CN114235517A - Method for automatically removing oxide layer of LIBS stokehole sample by nine-point surrounding - Google Patents
Method for automatically removing oxide layer of LIBS stokehole sample by nine-point surrounding Download PDFInfo
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- CN114235517A CN114235517A CN202111355566.2A CN202111355566A CN114235517A CN 114235517 A CN114235517 A CN 114235517A CN 202111355566 A CN202111355566 A CN 202111355566A CN 114235517 A CN114235517 A CN 114235517A
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- 238000002536 laser-induced breakdown spectroscopy Methods 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 26
- 230000003595 spectral effect Effects 0.000 claims abstract description 23
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 20
- 239000010959 steel Substances 0.000 claims abstract description 20
- 238000004445 quantitative analysis Methods 0.000 claims abstract description 17
- 238000001228 spectrum Methods 0.000 claims description 14
- 230000005284 excitation Effects 0.000 claims description 12
- 238000001514 detection method Methods 0.000 claims description 8
- 238000012935 Averaging Methods 0.000 claims description 3
- 238000003491 array Methods 0.000 claims description 3
- 238000004364 calculation method Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 238000004458 analytical method Methods 0.000 abstract description 8
- 238000003723 Smelting Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000002679 ablation Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/42—Low-temperature sample treatment, e.g. cryofixation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
Abstract
The invention provides a method for automatically removing an oxide layer of a LIBS stokehole sample by nine-point surrounding, and belongs to the field of steel sample component analysis. The method comprises the following steps: s101, placing a sample on a three-dimensional moving platform, taking a point which is 0.5mm away from one side of a laser focusing point as an initial point, exciting laser pulses for multiple times at the initial point, and removing an oxide layer at the initial point; s102, continuously exciting the laser pulse for multiple times at the starting point, selecting spectral data continuously excited by the laser as LIBS quantitative analysis data for judging whether the oxide layer is completely removed, and executing S103 if the oxide layer is completely removed; and S103, starting from the starting point, sequentially removing the oxide layers around the laser focusing point in the clockwise direction by taking 0.5mm as a step pitch, returning to the starting point, moving the laser focusing point by 0.5mm, and exciting the laser pulse at the laser focusing point for M times to finish nine-point surrounding oxide layer removal. By adopting the invention, the time required for preparing the sample can be shortened, the consumption of resources is reduced, and the production efficiency is improved.
Description
Technical Field
The invention relates to the field of steel sample component analysis, in particular to a nine-point surrounding automatic oxide layer removing method for an LIBS stokehole sample.
Background
Steel production is a national post, which gradually tends to be intelligent, continuous and high-precision, wherein the rapid and online detection of molten steel components in the production process is the key point of high-quality production. At present, most of steel sample component detection methods need to take a sample out of a converter or a smelting furnace, the taken high-temperature steel sample can be in contact with air, an oxide layer with ferroferric oxide as a main component is rapidly formed on the surface of the high-temperature steel sample, then the high-temperature steel sample with the oxide layer is cooled and then is manually or pneumatically conveyed to a physical and chemical inspection chamber, the analysis result of the steel sample components can be greatly influenced due to the oxide layer on the surface of the steel sample, the analysis of the steel sample components can be started after the surface of the sample is milled, wherein the time for preparing the sample before detection and analysis is long, the analysis result and the product quality can be influenced, and the energy can be seriously wasted.
Laser-Induced Breakdown Spectroscopy (LIBS) is a rapidly developed substance component detection technology in recent years, has low requirements on sample preparation and high analysis speed, can realize non-contact and long-distance online analysis, and realizes qualitative and quantitative analysis of an object to be detected by analyzing atomic ion characteristic spectral lines in a plasma emission spectrum. However, since the LIBS single-point excitation laser has a small ablation area, the diameter is about 0.3mm, and only the single-point excitation laser is used for removing the oxide layer, the laser excitation times are large, the consumed time is long, and the effect of removing the oxide layer is not good.
Disclosure of Invention
The embodiment of the invention provides a method for automatically removing an oxide layer of a LIBS stokehole sample in a nine-point surrounding manner, which can shorten the time required for preparing the sample, reduce the consumption of resources and improve the production efficiency. The technical scheme is as follows:
the embodiment of the invention provides a method for automatically removing an oxide layer of a LIBS stokehole sample in a nine-point surrounding manner, which comprises the following steps:
s101, placing a sample on a three-dimensional moving platform, taking a point which is 0.5mm away from one side of a laser focusing point as an initial point, exciting laser pulses for multiple times at the initial point, and removing an oxide layer at the initial point;
s102, continuously exciting the laser pulse for multiple times at the starting point, selecting spectral data continuously excited by the laser as LIBS quantitative analysis data for judging whether the oxide layer is completely removed, and executing S103 if the oxide layer is completely removed;
and S103, starting from the starting point, sequentially removing the oxide layers around the laser focusing point in the clockwise direction by taking 0.5mm as a step pitch, returning to the starting point, moving the laser focusing point by 0.5mm, exciting the laser pulses at the laser focusing point for M times, and finishing nine-point surrounding removal of the oxide layers, wherein the laser pulses are excited at each position for M times, and M is the total times of exciting the laser pulses at the starting point.
