CN109358036B - Laser-induced breakdown spectroscopy signal error correction system and method - Google Patents

Laser-induced breakdown spectroscopy signal error correction system and method Download PDF

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CN109358036B
CN109358036B CN201811565338.6A CN201811565338A CN109358036B CN 109358036 B CN109358036 B CN 109358036B CN 201811565338 A CN201811565338 A CN 201811565338A CN 109358036 B CN109358036 B CN 109358036B
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laser
light source
source
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spectrometer
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CN109358036A (en
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赵天卓
钟奇秀
樊仲维
连富强
林蔚然
刘洋
肖红
李欣
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Academy of Opto Electronics of CAS
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Abstract

The present disclosure discloses a laser-induced breakdown spectroscopy signal error correction system and method, the system comprising: the device comprises a laser-induced light source, one or more reference sources, a focusing lens, a first laser-induced light source spectroscope, a second laser-induced light source spectroscope, one or more reference source spectroscopes, a total reflection mirror, a collecting lens, a fiber-optic probe, a spectrometer, a computer and an n-dimensional adjustable sample table. The invention can compensate the influence of the surface property of the sample on the laser-induced breakdown spectrum, and can be suitable for all types of spectrometers.

Description

Laser-induced breakdown spectroscopy signal error correction system and method
Technical Field
The invention belongs to the field of laser-induced breakdown spectroscopy detection, and particularly relates to a system and a method for correcting laser-induced breakdown spectroscopy signal errors, aiming at compensating spectral wavelength and spectral intensity drift generated in an experimental process and the influence of sample surface properties on laser-induced breakdown spectroscopy, so that the precision and the stability of LIBS quantitative analysis are improved.
Background
The Laser Induced Breakdown Spectroscopy (LIBS) technology is a quantitative analysis technology based on plasma emission spectrum generated by interaction of Laser and materials, and the method can realize quantitative analysis of the element component proportion by consuming a few micrograms of detected materials during measurement, and belongs to a nondestructive detection technology. The LIBS technique has the following advantages: (1) and (4) carrying out nondestructive testing. Only a few micrograms of samples are needed in the detection process, and almost no consumption is caused to the detected samples; (2) and (4) detecting quickly. The whole detection process only needs several seconds, and has real-time performance and rapidity; (3) and (3) simultaneously detecting multiple elements. The simultaneous quantitative analysis of several to all elements can be realized; (4) no pretreatment of the sample is required. The requirements on the size, shape and physical properties of the sample are not strict; (5) and (4) measuring at a long distance. The device can be used for remote analysis in severe environments such as dangers (biological weapons, explosives and the like), high temperature, radiation and the like, and the detection distance reaches tens of meters.
However, compared with the material component analysis methods such as inductively coupled plasma atomic emission spectrometry (ICP-AES) and photoelectric direct-reading spectrometry, the method using laser-induced excitation is less stable, so the LIBS detection mode is affected by many factors, which also results in the lower repeatability and accuracy of the current LIBS detection than the former. Since a sample detected by the LIBS often contains a plurality of element components, the peak group in the plasma spectrum is very dense, and the wavelength shift of the plasma spectrum of only 0.1nm is likely to cause spurious peak finding, and the peak of some elements is misjudged as that of other elements. The strong spectral shift of the plasma spectrum is very unfavorable for the quantitative analysis of the element concentration in the sample.
Most LIBS detection devices only correct the spectrometer before measurement, however, in the measurement process, factors such as temperature change and vibration can cause strong drift of the wavelength and spectrum of the spectrometer, so that detection precision is affected. Temperature changes directly cause the dispersion coefficient (dn/d lambda) of a dispersion element in the spectrometer to change, and structural materials of the spectral imaging system can be expanded or deformed, so that surface shape changes and rigid body displacement of the system mirror surface are caused, and spectral line drift is generated on the imaging surface. The influence of rigid displacement of the imaging element caused by vibration on the detection precision is more serious, for example, an echelle grating spectrometer is taken as an example, wherein the radius of a central wavelength light spot can be widened by 0.07mm and the position of the central wavelength light spot can be shifted by 12.4mm when the incident angle of the echelle grating deviates from the theoretical incident angle by one degree.
In addition, in addition to the strong drift of the wavelength and spectrum of the spectrometer itself, the refractive index, curvature, etc. of the ablation surface will change with the increase of the number of pulses because the laser continuously ablates the surface of the sample during the LIBS detection process, and thus the collection efficiency of plasma signals of each wavelength by the spectrometer will also change, resulting in the decrease of the consistency among pulses of the measured spectrum.
Generally, to increase the laser power density at the ablation point to increase the excitation intensity of the plasma, the laser spot needs to be focused to a small size, so that LIBS detection can only sample a very small area when the sample position is fixed. In order to reduce the influence of the uneven distribution of sample components on the LIBS detection precision, multi-point sampling is often required, but the influence caused by the uneven distribution of sample surface properties (flatness, smoothness and the like) is also required to be considered.
Disclosure of Invention
Aiming at the defects or the improvement requirements of the prior art, the invention provides a system and a method for correcting the error of a laser-induced breakdown spectroscopy signal, which continuously collect the spectra of a plurality of reference signals reflected from the surface of a sample in the LIBS detection process, read out the wavelength and the spectral intensity of each main peak by using a computer, combine the reference wavelength and the spectral intensity measured before the detection starts, and respectively obtain the relation curve satisfied by the actually measured wavelength, the actually measured spectral intensity drift and the reference wavelength by polynomial fitting, thereby compensating the wavelength and the spectral intensity drift in the plasma spectrogram of the measured sample.
