CN116380874A - Laser-induced breakdown spectroscopy correction method and system based on energy level radiation attenuation - Google Patents
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Abstract
The disclosure belongs to the technical field of laser-induced breakdown spectroscopy, and in particular relates to a laser-induced breakdown spectroscopy correction method and system based on energy level radiation attenuation, comprising the following steps: obtaining a time resolution spectrum of a calibration sample; determining a correction spectral line of the calibration sample based on the acquired time resolution spectrum; calculating the energy level radiation attenuation coefficient of the calibration sample calibration spectral line according to the time resolution spectral line intensity of the selected calibration spectral line; and correcting the spectral line intensity of the time resolution spectrum of the obtained calibration sample according to the energy level radiation attenuation coefficient of the calibration spectral line of the obtained calibration sample, and completing the correction of the laser-induced breakdown spectrum. The embodiment calculates the energy level radiation attenuation rate, corrects the repeatability problem caused by the uncertainty of the attenuation deceleration rate of the energy level radiation in the laser-induced plasma and the uncertainty of the radiation attenuation in the integration time, and improves the measurement precision.
Description
Technical Field
The disclosure belongs to the technical field of laser-induced breakdown spectroscopy, and particularly relates to a laser-induced breakdown spectroscopy correction method and system based on energy level radiation attenuation.
Background
The statements in this section merely provide background information related to the present disclosure and may not necessarily constitute prior art.
Laser Induced Breakdown Spectroscopy (LIBS) is an atomic emission spectroscopy technique that performs qualitative and quantitative analysis on a sample by detecting transient plasma generated by coupling high-energy laser pulses with micro-regions on the surface of the sample. However, the repeatability problem caused by the plasma difference (internal parameters, morphology and material distribution) caused by the uncertainty factors of experimental parameters such as unstable laser energy, floating focal plane and surface variation of ablated micro-area seriously affects the measurement accuracy of the laser-induced breakdown spectroscopy.
The laser-induced breakdown spectroscopy measurement method comprises an internal standard method, full spectrum normalization, ablation volume correction, acoustic correction, ionization degree normalization and spectrum normalization; although the repeatability of the laser-induced breakdown spectroscopy can be partially corrected, and the measurement accuracy of the laser-induced breakdown spectroscopy can be improved, the methods take the spectral signal emission line intensity obtained by a spectrometer in the LIBS system through a period of integration time of energy level radiation as the instantaneous intensity of the energy level radiation, and the line intensity generated by the integration of a certain energy level transition process of atoms or ions in the plasma debilitating process is defaults to the radiation intensity generated by the energy level transition in unit time, so that the attenuation change of the energy level transition radiation in the integration time is ignored.
Enhanced charge coupled device (ICCD) cameras with high speed shutters are often used in laboratories to integrate spectral signals in microseconds or even less to approximate instantaneous energy level radiation, but the resulting line intensity is still far from being equivalent to the instantaneous intensity at the moment of delay, relative to the energy level radiation lifetime of the element under test in the laser-induced plasma. In field or portable applications, since ICCD is expensive, laser-induced breakdown spectroscopy instruments typically employ linear array or face-to-face Charge Coupled Device (CCD) detectors whose integration time covers the entire plasma evolution process relative to the energy level radiation lifetime, ignoring the uncertainty introduced by the energy level radiation decay rate within the integration time.
Disclosure of Invention
In order to solve the problems, the disclosure provides a laser-induced breakdown spectroscopy correction method and system based on energy level radiation attenuation, which aims at the problems of poor repetition and low measurement precision caused by the uncertainty of plasma change in the integration time in the laser-induced breakdown spectroscopy technology, calculates the energy level radiation attenuation rate, corrects the problem of repeatability caused by the uncertainty of the attenuation deceleration rate of energy level radiation in the laser-induced plasma and the uncertainty of radiation attenuation in the integration time, and improves the measurement precision.