Further, the sample is a normal-temperature steel sample or a high-temperature steel sample.
Further, the step of placing the sample on a three-dimensional moving platform, with a point 0.5mm away from one side of a laser focus point as an initial point, exciting a laser pulse at the initial point for multiple times, and removing an oxide layer at the initial point comprises:
and (3) placing the sample on a three-dimensional moving platform, taking a point which is 0.5mm away from the left side of a laser focusing point as an initial point, exciting laser pulses for multiple times at the initial point, and removing an oxide layer at the initial point.
Further, the continuously exciting the laser pulse at the starting point for multiple times, selecting spectral data continuously excited by the laser as LIBS quantitative analysis data for determining whether the oxide layer is completely removed, and if the oxide layer is completely removed, executing S103 includes:
continuing to excite the laser pulse P times at the starting point;
summing the spectrum intensities in the specified wavelength range of the spectrum, forming an intensity sum array from the summed P times data, calculating the adjacent difference between the intensity sum array formed by the P times data, and judging whether the intensity sum array meets the threshold requirement, wherein the length of the intensity sum array is P;
if the threshold requirement is met, the oxide layer is completely removed, and S103 is directly executed;
if the threshold requirement is not met, the laser pulse is continuously excited Q times at the starting point to carry out single-point oxide layer removal work, the spectrum data excited by the back P times of laser is selected as LIBS quantitative analysis data, the intensity formed by the P times of data and the adjacent difference of the array are calculated, whether the threshold requirement is met or not is judged, the analogy is carried out until the threshold requirement is met, and S103 is executed after the threshold requirement is met.
Further, said summing the spectral intensities within the spectrally specified wavelength range comprises:
the spectral intensities in the wavelength range of 179.23nm-907.64nm of the spectrum are summed.
Further, the step of forming a strength sum array from the summed P times data, calculating the adjacent difference between the strength sum array formed by the summed data, and determining whether the strength sum array meets the threshold requirement includes:
performing adjacent difference operation on the intensity and the array formed by the P times of data, and subtracting the sum of the spectral intensities acquired by the i-1 th excitation laser from the sum of the spectral intensities acquired by the i-1 th excitation laser to obtain an adjacent difference absolute value; carrying out adjacent difference calculation on the intensity formed by the P-time spectral intensity data and an array to obtain P-1 adjacent difference absolute values;
storing the P-1 adjacent difference absolute values into a new array, averaging the new array to obtain U, wherein the judgment threshold range of whether the new array can be used as quantitative analysis is as follows: [ U-Uxn%, U + Uxn% ], wherein U is the mean value of adjacent difference arrays, U is calculated according to each new array, n is a correction coefficient, and n is more than 0 and less than or equal to 5;
and judging whether all the data in the new array are in the threshold range, if so, meeting the threshold requirement, otherwise, not meeting the threshold requirement.
Further, starting from the starting point, after sequentially removing the oxide layer around the laser focusing point clockwise by taking 0.5mm as a step pitch, returning to the starting point, moving the laser focusing point by 0.5mm, exciting the laser pulse at the laser focusing point for M times, and after finishing removing the oxide layer by nine points in a surrounding manner, the method further comprises the following steps of:
and S104, refocusing the mobile platform to ensure that the data acquisition point is at the laser focusing point, exciting the laser pulse for multiple times at the laser focusing point, and selecting the K-time spectral data as LIBS quantitative analysis data for steel sample component detection.
The technical scheme provided by the embodiment of the invention has the beneficial effects that at least:
in the embodiment of the invention, the oxide layer on the surface of the sample taken out from the converter or the smelting furnace can be directly and automatically removed by adopting nine-point surrounding, the sample does not need to be cooled, fed and milled in advance, the oxide layer can be rapidly removed from the sample in a non-contact way, the time for preparing the sample is greatly shortened, the resource consumption is reduced, the production efficiency is improved, and the production cost is reduced.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a schematic flow chart of a nine-point surrounding automatic oxide layer removal method for an LIBS stokehole sample according to an embodiment of the present invention;
fig. 2 is a schematic diagram of a sequence of nine-point surrounding oxide layer removal according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in detail with reference to the accompanying drawings.