According to an aspect of the present invention, a laser-induced breakdown spectroscopy signal error correction system is provided, the system comprising: laser induction light source, one or more reference sources, focusing lens, first laser induction light source spectroscope, second laser induction light source spectroscope, one or more reference source spectroscopes, total reflection mirror, collecting lens, fiber optic probe, spectrum appearance, computer, n dimension adjustable sample platform, wherein:
the laser-induced light source and the one or more reference sources are placed in parallel, the laser-induced light source is used for emitting induced laser, and the reference source is used for emitting a reference signal;
the first laser-induced light source spectroscope and the one or more reference source spectroscopes are respectively arranged on one side of the light path of the laser-induced light source and one or more reference sources in parallel and used for reflecting or transmitting light rays emitted by the laser-induced light source and the reference source;
the focusing lens is arranged between the laser-induced light source and the first laser-induced light source spectroscope and is used for focusing laser emitted by the laser-induced light source;
the second laser-induced light source spectroscope is arranged behind the light path of the first laser-induced light source spectroscope and used for reflecting or transmitting the arriving light;
the measured sample is placed on the adjustable sample stage, and the adjustable sample stage is placed behind the optical path of the second laser-induced light source spectroscope;
the collecting lens and the total reflection mirror are sequentially arranged on one side of the second laser-induced light source spectroscope;
the optical fiber probe is arranged on an output light path of the total reflection mirror and is positioned on an image surface of a laser ablation point on the surface of the sample imaged by the collecting lens;
the spectrometer is connected with the optical fiber probe, and the computer is connected with the spectrometer;
the laser-induced breakdown spectroscopy signal error correction system enables a laser-induced light source and a reference source to coaxially enter the surface of a sample after combination, and takes a signal reflected from the surface of the sample as a reference, so that wavelength and spectrum intensity drift caused by using factors or change of the refractive index/curvature of the surface of the sample can be compensated.
Optionally, the reference source is a single-wavelength reference source or a multi-wavelength reference source, when the reference source is a single-wavelength reference source, the number of the reference sources is two or more, and the reference source spectroscope located on the side of the reference source far away from the laser-induced light source is a total reflection mirror; when the reference source is a multi-wavelength reference source, the number of the reference sources is one, and the reference source spectroscope positioned on one side of the reference source is a total reflection mirror.
Optionally, the laser-induced light source is a semiconductor laser, a solid-state or a gas laser.
Optionally, the reference source is a vapor discharge light source or a laser.
Optionally, the n-dimensional adjustable sample stage is movable in n directions.
Optionally, the n-dimensional adjustable sample stage is a translation stage or a rotation stage.
Optionally, the spectrometer is a linear array spectrometer, an area array spectrometer or a direct-reading spectrometer.
According to another aspect of the present invention, a method for correcting an error of a laser-induced breakdown spectroscopy signal is provided, the method comprising the steps of:
step S1, starting a reference source and a spectrometer, wherein a reference signal emitted by the reference source reaches the surface of the sample, is reflected and then is received by the fiber probe and the spectrometer in sequence to obtain reference data, and the reference data comprises a reference wavelength lambda ' of the reference signal and a spectrum intensity average value I ' of the reference signal in a period of time 'λ；
Step S2, laser pulses emitted by the laser-induced light source reach the surface of the sample, are reflected and then are received by the fiber probe and the spectrometer in sequence to form a plasma spectrum;
step S3, after the plasma signal excited by each pulse is sufficiently attenuated, acquiring a beam combination reference signal actual measurement spectrogram by using a spectrometer;
and step S4, correcting the plasma spectrum according to the actually measured spectrogram and the reference data of the beam combination reference signal.
Optionally, the step S1 includes the following steps:
starting the reference source and the spectrometer;
combining the reference signals sent by the reference source at the first laser-induced light source spectroscope to form combined beam reference signals;
the beam combination reference signal reaching the surface of the sample and reflected by the beam combination reference signal passes through the second laser-induced light source spectroscope and the collecting lens and is sequentially received by the fiber-optic probe and the spectrometer to obtain reference data, wherein the reference data comprises a reference wavelength lambda ' of the reference signal and a spectrum intensity mean value I ' of the reference signal in a period of time 'λ。
Optionally, the step S4 includes the following steps:
step S41, determining the measured wavelength lambda of each reference signal in the measured spectrogram of the reference wavelength lambda' and the ith opening and closing beam reference signaliA variable coefficient of the relation curve, which corresponds to the actually measured spectrogram of the ith opening and closing beam reference signalMeasured wavelength lambda in the plasma spectrogramiePerforming drift compensation correction;
step S42, obtaining the actually measured spectrum intensity I of each reference signal in the actually measured spectrogram of the combined beam reference signaliλAnd the spectral intensity mean value I'λThe difference I 'between'ΔDetermining the difference value I'ΔAnd (3) carrying out drift compensation correction on the actually measured spectrum intensity corresponding to each wavelength in the plasma spectrogram according to the relation curve coefficient along with the change of the reference wavelength lambda'.
The method can overcome the problem that the existing spectrometer is calibrated only before use and cannot compensate strong drift of wavelength and spectrum caused by working temperature change or vibration and the like in the using process. In addition, the invention creatively enables the laser source and other reference sources to coaxially enter the surface of the sample to be measured after the laser source and the other reference sources are combined, and the signal reflected from the surface of the sample is used as a reference, so that the influence of the change of the refractive index, the curvature and the like of the surface of the sample caused by laser ablation on the collection efficiency of plasma signals of each wavelength can be compensated aiming at the same sample point. In order to reduce the influence of the uneven element concentration distribution in the sample on the LIBS detection, multi-point sampling is often needed, and the spectrometer drift real-time compensation method provided by the invention can compensate the influence of the surface property of the sample on the laser-induced breakdown spectrum. In addition, the drift compensation method belongs to a spectral image processing method, does not relate to the working principle of a spectrometer, and therefore can be applied to all types of spectrometers.