According to some embodiments, a first aspect of the present disclosure provides a laser-induced breakdown spectroscopy correction method based on energy level radiation attenuation, which adopts the following technical scheme:
a laser-induced breakdown spectroscopy correction method based on energy level radiation attenuation, comprising:
obtaining a time resolution spectrum of a calibration sample;
determining a correction spectral line of the calibration sample based on the acquired time resolution spectrum;
calculating the energy level radiation attenuation coefficient of the calibration sample calibration spectral line according to the time resolution spectral line intensity of the selected calibration spectral line;
and correcting the spectral line intensity of the time resolution spectrum of the obtained calibration sample according to the energy level radiation attenuation coefficient of the calibration spectral line of the obtained calibration sample, and completing the correction of the laser-induced breakdown spectrum.
As a further technical limitation, in the process of obtaining the time resolution spectrum of the calibration sample, the laser-induced plasma spectrum measurement system is utilized to detect the calibration sample at different positions and different delay times respectively, and the spectrum of the characteristic spectral line containing each element ion and atom of the sample is obtained at each position under one delay time of the same calibration sample, so as to obtain the time resolution spectrum of the calibration sample.
Further, the delay time is the time from the beginning of the decay to the disappearance of the calibration sample plasma in the acquired time resolution spectrum.
Further, when determining the correction spectral line of the calibration sample, selecting the time resolution spectrum with the excited state particle number at the upper energy level in the delay time in the descending trend as the correction spectral line of the calibration sample.
As a further technical limitation, exponential function fitting is performed on the time resolution spectral line intensity after removing negative values in the spectral line intensity of the time resolution of the selected correction spectral line, and the obtained fitting exponential coefficient is the energy level radiation attenuation coefficient of the calibration sample.
As a further technical limitation, linear function fitting is performed on the time resolution spectral line intensity which is linear after removing the negative value in the spectral line intensity of the time resolution of the selected correction spectral line, and the obtained fitting linear coefficient is the energy level radiation attenuation coefficient of the calibration sample.
As a further technical definition, the spectral line intensity at the first delay moment and the spectral line intensity at the last delay moment are subjected to difference, and the obtained difference is multiplied by the energy level radiation attenuation coefficient of the calibration sample calibration spectral line to obtain the corrected spectral line intensity.
According to some embodiments, a second aspect of the present disclosure provides a laser-induced breakdown spectroscopy correction system based on energy level radiation attenuation, which adopts the following technical scheme:
a laser-induced breakdown spectroscopy correction system based on energy level radiation attenuation, comprising:
the acquisition module is used for acquiring a time resolution spectrum of the calibration sample;
the determining module is used for determining a correction spectral line of the calibration sample based on the acquired time resolution spectrum;
the calculation module is used for calculating the energy level radiation attenuation coefficient of the calibration sample calibration spectral line according to the time resolution spectral line intensity of the selected calibration spectral line;
and the correction module is used for correcting the spectral line intensity of the time resolution spectrum of the obtained calibration sample according to the energy level radiation attenuation coefficient of the calibration spectral line of the obtained calibration sample, and completing the correction of the laser-induced breakdown spectrum.
According to some embodiments, a third aspect of the present disclosure provides a computer-readable storage medium, which adopts the following technical solutions:
a computer readable storage medium having stored thereon a program which when executed by a processor performs the steps in a laser induced breakdown spectroscopy correction method based on energy level radiation attenuation as described in the first aspect of the present disclosure.
According to some embodiments, a fourth aspect of the present disclosure provides an electronic device, which adopts the following technical solutions:
an electronic device comprising a memory, a processor and a program stored on the memory and executable on the processor, the processor implementing the steps in the laser induced breakdown spectroscopy correction method based on energy level radiation attenuation as described in the first aspect of the present disclosure when the program is executed.
Compared with the prior art, the beneficial effects of the present disclosure are:
according to the method, the spectrum of the plasma time resolution is obtained, the attenuation coefficient which can represent the attenuation condition of the plasma radiation is obtained by utilizing exponential function fitting or linear fitting after natural logarithm is obtained, uncertainty caused by the change of the plasma in the integral time is corrected, so that the change of the plasma reaches the same level, and the quantitative analysis capability of the laser-induced breakdown spectrum is improved; the method can be applied to differential spectrometers consisting of a plurality of CCDs, so that the precision of the differential spectrometers is higher than that of an expensive ICCD spectrometer.