As shown in fig. 1, an embodiment of the present invention provides a method for removing an oxide layer of a LIBS stokehold sample by nine-point surrounding automatic method, including:
s101, placing a sample on a three-dimensional moving platform, taking a point which is 0.5mm away from one side of a laser focusing point as an initial point, exciting laser pulses for multiple times at the initial point, and removing an oxide layer at the initial point;
in this embodiment, the sample is a normal temperature steel sample or a high temperature steel sample.
In this embodiment, a sample is placed on a three-dimensional moving platform, a point 0.5mm away from the left side of a laser focusing point is used as an initial point, a laser pulse is excited for multiple times (for example, 30 times) at the initial point, and an oxide layer at the initial point is removed.
S102, continuously exciting the laser pulse for multiple times at the starting point, selecting spectral data continuously excited by the laser as LIBS quantitative analysis data for judging whether the oxide layer is completely removed, and executing S103 if the oxide layer is completely removed; the method specifically comprises the following steps:
a1, continuing to excite the laser pulse P times at the initial point;
in this example, it is assumed that P is 20, and the laser pulse is continuously excited 20 times at the start point.
A2, summing the spectrum intensities in the specified wavelength range of the spectrum, forming an intensity sum array from the summed P times data, calculating the adjacent difference of the intensity sum array formed by the P times data, and judging whether the intensity sum array meets the threshold requirement, wherein the length of the intensity sum array is P;
in this embodiment, summing the spectrum intensities in the wavelength range of 179.23nm to 907.64nm, forming an intensity sum array from the summed 20 times of data, calculating the adjacent difference between the intensity sum array formed by the 20 times of data, and determining whether the intensity sum array meets the threshold requirement, specifically, the method may include the following steps:
a21, performing adjacent difference operation on the intensity and the array formed by P times (20 times) of data, and subtracting the sum of the spectral intensities acquired by the i-1 th excitation laser from the sum of the spectral intensities acquired by the i-th excitation laser to obtain an absolute value of the adjacent difference; carrying out adjacent difference calculation on the intensity formed by the P-time spectral intensity data and an array to obtain P-1 adjacent difference absolute values;
a22, storing the P-1 adjacent difference absolute values into a new array, and averaging the new array to obtain U, wherein the judgment threshold range of whether the new array can be used as quantitative analysis is as follows: [ U-Uxn%, U + Uxn% ], wherein U is the mean value of adjacent difference arrays, U is calculated according to each new array, n is a correction coefficient, and n is more than 0 and less than or equal to 5;
and A23, judging whether all the data in the new array are in the threshold range, if so, meeting the threshold requirement, otherwise, not meeting the threshold requirement.
A3, if the threshold requirement is met, the oxide layer is completely removed, and S103 is directly executed;
a4, if the threshold requirement is not met, continuing to excite the laser pulse Q times at the starting point to remove the single-point oxide layer, selecting the spectrum data excited by the laser P times as LIBS quantitative analysis data, calculating the intensity formed by the data P times and the adjacent difference of the array, judging whether the threshold requirement is met, repeating until the threshold requirement is met, and executing S103 after the threshold requirement is met.
Because the times of exciting the laser light for the oxide layers in different states are different, for example, if the oxide layer is slightly thicker, the times of exciting the laser light are more, in this embodiment, the times of exciting the laser light can be determined through the threshold range interval, so as to achieve the effect of dynamically removing the oxide layer.
In this embodiment, if Q is equal to 50, if the threshold requirement is not satisfied, the laser pulse is continuously excited at the starting point for 50 times to perform the single-point oxide layer removal operation, the spectral data excited by the last 20 times of laser is selected as LIBS quantitative analysis data, the intensity formed by the 20 times of laser excitation data and the adjacent difference of the array are calculated, whether the threshold requirement is satisfied is determined, and so on until the requirement is satisfied.
And S103, starting from the starting point, sequentially removing the oxide layers around the laser focusing point in the clockwise direction by taking 0.5mm as a step pitch, returning to the starting point, moving the laser focusing point by 0.5mm, exciting the laser pulses at the laser focusing point for M times, and finishing nine-point surrounding removal of the oxide layers, wherein the laser pulses are excited at each position for M times, and M is the total times of exciting the laser pulses at the starting point.
In this embodiment, as shown in fig. 2, starting from the starting point 1, the oxide layer around the laser focusing point is sequentially removed clockwise by taking 0.5mm as a step pitch, and each point excites the laser pulse M times, where M is the total number of times of exciting the laser pulse at the starting point 1, and then returns to the starting point 1, moves rightward by 0.5mm, reaches the laser focusing point 9, and then excites the laser pulse at the laser focusing point 9M times, thereby completing nine-point surrounding removal of the oxide layer.