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FIG. 1 is a schematic diagram of a laser induced breakdown spectroscopy signal error correction system according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of a laser induced breakdown spectroscopy signal error correction system according to another embodiment of the present invention, wherein a multi-wavelength reference source is used as a reference for wavelength and spectral intensity drift compensation;
FIG. 3 is a flowchart of a method for correcting an error in a laser induced breakdown spectroscopy signal according to an embodiment of the invention.
Detailed Description
Hereinafter, exemplary embodiments of the present disclosure will be described in detail with reference to the accompanying drawings so that those skilled in the art can easily implement them. Also, for the sake of clarity, parts not relevant to the description of the exemplary embodiments are omitted in the drawings.
In the present disclosure, it is to be understood that terms such as "including" or "having," etc., are intended to indicate the presence of the disclosed features, numbers, steps, behaviors, components, parts, or combinations thereof, and are not intended to preclude the possibility that one or more other features, numbers, steps, behaviors, components, parts, or combinations thereof may be present or added.
It should be further noted that the embodiments and features of the embodiments in the present disclosure may be combined with each other without conflict. The present disclosure will be described in detail below with reference to the accompanying drawings in conjunction with embodiments.
To achieve the above object, according to an aspect of the present invention, there is provided a laser induced breakdown spectroscopy signal error correction system, the system comprising: laser induction light source, one or more reference sources, focusing lens, first laser induction light source spectroscope, second laser induction light source spectroscope, one or more reference source spectroscopes, total reflection mirror, collecting lens, fiber optic probe, spectrum appearance, computer, n dimension adjustable sample platform, wherein:
the laser-induced light source and the one or more reference sources are placed in parallel, the laser-induced light source is used for emitting induced laser, and the reference source is used for emitting a reference signal;
the first laser-induced light source spectroscope and the one or more reference source spectroscopes are respectively arranged on one side of the light path of the laser-induced light source and one or more reference sources in parallel and used for reflecting or transmitting light rays emitted by the laser-induced light source and the reference source;
the focusing lens is arranged between the laser-induced light source and the first laser-induced light source spectroscope and is used for focusing laser emitted by the laser-induced light source;
the second laser-induced light source spectroscope is arranged behind the light path of the first laser-induced light source spectroscope and used for reflecting or transmitting the arriving light;
the measured sample is placed on the adjustable sample stage, and the adjustable sample stage is placed behind the optical path of the second laser-induced light source spectroscope;
the collecting lens and the total reflection mirror are sequentially arranged on one side of the second laser-induced light source spectroscope;
the optical fiber probe is arranged on an output light path of the total reflection mirror and is positioned on an image surface of a laser ablation point on the surface of the sample imaged by the collecting lens;
the spectrometer is connected with the optical fiber probe, and the computer is connected with the spectrometer;
the laser-induced breakdown spectroscopy signal error correction system enables a laser-induced light source and a reference source to coaxially enter the surface of a sample after combination, and takes a signal reflected from the surface of the sample as a reference, so that wavelength and spectrum intensity drift caused by using factors or change of the refractive index/curvature of the surface of the sample can be compensated.
In an embodiment of the present invention, the reference source is a reference source with a single wavelength, the number of the reference sources is two or more, and the reference source spectroscope located on the side of the reference source far away from the laser-induced light source is a total reflection mirror. Namely, the system includes: laser induction light source, two or more reference sources, focusing lens, first laser induction light source spectroscope, second laser induction light source spectroscope, one or more reference source spectroscopes, first total reflection mirror, collecting lens, second total reflection mirror, fiber optic probe, spectrum appearance, computer, n dimension adjustable sample platform, wherein:
the laser induction light source and the two or more reference sources are placed in parallel, the laser induction light source is used for emitting induction laser, and the reference sources are used for emitting reference signals;
the first laser-induced light source spectroscope, the one or more reference source spectroscopes and the first total reflection mirror are respectively arranged on one side of the light path of the laser-induced light source and one side of the light path of the two or more reference sources in parallel and used for reflecting or transmitting light rays emitted by the laser-induced light source and the reference source;
the focusing lens is arranged between the laser-induced light source and the first laser-induced light source spectroscope and is used for focusing laser emitted by the laser-induced light source;
the second laser-induced light source spectroscope is arranged behind the light path of the first laser-induced light source spectroscope and used for reflecting or transmitting the arriving light;
the measured sample is placed on the adjustable sample stage, and the adjustable sample stage is placed behind the optical path of the second laser-induced light source spectroscope;
the collecting lens and the second total reflection mirror are sequentially arranged on one side of the second laser-induced light source spectroscope;
the optical fiber probe is arranged on an output light path of the second total reflection mirror and is positioned at an image surface of a laser ablation point on the surface of the sample imaged by the collecting lens;
the spectrometer is connected with the optical fiber probe, and the computer is connected with the spectrometer;
the laser-induced breakdown spectroscopy signal error correction system enables a laser-induced light source and a reference source to coaxially enter the surface of a sample after combination, and takes a signal reflected from the surface of the sample as a reference, so that wavelength and spectrum intensity drift caused by using factors or change of the refractive index/curvature of the surface of the sample can be compensated.