Drawings
The accompanying drawings, which are included to provide a further understanding of the disclosure, illustrate and explain the exemplary embodiments of the disclosure and together with the description serve to explain the disclosure, and do not constitute an undue limitation on the disclosure.
FIG. 1 is a flow chart of a laser induced breakdown spectroscopy correction method based on energy level radiation attenuation in a first embodiment of the present disclosure;
FIG. 2 is a schematic diagram of the structural principle of a conventional laser-induced plasma spectrometry apparatus and a differential spectrometry apparatus according to a first embodiment of the present disclosure;
FIG. 3 is a schematic illustration of the decay rate leading to repeatability problems in accordance with the first embodiment of the present disclosure;
FIG. 4 (a) is a graph showing exponential fit of elemental silicon in different calibration samples in accordance with one embodiment of the present disclosure;
FIG. 4 (b) is a schematic diagram of a natural log linear fit of silicon in different calibration samples in accordance with one embodiment of the present disclosure;
FIG. 5 (a) is a graph showing the comparison of calibration curves before and after correction of silicon element in a calibration sample according to the first embodiment of the present disclosure;
FIG. 5 (b) is a graph showing the comparison of calibration curves before and after correction of aluminum element in the calibration sample according to the first embodiment of the present disclosure;
FIG. 5 (c) is a graph showing the comparison of calibration curves before and after correction of calcium in the calibration sample according to the first embodiment of the present disclosure;
FIG. 5 (d) is a graph showing the comparison of calibration curves before and after correction of magnesium element in the calibration sample according to the first embodiment of the present disclosure;
the device comprises a pulse laser, a laser focusing light path, a calibration sample, a collecting lens, an optical fiber and a spectrum system, wherein the pulse laser is 1, the laser focusing light path is 2, the calibration sample is 3, the collecting lens is 4, and the optical fiber is 6.
Detailed Description
The disclosure is further described below with reference to the drawings and examples.
It should be noted that the following detailed description is illustrative and is intended to provide further explanation of the present disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this disclosure belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments in accordance with the present disclosure. As used herein, the singular is also intended to include the plural unless the context clearly indicates otherwise, and furthermore, it is to be understood that the terms "comprises" and/or "comprising" when used in this specification are taken to specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof.
Embodiments of the present disclosure and features of embodiments may be combined with each other without conflict.
Laser-induced breakdown spectroscopy (Laser-induced breakdown spectroscopy, LIBS) technology focuses the surface of a sample to form plasma by ultra-short pulse Laser, and further analyzes the plasma emission spectrum to determine the substance composition and content of the sample.
Time resolved spectroscopy (time-resolved spectrum) refers to knowing events and processes that occur during transients by the change in the recorded spectrum over time, resulting in information that is not available in the steady state spectrum (integral spectrum).
Line intensity, which represents the physical quantity of spectral line energy. Any emission line or absorption line has a certain width and profile, i.e. line intensity distribution over a certain frequency range, due to the inherent nature of the atoms and its influence on it by the surrounding physical environment.
Example 1
The embodiment of the disclosure first introduces a laser-induced breakdown spectroscopy correction method based on energy level radiation attenuation.
