, the area array detector 70 is an area array CCD, and the whole area array CCD chip is rectangular and is composed of a plurality of pixels 71. The induced breakdown spectrum signal split by the grating 42 can split light with different wavelengths on the same plane, the light with different wavelengths has different emergence angles, a group of parallel light is obtained after passing through the collimating mirror 41, in the same group of experiments, the composition of a sample is unchanged, a rectangular area array CCD chip consisting of a plurality of pixel points 71 is used for collecting spectrum signals, so that the data of the same column corresponds to the data with the same wavelength, and the positions of the starting point and the ending point of the data of each line are always fixed. And the later data generation is facilitated.
In another embodiment, 2048 pixel points 71 are horizontally arranged on the area array CCD chip, 512 pixel points 71 are vertically arranged, the size of each pixel point 71 is 13.5 μm × 13.5 μm, and the resolution affecting the system depends on the 4f lens group 60 system, the spectrometer resolution, the total optical power and the CCD pixel size. The maximum resolution that can be achieved ultimately depends on the pixel values of the area array ccd. The 4f lens group 60 system reduces the light spot at the scanning galvanometer 50 by 20 times and images on the area array detector 70. The system is designed to have a laser line spot size of at most 3 pixels full width at half maximum, with an estimated maximum spectral resolution of about 0.5nm calculated in conjunction with the spectrometer resolution.
Fig. 5 is a graph illustrating the laser induced breakdown spectroscopy signal measured with a time delay of 0.5 μ s according to the present invention, fig. 4 is a graph illustrating the laser induced breakdown spectroscopy signal measured with a time delay of 2 μ s according to the present invention, and fig. 5 is a graph illustrating the laser induced breakdown spectroscopy signal measured with a time delay of 2 μ s according to the present invention. In this embodiment, the apparatus for one-time measurement of a full spectrum laser induced breakdown spectroscopy further comprises a time delay control module, one end of the time delay control module is connected to the laser generation module 10, and the other end is connected to the galvanometer 50 and the area array detector 70. The time delay control module is used for controlling the galvanometer 50 to start deflecting and controlling the area array detector 70 to start receiving laser-induced spectrum signals after receiving the laser output zero point signals and delaying for a set time, and therefore the time delay module is used for delaying the time of data acquisition and acquiring spectrum signals with low noise because the continuous radiation can generate strong background radiation signals to cause the acquired spectrum signals.
In another embodiment, the laser light source used by the laser generation module 10 has a wavelength of 1535nm or 1570nm. The use of laser has certain risks, the conventional laser light source is 1310nm wavelength light which is dangerous for human eyes, so additional safety lock devices such as spectrum detection interlock and room light interlock are often used to ensure the use safety, and the use of 1535nm or 1570nm long wavelength light source can avoid the addition of additional devices.
The specific use process of the device is as follows:
placing a sample to be detected, starting a laser generation module 10 to generate laser, focusing the laser on the surface of the sample to be detected through a focusing lens 20, ionizing the surface of the sample to be detected to form plasma, and exciting an excitation induced breakdown spectroscopy (LIBS), wherein LIBS signals on the surface of the sample are received by a receiving probe 31 of an optical fiber 32 coupling module, the LIBS signals are transmitted to a transmitting probe 33 through an optical fiber 32, the transmitting probe 33 is arranged at an entrance slit of a spectrometer, all LIBS signals enter the spectrometer from the entrance slit, and are changed into parallel light through a collimating mirror 41, after diffraction action of a grating 42, optical signals with different wavelengths in the LIBS signals are spatially separated, then the separated optical signals with different wavelengths are focused to an exit slit through a focusing mirror 43, the vibration mirror 50 at the exit slit reflects the optical signals, the reflected optical signals pass through a 4f lens group 60, the spot size of the optical signals is reduced to 1/20 of the original optical signals, finally the optical signals with different wavelengths are received by different photosensitive units in the same row of an area array detector 70, and after a time period, the vibration mirror 50 deflects a preset angle to enable the optical signals to be received by the next row of the area array detector 70, and all the optical signals with the same wavelength of the next row of the data of the LIBS detector 70 are received by the same row, and all the data of the next row of the data of the light detector, and the data of the light detector 70 are calculated sequentially received by the light signals, and the data of the light signals with the data of the light detector 70, and the light detector. So that signal data of the same wavelength can be extracted separately from all LIBS signal data by setting an initial point, and fixing a step size.