In an embodiment of the present invention, there are three reference sources, and two reference source beam splitters, as shown in fig. 1, in this embodiment, the system includes: the system comprises a laser-induced light source 101, a first reference source 102, a second reference source 103, a third reference source 104, a focusing lens 105, a first laser-induced light source spectroscope 106, a first reference source spectroscope 107, a second reference source spectroscope 108, a first total reflection mirror 109, a second laser-induced light source spectroscope 110, a collecting lens 111, a second total reflection mirror 112, a fiber-optic probe 113, a spectrometer 114, a computer 115 and an n-dimensional adjustable sample stage 116, wherein:
the laser induction light source 101, the first reference source 102, the second reference source 103 and the third reference source 104 are arranged in parallel, the laser induction light source 101 is used for emitting induction laser, and the first reference source 102, the second reference source 103 and the third reference source 104 are used for emitting reference signals;
the first laser-induced light source spectroscope 106, the first reference source spectroscope 107, the second reference source spectroscope 108 and the first total reflection mirror 109 are arranged on one side of the optical paths of the laser-induced light source 101, the first reference source 102, the second reference source 103 and the third reference source 104 in parallel and used for reflecting or transmitting light rays emitted by the laser-induced light source 101 and the reference sources;
the focusing lens 105 is disposed between the laser-induced light source 101 and the first laser-induced light source spectroscope 106, and is configured to focus the laser light emitted by the laser-induced light source 101;
the second laser-induced light source spectroscope 110 is disposed behind the optical path of the first laser-induced light source spectroscope 106, and is used for reflecting or transmitting the arriving light;
the measured sample 117 is placed on the adjustable sample stage 116, and the adjustable sample stage 116 is placed behind the optical path of the second laser-induced light source spectroscope 110;
the collecting lens 111 and the second total reflection mirror 112 are sequentially arranged at one side of the second laser-induced light source spectroscope 110;
the optical fiber probe 113 is arranged on an output light path of the second total reflection mirror 112, is positioned at a laser ablation point on the surface of the sample 117, namely the central position of the excited plasma, and is positioned at an image surface imaged by the collecting lens 111;
the spectrometer 114 is connected to the fiber optic probe 113, and the computer 115 is connected to the spectrometer 114.
Wherein the n-dimensional adjustable sample stage 116 is movable in n directions.
In this embodiment, before the experiment begins, the system starts three monochromatic reference sources and spectrometers, and makes the reference signal emitted by the first reference source 102 reach the first laser-induced light source spectroscope 106 after being reflected by the first reference source spectroscope 107; what is needed isThe reference signal emitted by the second reference source 103 is reflected by the second reference source spectroscope 108, then is transmitted through the first reference source spectroscope 107, and then reaches the first laser-induced light source spectroscope 106; the reference signal emitted by the third reference source 104 is reflected by the first total reflection mirror 109, then transmitted through the second reference source beam splitter 108 and the first reference source beam splitter 107, and combined with the reference signals emitted by the first reference source 102 and the second reference source 103 at the first laser-induced light source beam splitter 106 to form a combined reference signal. The combined reference signal is reflected by the first laser-induced light beam splitter 106 and then transmitted through the second laser-induced light beam splitter 110 to the surface of the sample 117. The combined reference signal reflected by the sample surface returns to the second laser-induced light source spectroscope 110 and is reflected, after passing through the collecting lens 111, the combined reference signal is collected by the fiber-optic probe 113 at the image plane imaged by the collecting lens 111 at the laser ablation point of the sample surface and is further received by the spectrometer 114, and the combined reference signal data is further transmitted to the computer 115 to record the wavelength λ ' of the reference signal emitted by each reference source and the spectrum intensity average value I ' of the reference signal in a period of time 'λ。
After the experiment starts, the laser-induced light source 101 is turned on under the condition that the three monochromatic reference sources and the spectrometer continuously work. Laser pulses emitted by the laser-induced light source 101 pass through the focusing lens 105, are transmitted through the first laser-induced light source spectroscope 106 and the second laser-induced light source spectroscope 110 and are focused on the surface of a detected sample to generate plasma signals; the plasma signal is reflected by the second laser-induced light source spectroscope 110, focused after passing through the collecting lens 111, collected by the fiber optic probe 113 at the image plane where the laser ablation point on the surface of the sample is imaged by the collecting lens 111, and further received by the spectrometer 114 to form a plasma spectrum, and the plasma spectrum data is further transmitted to the computer 115. In one experiment, i plasma spectrograms can be collected.
In the experimental process, after the plasma signal excited by each laser pulse is sufficiently attenuated (generally, the delay is hundreds of microseconds), the spectrometer 114 is used to collect a measured spectrum of the combined reference signal, and at this time, the spectrometer 114 operates in a pulse mode triggered by the laser-induced light source 101.
After the experiment is finished, the computer is used for respectively reading the wave length lambda of each signal peak in the actually measured spectrogram of the i-opening-closing beam reference signaliAnd spectral intensity Iiλ. Will be lambdaiCombining with the measured lambda 'before experiment, obtaining the reference wavelength lambda' of each reference signal in the ith reference signal measured spectrogram along with the measured wavelength lambda by means of polynomial fittingiAnd correcting the drift of each wavelength in the ith plasma spectrogram corresponding to the actually measured spectrogram of the combined reference signal by using the changed relation curve.
Will IiλAnd measured before experiment I'λMaking a difference to obtain the spectral intensity drift I 'at each reference signal wavelength in the ith opening-closing beam reference signal spectrogram'ΔObtaining strong spectrum drift I 'by adopting a polynomial fitting mode'ΔAnd correcting the spectrum intensity drift of each wavelength in the ith plasma spectrum by using the relation curve which changes along with the wavelength lambda' of the reference signal.