A laser induced breakdown spectroscopy correction method based on energy level radiation attenuation as shown in fig. 1, comprising the steps of:
step S01: for a calibration sample with known concentrations of each element, the sample is detected by using a laser-induced plasma spectrometry system at different positions with different delay times, each position can obtain a spectrum of a characteristic spectral line containing each element atom and ion at a next delay time, the delay time is the moment when the plasma starts to weaken to disappear, the smaller the delay interval is, the better the integral time is, and the whole plasma life is covered. Different sampling conditions, upper and lower limits of delay time under sample types and different delay intervals;
step S02: repeating step S01 for a set of different calibration samples;
step S03: selecting a correction line to ensure that the number of excited state particles at the upper energy level of the line for each sample is consistently decreasing over a selected delay time;
step S04: removing negative values in the time resolution intensity of spectral lines of one element to be corrected of each calibration sample;
step S05: fitting the time resolution intensities of each element of each set of samples, e may be used -Fx 、ae -Fx 、y 0 +e -Fx Exponential function fitting, wherein the first fitting functionThe number is fitted after 0 value is added and normalized to the intensity of the time resolution, wherein F is an attenuation coefficient, and the attenuation condition of the element energy level radiation can be reflected;
step S06: or taking the natural logarithm of the spectral line intensity after the step S03 is performed, then performing a step S04, and then fitting a part which shows linearity of the intensity of the time resolution by using a linear function Fx+c, wherein F is an attenuation coefficient;
step S07: for the traditional spectrum acquisition system shown in fig. 2, the attenuation coefficient is optimized by adopting the step S06, so that the boundary point between noise and spectral line intensity can be found; multiplying the attenuation coefficient by the spectral line intensity at any delay time to obtain corrected intensity;
step S08: for spectrometers that can obtain a time series of line intensities for the same plasma, both step S05 and step S06 can be used; multiplying the difference of the spectral line intensity at the first delay moment minus the spectral line intensity at the last delay moment by using the attenuation coefficient to obtain corrected spectral line intensity;
step S09: verifying a correction result; establishing a calibration curve according to the concentration of a certain element in a group of different calibration samples in the step S02 and the spectral line intensity before correction, and simultaneously establishing a calibration curve according to the concentration of a certain element in a group of different calibration samples in the step S02 and the spectral line intensity after correction; correlation coefficient R through two calibration curves 2 The correction effect can be compared, and the correction result can be verified.
It should be noted that, the step S07 and the step S08 are specific to different spectrum acquisition systems, so the processing methods are somewhat different, the line intensity before correction in the step S07 may be the line intensity at any delay time, and the corrected line intensity is the result obtained by multiplying the line intensity at any delay time by the attenuation coefficient; the line intensity before correction in step S08 is also the line intensity at any time, but the line intensity after correction is the line intensity at the first delay time minus the line intensity at the last delay time and then multiplied by the attenuation coefficient.
In step S08, the spectral line intensity at the first delay time and the spectral line intensity at the last delay time are subjected to difference, and the obtained difference is multiplied by the energy level radiation attenuation coefficient of the calibration sample calibration spectral line to obtain the corrected spectral line intensity; such as: for a spectrometer which can obtain the same plasma time sequence, for example, the spectrometer can obtain 3 spectral line intensities with delay time of 1us, 2us and 3us, fitting the spectral line intensities of 1us to 3us to obtain an attenuation coefficient, subtracting the spectral line intensity of 3us from the spectral line intensity of 1us, and multiplying the difference between the two delayed spectral line intensities by the attenuation coefficient to obtain corrected spectral line intensity; the line intensity before correction at this time is 1us-3us at any time.
The correction method in this embodiment is described below in conjunction with actual calculation analysis:
firstly, taking 7 standard ore samples with known concentrations of each principal element as a group of calibration samples, wherein the principal elements in the group of samples comprise silicon, aluminum, magnesium and calcium, and the labels and the element concentrations of each sample are shown in table 1:
table 1 labeling of samples and elemental concentrations
Since conventional spectral acquisition systems cannot acquire a time series of plasma radiation per single pulse, and thus cannot directly correct for the problem of repeatability of the single pulse, it can be considered that the time-resolved spectrum obtained in each sample is derived from one average plasma of the sample, whereas the problem of repeatability between samples is more pronounced than the problem of repeatability within samples (changes in focal plane due to sample substitution, changes in reflectivity of the sample surface, etc.), and therefore aims to correct for the reproducibility between samples and thus to improve the ability of quantitative analysis.
Repeatability problem I caused by uncertainty in the rate of decay of radiation over the integration time as shown in fig. 3 ul () 1 And I ul () 2 Is that energy level radiation from two different plasmas decays with time at different decay ratesThe curve of the subtraction is given by,
and->
Then the spectrometer is at delay time t d The line intensities acquired at the moment, it can be seen that, as the integration time increases,/is>
And->
The gap between them also builds up, resulting in more serious repeatability problems.
Acquiring a spectrum of time resolution for each sample using a conventional spectrum acquisition system (acquiring spectra at different positions of each sample with different delays); the delay time is 1us-65us, which covers all the processes of attenuating spectral lines into noise, the delay interval is 1us, and the integration time is 1ms.