Through the data obtained by the device, LIBS signals generated by a sample to be tested in the whole excitation process can be screened, a group of LIBS spectrograms with different wavelengths and the minimum noise are selected to analyze the composition element types and the element proportions of the sample to be tested, and a more accurate experimental result is obtained.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that numerous changes and modifications can be made by those skilled in the art without departing from the inventive concepts and it is intended that such changes and modifications be covered by the present invention.
Claims (6)
1. A laser-induced breakdown spectroscopy device for measuring a full spectrum at one time is used for detecting the laser-induced breakdown spectrum of a sample to be detected, and is characterized by comprising:
the device comprises a laser generation module, a focusing lens, an optical fiber coupling module, a spectrometer, a galvanometer, a 4f lens group and an area array detector;
the laser generating module is used for generating single-pulse laser;
the focusing lens is used for focusing the laser generated by the laser generating module on the sample to be detected;
the optical fiber coupling module comprises a receiving probe, an optical fiber and a transmitting probe, wherein the receiving probe is used for collecting laser-induced breakdown spectrum signals emitted by a sample excitation surface, the optical fiber is used for transmitting the laser-induced breakdown spectrum signals to the transmitting probe, and the transmitting probe is used for emitting the laser-induced breakdown spectrum signals into the spectrometer through an entrance slit;
the spectrometer comprises a collimating lens, a grating and a focusing lens, wherein the collimating lens is used for collimating the laser-induced breakdown spectrum signal, the grating is used for splitting the collimated laser-induced breakdown spectrum signal, the split laser-induced breakdown spectrum signal is separated in a spatial domain at different angles according to the light wave length, and the focusing lens is used for focusing the laser-induced breakdown spectrum signal split by the grating to an emergent slit of the spectrometer;
the vibrating mirror is arranged at the emergent slit and used for periodically adjusting the emergent angle of the laser-induced breakdown spectrum signal;
the front focal plane of the 4f lens group is coincided with the initial position of the galvanometer, the rotating shaft of the galvanometer is positioned on the front focal plane, and the rear focal plane of the 4f lens group is coincided with the plane of the area array detector;
the area array detector is arranged opposite to the vibrating mirror and is used for simultaneously receiving the laser-induced spectrum signals of all the wave bands after light splitting and transmitting the received signals to the computing and processing equipment.
2. The apparatus according to claim 1, wherein the apparatus is characterized in that:
the area array detector is an area array CCD, and the whole area array CCD chip is rectangular and is composed of a plurality of pixel points.
3. The apparatus for laser induced breakdown spectroscopy for one-time measurement of a full spectrum according to claim 2, wherein:
2048 pixel points are arranged in the horizontal direction of the area array CCD chip, 512 pixel points are arranged in the vertical direction of the area array CCD chip, and the size of each pixel point is 13.5 micrometers multiplied by 13.5 micrometers.
4. The apparatus according to claim 3, further comprising:
and one end of the time delay control module is connected with the laser generation module, the other end of the time delay control module is connected with the vibrating mirror and the area array detector, and the time delay control module is used for delaying the set time after receiving the laser output zero point signal and controlling the area array detector to receive the laser induced spectrum signal.
5. The device for laser-induced breakdown spectroscopy for one-time measurement of a full spectrum according to claim 4, wherein:
the wavelength of the laser light source used by the laser generation module is 1535nm or 1570nm.
6. The apparatus according to claim 5, wherein the apparatus is capable of measuring a full spectrum of laser induced breakdown spectroscopy at a time, and comprises:
the speed of galvanometer scanning is 10000 points per second.
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