In another embodiment of the present invention, the system uses reference sources (such as high-pressure mercury lamps) with multiple wavelengths, where the number of the reference sources is one, and the reference source spectroscope located at one side of the reference sources is a total reflection mirror. As shown in fig. 2, in this embodiment, the system includes: the system comprises a laser-induced light source 201, a multi-wavelength reference source 202, a focusing lens 203, a first laser-induced light source spectroscope 204, a first total reflection mirror 205, a second laser-induced light source spectroscope 206, a collecting lens 207, a second total reflection mirror 208, a fiber-optic probe 209, a spectrometer 210, a computer 211 and an n-dimensional adjustable sample stage 212, wherein:
the laser induction light source 201 and the multi-wavelength reference source 202 are placed in parallel, the laser induction light source 201 is used for emitting induction laser, and the multi-wavelength reference source 202 is used for emitting reference signals;
the first laser-induced light source spectroscope 204 and the first total reflection mirror 205 are arranged on one side of the optical paths of the laser-induced light source 201 and the multi-wavelength reference source 202 in parallel and are used for reflecting or transmitting light rays emitted by the laser-induced light source 201 and the multi-wavelength reference source 202;
the focusing lens 203 is disposed between the laser-induced light source 201 and the first laser-induced light source beam splitter 204, and is configured to focus the laser light emitted by the laser-induced light source 201;
the second laser-induced light source spectroscope 206 is disposed behind the optical path of the first laser-induced light source spectroscope 204, and is used for reflecting or transmitting the arriving light;
the measured sample 213 is placed on the n-dimensional adjustable sample stage 212, and the n-dimensional adjustable sample stage 212 is placed behind the optical path of the second laser-induced light source spectroscope 206;
the collecting lens 207 and the second total reflection mirror 208 are sequentially arranged on one side of the second laser-induced light source beam splitter 206;
the optical fiber probe 209 is arranged on the output light path of the second total reflection mirror 208, is positioned at a laser ablation point on the surface of the sample 213, namely the central position of the excited plasma, and is positioned at an image surface imaged by the collecting lens 207;
the spectrometer 210 is connected to the fiber optic probe 209 and the computer 211 is connected to the spectrometer 210.
In this embodiment, the working principle of the system is similar to that of the system in the previous embodiment, and is not described herein again.
The following explains and explains the main components in the system respectively:
1) laser induced light source
The laser-induced light source that outputs the induced laser light may be one of a semiconductor laser, a solid or gas laser, such as Nd: YAG laser, fiber laser, semiconductor laser coupled by fiber, or carbon dioxide laser;
a) the laser can be a pulse laser (the pulse width is nanosecond, picosecond and femtosecond), a quasi-continuous laser (the pulse width is millisecond), and even a high-power continuous laser;
b) multiple pulse outputs with adjustable interval time can be realized through a power supply or an optical modulation method, so that plasma is induced and generated on the surface of a tested sample for multiple times for repeated measurement;
c) or continuously outputting the sample in a period of time, and continuously inducing the surface of the sample to be detected to generate plasma;
d) according to the excitation requirement of the plasma, lasers with multiple wavelengths can be output simultaneously or by different light sources, so that the excitation effect of the plasma is improved;
e) the plasma signal can be excited in a single pulse mode, and can also be excited in a multi-pulse mode;
f) to accomplish the collection of the plasma signal, the laser can be triggered by a spectrometer, or the spectrometer can be triggered by a laser.
2) Reference source
The purpose is to serve as a reference for compensating the wavelength and spectrum strong drift of the spectrometer in the collection process of plasma signals.
a) The reference source can be a vapor discharge light source, a laser, or other light sources with good wavelength and intensity stability;
b) the reference source can be a single-wavelength light source such as a magnesium lamp, a sodium lamp, a thallium lamp and a He-Ne laser, and can also be a multi-wavelength light source such as a high-pressure mercury lamp;
c) the reference signal emitted by the reference source may be continuous or pulsed.
3) Adjustable sample table
Its usage holds the sample, through the translation or the rotation of mesa, can also accurately control the sample point position.
a) The adjustable sample stage can be n-dimensional, wherein n can be one, two or three, and the specific value of n can depend on the size consistency of the sample and the number of sampling points;
b) the adjustable sample stage can be a translation stage or a rotation stage;
c) the adjustable sample stage can be controlled by a power supply and can also be manually controlled.
4) Spectrum information acquisition subsystem
One of the purposes is to collect plasma signal light excited from the surface of the sample, and the other is to collect a reference signal reflected from the surface of the sample.
a) Consisting of one or more optical elements disposed in the receive path, such as in the embodiment shown in fig. 1, the spectral information collection subsystem includes a second laser-induced light source beam splitter 110, a collection lens 111, a second holomirror 112, and a fiber optic probe 113; in the embodiment shown in fig. 2, the spectral information collection subsystem includes a second laser-induced light source beam splitter 206, a collecting lens 207, a second holophote 208, and a fiber-optic probe 209;
b) the spectrum information acquisition subsystem is used for responding to plasma signals and reference signals in a wider wavelength range, and has higher collection efficiency;
c) the plasma signal and the reference signal can be converged by using a transmission type optical element such as a spherical lens, an aspherical lens and the like;
d) or the plasma signal and the reference signal can be converged by using a reflective optical element such as a parabolic mirror;
5) spectral splitting subsystem
The purpose of the system is to separate the signals collected by the spectrum information collection subsystem according to the wavelength and convert the signals into digital signals, and in the embodiment shown in fig. 1, the spectrum light splitting subsystem is the spectrometer 114; in the embodiment shown in fig. 2, the spectral splitting subsystem is a spectrometer 210.