Secondly, the correction lines are selected from Si I251.61, al I309.27, ca I527.02 and Mg I285.17, and the upper-level excited state particle numbers of the 4 lines are all declining within the selected delay time range.
Thirdly, replacing all negative values of the line intensities of the 4 lines within 1-65us with 0 values, and enabling the time series lower limits of the line intensities to be consistent while removing negative values; normalizing the time resolution intensity of each element of each sample using e -bx The attenuation coefficient F can be obtained, and for a traditional spectrum acquisition system, as the demarcation point of spectral line intensity and noise cannot be found, exponential fitting can enable the attenuation coefficient F to be fitted into a large amount of noise, and the fitting schematic diagram is shown in fig. 4 (a). As shown in fig. 4 (b), the natural logarithm of the line intensity is obtained, the linear function fx+c is used to fit the linear part of the intensity of the time resolution, and the attenuation coefficient F obtained by the linear function fitting is more accurate by comparing fig. 4 (a) with fig. 4 (b); si I251.61, al I309 obtained for each sample.27. The attenuation coefficients F of the 4 lines Ca I527.02 and Mg I285.17 are multiplied by the line intensities at each delay to obtain corrected line intensities as shown in fig. 5 (a), 5 (b), 5 (c) and 5 (d), respectively.
Finally, a standard curve is established for the spectral line intensity before correction of the 4 spectral lines at 1-10us, and then a standard curve is established for the corrected spectral line intensity, R2 of the two curves can be compared, and the result is shown in Table 2:
TABLE 2 correction results for different elements
According to the embodiment, the spectrum of the plasma time resolution is obtained, the attenuation coefficient which can represent the attenuation condition of the plasma radiation is obtained by utilizing exponential function fitting or linear fitting after natural logarithm is obtained, uncertainty caused by the change of the plasma in the integration time is corrected, so that the change of the plasma reaches the same level, and the quantitative analysis capability of the laser-induced breakdown spectrum is improved.
Example two
The second embodiment of the disclosure introduces a laser-induced breakdown spectroscopy correction system based on energy level radiation attenuation.
A laser-induced breakdown spectroscopy correction system based on energy level radiation attenuation, comprising:
the acquisition module is used for acquiring a time resolution spectrum of the calibration sample;
the determining module is used for determining a correction spectral line of the calibration sample based on the acquired time resolution spectrum;
the calculation module is used for calculating the energy level radiation attenuation coefficient of the calibration sample calibration spectral line according to the time resolution spectral line intensity of the selected calibration spectral line;
and the correction module is used for correcting the spectral line intensity of the time resolution spectrum of the obtained calibration sample according to the energy level radiation attenuation coefficient of the calibration spectral line of the obtained calibration sample, and completing the correction of the laser-induced breakdown spectrum.
The detailed steps are the same as those of the laser-induced breakdown spectroscopy correction method based on energy level radiation attenuation provided in the first embodiment, and will not be described here again.
Example III
A third embodiment of the present disclosure provides a computer-readable storage medium.
A computer readable storage medium having stored thereon a program which when executed by a processor performs the steps in a laser induced breakdown spectroscopy correction method based on energy level radiation attenuation as described in one embodiment of the present disclosure.
The detailed steps are the same as those of the laser-induced breakdown spectroscopy correction method based on energy level radiation attenuation provided in the first embodiment, and will not be described here again.
Example IV
The fourth embodiment of the disclosure provides an electronic device.
An electronic device comprising a memory, a processor and a program stored on the memory and executable on the processor, wherein the processor performs the steps in the laser induced breakdown spectroscopy correction method based on energy level radiation attenuation according to the first embodiment of the present disclosure when executing the program.
The detailed steps are the same as those of the laser-induced breakdown spectroscopy correction method based on energy level radiation attenuation provided in the first embodiment, and will not be described here again.
The foregoing description of the preferred embodiments of the present disclosure is provided only and not intended to limit the disclosure so that various modifications and changes may be made to the present disclosure by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present disclosure should be included in the protection scope of the present disclosure.
While the specific embodiments of the present disclosure have been described above with reference to the drawings, it should be understood that the present disclosure is not limited to the embodiments, and that various modifications and changes can be made by one skilled in the art without inventive effort on the basis of the technical solutions of the present disclosure while remaining within the scope of the present disclosure.