a) The spectrometer can be a linear array spectrometer such as an optical fiber spectrometer, an area array spectrometer such as a echelle grating spectrometer, other direct-reading spectrometers or other spectrum signal detection equipment such as a spectrophotometer;
b) the CCD or CMOS photosensitive device can be combined with the optical grating light splitting device to form a light splitting subsystem, and the light splitting subsystem is calibrated by using a reference source to replace a spectrometer;
c) only one kind of spectral signal detection equipment can be used, and multiple kinds of spectral signal detection equipment can be used for detecting the plasma signal and the reference signal simultaneously or sequentially;
2. error correction method for laser-induced breakdown spectroscopy signals
According to another aspect of the present invention, there is also provided a method for error correction of a laser-induced breakdown spectroscopy signal, the method comprising the steps of:
s1, starting a reference source and a spectrometer, wherein a reference signal emitted by the reference source reaches the surface of a sample, is reflected and then is sequentially received by the fiber probe and the spectrometer to obtain reference data, and the reference data comprises a reference wavelength lambda ' of the reference signal and a spectrum intensity mean value I ' of the reference signal in a period of time 'λ；
Taking the system shown in fig. 1 as an example, in this step, a first reference source 102, a second reference source 103, a third reference source 104 and a spectrometer 116 are turned on, reference signals emitted by the first reference source 102, the second reference source 103 and the third reference source 104 are combined at a first laser-induced light source spectroscope 106 to form a combined reference signal, the combined reference signal reaching the surface of the sample and reflected passes through a second laser-induced light source spectroscope 110 and a collecting lens 111, and is successively received by a fiber-optic probe 113 and the spectrometer 114 to obtain reference data, the reference data includes a reference wavelength λ ' of the reference signal and a spectral intensity average I ' thereof over a period of time 'λ。
More specifically, before the experiment starts, the first reference source 102, the second reference source 103, the third reference source 104 and the spectrometer 116 are turned on, and the reference signal emitted by the first reference source 102 is reflected by the first reference source beam splitter 107; the reference signal emitted by the second reference source 103 is reflected by the second reference source spectroscope 108, then is transmitted through the first reference source spectroscope 107 and then reaches the first laser-induced light source spectroscope 106, the reference signal emitted by the third reference source 104 is reflected by the first total reflection mirror 109, then is transmitted through the second reference source spectroscope 108 and the first reference source spectroscope 107, and is combined with the reference signals emitted by the first reference source 102 and the second reference source 103 at the first laser-induced light source spectroscope 106 to form a combined beam reference signal. The combined reference signal is reflected by the first laser-induced light source spectroscope 106, and then transmitted through the second laser-induced light source spectroscope 110 to reach the surface of the sample. The combined reference signal reflected by the sample surface is reflected by the second laser-induced light source spectroscope 110, passes through the collecting lens 111, is collected by the laser ablation point on the sample surface through the fiber optic probe 113 at the image plane imaged by the collecting lens 111, is further received by the spectrometer 114, and the obtained combined reference signal spectral data is transmitted to the computer 115.
Wherein the spectrometer 114 operates in a continuous mode and compares the measured wavelength λ ' of each reference signal with its spectral intensity average I ' over a period of time 'λTaking the data as reference data;
s2, laser pulses emitted by the laser induction light source reach the surface of a sample, are reflected and then are received by the optical fiber probe and the spectrometer in sequence to form a plasma spectrum;
specifically, in this step, a laser pulse emitted from the laser-induced light source 101 passes through the focusing lens 105, is transmitted through the first laser-induced light source spectroscope 106 and the second laser-induced light source spectroscope 110, and is focused on the surface of the sample 117 to be measured, so as to generate a plasma signal; the plasma signal is reflected by the second laser-induced light source spectroscope 110, focused after passing through the collecting lens 111, collected by the fiber optic probe 113 positioned at the image plane where the laser ablation point on the surface of the sample is imaged by the collecting lens 111, and further received by the spectrometer 114 to form a plasma spectrum, and the plasma spectrum data is further transmitted to the computer 115.
Wherein, the spectrometer 114 works in a pulse mode, the door opening delay time of the spectrometer is tens of microseconds to hundreds of microseconds after the laser pulse acts, and the specific delay time is determined according to an induction system;
and S3, in the experiment process, after the plasma signal excited by each pulse is sufficiently attenuated, collecting a beam combination reference signal actual measurement spectrogram by using a spectrometer 114.
Wherein, the spectrometer 114 works in a pulse mode, the door opening time of the spectrometer is delayed by hundreds of microseconds compared with the door opening time when the plasma signal is recorded, and the specific delay time depends on an induction system; each reference signal spectrogram corresponds to a plasma spectrogram, and the spectrogram comprises drift information of spectral wavelength and spectral intensity. The collected spectral data is then transmitted to the computer 115.
And S4, correcting the plasma spectrum according to the actually measured spectrogram and the reference data of the combined beam reference signal.
The step S4 includes the steps of:
step S41, determining the measured wavelength lambda of each reference signal in the measured spectrogram of the reference wavelength lambda' and the ith opening and closing beam reference signaliA changed relation curve coefficient according to which the measured wavelength lambda in the plasma spectrogram corresponding to the measured spectrogram of the ith open-close beam reference signaliePerforming drift compensation correction;
specifically, the computer 115 reads out the measured wavelength λ of each reference signal in the measured spectrogram of the ith split-beam reference signaliCombining the wavelengths lambda ' of all reference signals in the reference data, and obtaining the reference wavelength lambda ' of all reference signals along with the actually measured wavelength lambda ' in the actually measured spectrogram of the ith split-combined reference signal by utilizing a polynomial fitting modeiThe relationship of change, i.e.
λ'＝a1λi 2+b1λi+c1 (1)
Wherein, a1、b1、c1Is a polynomial coefficient.
Subsequently, for each measured wavelength λ in the corresponding plasma spectrogram of the reference signal measured spectrogramieThe wavelength drift appearing in the plasma spectrogram can be compensated by performing the conversion of the formula (1);
step S42, obtaining the actually measured spectrum intensity I of each reference signal in the actually measured spectrogram of the combined beam reference signaliλAnd the spectral intensity mean value I'λThe difference I 'between'ΔDetermining the difference value I'ΔAnd (3) carrying out drift compensation correction on the actually measured spectrum intensity corresponding to each wavelength in the plasma spectrogram according to the relation curve coefficient along with the change of the reference wavelength lambda'.
Specifically, the computer 115 reads out the measured spectrum intensity I of each reference signal in the measured spectrogram of each combined reference signaliλAnd each reference signal spectrum intensity I 'in the reference data'λThe difference is made to obtain the spectrum intensity drift I 'at each reference signal wavelength'ΔNamely:
I'Δ＝I'λ-Iiλ (2)
then, obtaining the strong spectrum drift I 'in the actually measured spectrogram of the reference signal by means of polynomial fitting'ΔThe relationship curve as a function of the reference wavelength λ' of the reference signal, namely:
I'Δ＝a2λ'2+b2λ'+c2 (3)
wherein, a2、b2、c2Is a polynomial coefficient.
The drift compensation correction of the actually measured spectrum intensity corresponding to each wavelength in the plasma spectrogram must follow the following formula:
I'i＝I'Δ+Ii (4)
in the formula IiIs the measured spectrum intensity corresponding to each wavelength in the ith plasma spectrum, and is'iThe spectrum intensity corresponding to each wavelength in the ith plasma spectrum obtained after the spectrum intensity drift correction.
Fig. 3 is a flowchart of a method for correcting an error of a laser-induced breakdown spectroscopy signal according to an embodiment of the present invention, in which, in order to reduce an influence of a random error, sampling of a plurality of sampling points is implemented by using an N-dimensional adjustable sample stage, and each sampling point is repeatedly sampled for a plurality of times, where in fig. 3, M represents a sampling number of times of a plasma signal generated at the same sampling point, and N represents the number of sampling points.
In the practice of the present invention, a high-pressure mercury lamp is used as a reference source, and therefore an optical path configuration is adopted as shown in fig. 2, in which:
the laser-induced light source 201 adopts a self-developed Nd of 1064 nm: YAG pulse laser, the pulse energy is 70mJ, the pulse width is 260 mus, the repetition frequency is 2 Hz;the reference source 202 adopts a CEL-WLAM500 type external illumination long arc mercury lamp of a middle and education gold source, the main peak wavelength is 313nm, 334nm and 365nm, and the input power is 500W; the focusing lens 203 has a focal length of 500mm and a diameter of 500mm
Figure BDA0001914385460000151
The plano-convex lens of (1); the first laser-induced light beam splitter 204 and the second laser-induced light beam splitter 206 both use K9 dichroic mirrors, one side of which is coated with high reflectivity (R)>70% @200->85% @1064 nm); the first total reflection mirror 205 and the second total reflection mirror 208 are ultraviolet enhanced aluminum film reflection mirrors (R)>75% @ 200-; the collecting lens 207 is an ultraviolet fused quartz lens coated with an ultraviolet antireflection film (T)>99.5% @250-
Figure BDA0001914385460000152
The optical fiber probe 209 adopts a Shanghai wide-spectrum optical 84UV optical fiber collimating lens, and is applicable to the wavelength range of 200 and 2500 nm; the spectrometer 210 adopts an AvaSpec-Desktop four-channel spectrometer, wherein the four channels respectively cover 190-; sample stage 212 is a two-dimensional manual translation stage with stage dimensions of 60mm by 60 mm.
Before the experiment is started, after a sample is placed on a two-dimensional translation table, the power supply of an externally-illuminated long-arc mercury lamp is switched on, a spectrometer is switched on and works in a continuous mode, mercury lamp signals reflected from the surface of the sample are continuously collected within 10 minutes, and the wavelength lambda ' and the spectrum intensity average value I ' of a plurality of main peaks are recorded 'λAnd the reference data is used as the reference data.
After obtaining the reference data, the spectrometer was set to laser trigger mode, delay time 1 was set to 297.60 μ s, delay time 2 was set to 500 μ s, and integration time was set to 1.05 ms. Opening Nd: YAG laser, set its repetition frequency as 2Hz, and use the energy meter to monitor its output pulse energy, through adjusting applied voltage and working current, control its output pulse energy to be about 70mJ, begin the experiment when the pulse energy is more stable.
At the beginning of the experiment, laser pulses generated by the laser were focused on the sample surface to generate a plasma, and the spectrometer started to collect plasma signals through 297.60 μ s (delay time 1). After 500 mus (delay time 2) the plasma decayed sufficiently and the spectrometer started collecting the mercury lamp signal reflected from the sample surface. For a single sample point, 20 pulses of test data were recorded, and then 10 different sample points were measured by manually adjusting the translation stage. A total of 200 plasma spectra and 200 mercury lamp signal spectra were collected for a single sample.
The following describes the drift compensation process of the ith plasma spectrum:
1. wavelength drift compensation
Reading the signal spectrogram of the ith mercury lamp by a computer to obtain the wavelength and spectrum intensity information of each main peak, comparing the wavelength and spectrum intensity information with the wavelength and spectrum intensity information in the reference data, and fitting the reference wavelength lambda' along with the actually measured wavelength lambda according to a formula (1)iA changing relationship curve; then, each measured wavelength lambda in the ith plasma spectrogramiThe transformation of equation (1) is performed to compensate for the wavelength shift that occurs in the plasma spectrum.
2. Spectral strong drift compensation
Averaging the reference signal according to equation (2) for spectral intensity I'λAnd measured spectrum intensity IiλDifference is made to obtain the spectrum intensity drift I 'at each reference signal wavelength'Δ(ii) a Then, the strong spectrum drift I 'in the reference signal spectrogram is fitted according to the formula (3)'ΔA relation (i) as a function of the reference wavelength λ' of the reference signal; and finally, according to the formula (4) and the relation curve (i), drift compensation is carried out on the actually measured spectrum intensity of each wavelength in the plasma spectrum.