Claims (10)
1. The laser-induced breakdown spectroscopy correction method based on energy level radiation attenuation is characterized by comprising the following steps of:
obtaining a time resolution spectrum of a calibration sample;
determining a correction spectral line of the calibration sample based on the acquired time resolution spectrum;
calculating the energy level radiation attenuation coefficient of the calibration sample calibration spectral line according to the time resolution spectral line intensity of the selected calibration spectral line;
and correcting the spectral line intensity of the time resolution spectrum of the obtained calibration sample according to the energy level radiation attenuation coefficient of the calibration spectral line of the obtained calibration sample, and completing the correction of the laser-induced breakdown spectrum.
2. The method for correcting a laser-induced breakdown spectroscopy based on energy level radiation attenuation as claimed in claim 1, wherein in the process of obtaining the time resolution spectrum of the calibration sample, the laser-induced plasma spectroscopy measurement system is used for respectively detecting the calibration sample at different positions and different delay times, and the time resolution spectrum of the calibration sample is obtained by respectively obtaining the spectrum of the characteristic spectral line containing each element ion and each atom of the sample at each position under one delay time of the same calibration sample.
3. A laser induced breakdown spectroscopy correction method based on energy level radiation attenuation as claimed in claim 2 wherein said delay time is the time from onset to extinction of the calibrated sample plasma in the acquired time resolution spectrum.
4. A method of correcting a laser induced breakdown spectroscopy based on energy level radiation decay as defined in claim 2, wherein when determining the correction line for the calibration sample, a time-resolved spectrum with the number of excited state particles at an upper energy level in a decreasing trend during the delay time is selected as the correction line for the calibration sample.
5. The method of claim 1, wherein the exponential function fitting is performed on the time resolution line intensity after removing negative values in the line intensity of the time resolution of the selected correction line, and the obtained fitting exponential coefficient is the energy level radiation attenuation coefficient of the calibration sample.
6. The method of claim 1, wherein the linear function fitting is performed on the time resolution line intensity which is linear after removing the negative value in the line intensity of the time resolution of the selected correction line, and the obtained fitting linear coefficient is the energy level radiation attenuation coefficient of the calibration sample.
7. The method of claim 1, wherein the line intensity at the first delay time is different from the line intensity at the last delay time, and the obtained difference is multiplied by the energy level radiation attenuation coefficient of the calibration sample calibration line to obtain the corrected line intensity.
8. A laser-induced breakdown spectroscopy correction system based on energy level radiation attenuation, comprising:
the acquisition module is used for acquiring a time resolution spectrum of the calibration sample;
the determining module is used for determining a correction spectral line of the calibration sample based on the acquired time resolution spectrum;
the calculation module is used for calculating the energy level radiation attenuation coefficient of the calibration sample calibration spectral line according to the time resolution spectral line intensity of the selected calibration spectral line;
and the correction module is used for correcting the spectral line intensity of the time resolution spectrum of the obtained calibration sample according to the energy level radiation attenuation coefficient of the calibration spectral line of the obtained calibration sample, and completing the correction of the laser-induced breakdown spectrum.
9. A computer readable storage medium having stored thereon a program, which when executed by a processor, implements the steps of the laser induced breakdown spectroscopy correction method based on energy level radiation attenuation as claimed in any one of claims 1 to 7.
10. An electronic device comprising a memory, a processor and a program stored on the memory and executable on the processor, wherein the processor performs the steps in the laser induced breakdown spectroscopy correction method based on energy level radiation attenuation as claimed in any one of claims 1 to 7.
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| CN117420121A (en) * | 2023-12-19 | 2024-01-19 | 哈尔滨工业大学 | Metal spectrum identification method and system based on collision radiation and spectrum correlation |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117420121A (en) * | 2023-12-19 | 2024-01-19 | 哈尔滨工业大学 | Metal spectrum identification method and system based on collision radiation and spectrum correlation |
| CN117420121B (en) * | 2023-12-19 | 2024-05-14 | 哈尔滨工业大学 | Metal spectrum identification method and system based on collision radiation and spectrum correlation |
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