The above-described embodiments are intended to be illustrative only, and various modifications and alterations will readily occur to those skilled in the art based upon the teachings herein and the principles and applications of the invention, rather than being limited to the details and instrumentalities shown and described, and it is intended that the foregoing description be regarded as illustrative rather than restrictive.
The above-mentioned embodiments are intended to illustrate the objects, aspects and advantages of the present disclosure in further detail, and it should be understood that the above-mentioned embodiments are only illustrative of the present disclosure and are not intended to limit the present disclosure, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present disclosure should be included in the scope of the present disclosure.

Claims (10)

1. A laser induced breakdown spectroscopy signal error correction system, the system comprising: laser induction light source, one or more reference sources, focusing lens, first laser induction light source spectroscope, second laser induction light source spectroscope, one or more reference source spectroscopes, total reflection mirror, collecting lens, fiber optic probe, spectrum appearance, computer, n dimension adjustable sample platform, wherein:
the laser-induced light source and the one or more reference sources are placed in parallel, the laser-induced light source is used for emitting induced laser, and the reference source is used for emitting a reference signal;
the first laser-induced light source spectroscope and the one or more reference source spectroscopes are respectively arranged on one side of the light path of the laser-induced light source and one or more reference sources in parallel and used for reflecting or transmitting light rays emitted by the laser-induced light source and the reference source;
the focusing lens is arranged between the laser-induced light source and the first laser-induced light source spectroscope and is used for focusing laser emitted by the laser-induced light source;
the second laser-induced light source spectroscope is arranged behind the light path of the first laser-induced light source spectroscope and used for reflecting or transmitting the arriving light;
a measured sample is placed on the adjustable sample stage, and the adjustable sample stage is placed behind the optical path of the second laser-induced light source spectroscope;
the collecting lens and the total reflection mirror are sequentially arranged on one side of the second laser-induced light source spectroscope;
the optical fiber probe is arranged on the output light path of the total reflection mirror and is positioned on an image surface of a laser ablation point on the surface of a sample imaged by the collecting lens;
the spectrometer is connected with the optical fiber probe, and the computer is connected with the spectrometer;
the laser-induced breakdown spectroscopy signal error correction system enables a laser-induced light source and a reference source to coaxially enter the surface of a sample after combination, and takes a signal reflected from the surface of the sample as a reference, so that wavelength and spectrum intensity drift caused by using factors or change of the refractive index/curvature of the surface of the sample can be compensated.
2. The system according to claim 1, wherein the reference source is a single-wavelength reference source or a multi-wavelength reference source, when the reference source is a single-wavelength reference source, the number of the reference sources is two or more, and the reference source spectroscope located on the side of the reference source away from the laser-induced light source is a total reflection mirror; when the reference source is a multi-wavelength reference source, the number of the reference sources is one, and the reference source spectroscope positioned on one side of the reference source is a total reflection mirror.
3. A system according to claim 1 or 2, wherein the laser-induced light source is a semiconductor laser, a solid-state or a gas laser.
4. The system of claim 1 or 2, wherein the reference source is a vapor discharge light source or a laser.
5. The system of claim 1 or 2, wherein the n-dimensional adjustable sample stage is movable in n directions.
6. The system of claim 1 or 2, wherein the n-dimensional adjustable sample stage is a translation stage or a rotation stage.
7. The system of claim 1 or 2, wherein the spectrometer is a line array spectrometer, an area array spectrometer, or a direct-reading spectrometer.
8. An error correction method based on the laser-induced breakdown spectroscopy signal error correction system of any one of claims 1 to 7, wherein the method comprises the steps of:
step S1, starting a reference source and a spectrometer, wherein a reference signal emitted by the reference source reaches the surface of the sample, is reflected and then is received by the fiber probe and the spectrometer in sequence to obtain reference data, and the reference data comprises a reference wavelength lambda ' of the reference signal and a spectrum intensity average value I ' of the reference signal in a period of time 'λ；
Step S2, laser pulses emitted by the laser-induced light source reach the surface of the sample, are reflected and then are received by the fiber probe and the spectrometer in sequence to form a plasma spectrum;
step S3, after the plasma signal excited by each pulse is sufficiently attenuated, acquiring a beam combination reference signal actual measurement spectrogram by using a spectrometer;
and step S4, correcting the plasma spectrum according to the actually measured spectrogram and the reference data of the beam combination reference signal.
9. The method according to claim 8, wherein the step S1 includes the steps of:
starting the reference source and the spectrometer;
combining the reference signals sent by the reference source at the first laser-induced light source spectroscope to form combined beam reference signals;
the beam combination reference signal reaching the surface of the sample and reflected by the beam combination reference signal passes through the second laser-induced light source spectroscope and the collecting lens and is sequentially received by the fiber-optic probe and the spectrometer to obtain reference data, wherein the reference data comprises a reference wavelength lambda ' of the reference signal and a spectrum intensity mean value I ' of the reference signal in a period of time 'λ。
10. The method according to claim 8 or 9, wherein the step S4 comprises the steps of:
step S41, determining the measured wavelength lambda of each reference signal in the measured spectrogram of the reference wavelength lambda' and the ith opening and closing beam reference signaliA changed relation curve coefficient according to which the measured wavelength lambda in the plasma spectrogram corresponding to the measured spectrogram of the ith open-close beam reference signaliePerforming drift compensation correction;
step S42, obtaining the actually measured spectrum intensity I of each reference signal in the actually measured spectrogram of the combined beam reference signaliλAnd the spectral intensity mean value I'λThe difference I 'between'ΔDetermining the difference value I'ΔAnd (3) carrying out drift compensation correction on the actually measured spectrum intensity corresponding to each wavelength in the plasma spectrogram according to the relation curve coefficient along with the change of the reference wavelength lambda'.
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