In the embodiment, one point (laser focusing point 9) is taken as the center, eight points are arranged around the center, nine points are used for removing the oxide layer in a surrounding manner, the time required by sample preparation is greatly shortened, and the resource consumption is reduced.
In this embodiment, after S103, the method further includes:
and S104, refocusing the mobile platform to ensure that the data acquisition point is at the laser focusing point, exciting the laser pulse for multiple times at the laser focusing point, and selecting the K-time spectral data as LIBS quantitative analysis data for steel sample component detection.
The method for automatically removing the oxide layer by nine-point surrounding of the LIBS stokehole sample, provided by the embodiment of the invention, at least has the following beneficial effects:
1) the method has the advantages that the method can directly and automatically remove oxidation of the oxide layer on the surface of the sample taken out of the converter or the smelting furnace by adopting nine-point surrounding, does not need to cool, feed and mill the sample in advance, can realize non-contact rapid removal of the oxide layer on the sample, greatly shortens the time required by preparing the sample, reduces the consumption of resources, improves the production efficiency and reduces the production cost;
2) the laser excitation frequency can be dynamically adjusted according to the oxide layers in different states on the surface of the sample, so that the oxide layer can be dynamically removed, the effect of removing the oxide layer is good, the speed is high, and the method can be used for LIBS (laser induced breakdown spectroscopy) in the production and detection of a converter or an electric furnace.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. A method for automatically removing an oxide layer of a LIBS stokehole sample in a nine-point surrounding manner is characterized by comprising the following steps:
s101, placing a sample on a three-dimensional moving platform, taking a point which is 0.5mm away from one side of a laser focusing point as an initial point, exciting laser pulses for multiple times at the initial point, and removing an oxide layer at the initial point;
s102, continuously exciting the laser pulse for multiple times at the starting point, selecting spectral data continuously excited by the laser as LIBS quantitative analysis data for judging whether the oxide layer is completely removed, and executing S103 if the oxide layer is completely removed;
and S103, starting from the starting point, sequentially removing the oxide layers around the laser focusing point in the clockwise direction by taking 0.5mm as a step pitch, returning to the starting point, moving the laser focusing point by 0.5mm, exciting the laser pulses at the laser focusing point for M times, and finishing nine-point surrounding removal of the oxide layers, wherein the laser pulses are excited at each position for M times, and M is the total times of exciting the laser pulses at the starting point.
2. The LIBS stokehole sample nine-point surrounding automatic oxide layer removing method according to claim 1, wherein the sample is a normal temperature steel sample or a high temperature steel sample.
3. The method for nine-point surrounding automatic oxide layer removal of the LIBS stokehole sample according to claim 1, wherein the step of placing the sample on a three-dimensional moving platform with a point 0.5mm away from one side of a laser focusing point as a starting point, exciting a laser pulse at the starting point for a plurality of times, and removing the oxide layer at the starting point comprises:
and (3) placing the sample on a three-dimensional moving platform, taking a point which is 0.5mm away from the left side of a laser focusing point as an initial point, exciting laser pulses for multiple times at the initial point, and removing an oxide layer at the initial point.
4. The method for the nine-point surrounding automatic oxide layer removal of the LIBS stokehold sample according to claim 1, wherein the laser pulse is continuously excited for a plurality of times at the starting point, the spectrum data of the laser continuous excitation is selected as LIBS quantitative analysis data for determining whether the oxide layer is completely removed, and if the oxide layer is completely removed, the step S103 includes:
continuing to excite the laser pulse P times at the starting point;
summing the spectrum intensities in the specified wavelength range of the spectrum, forming an intensity sum array from the summed P times data, calculating the adjacent difference between the intensity sum array formed by the P times data, and judging whether the intensity sum array meets the threshold requirement, wherein the length of the intensity sum array is P;
if the threshold requirement is met, the oxide layer is completely removed, and S103 is directly executed;
if the threshold requirement is not met, the laser pulse is continuously excited Q times at the starting point to carry out single-point oxide layer removal work, the spectrum data excited by the back P times of laser is selected as LIBS quantitative analysis data, the intensity formed by the P times of data and the adjacent difference of the array are calculated, whether the threshold requirement is met or not is judged, the analogy is carried out until the threshold requirement is met, and S103 is executed after the threshold requirement is met.
5. The method for nine-point surrounding automatic oxide layer removal of the LIBS stokehole sample according to claim 4, wherein the summing the spectral intensities within the specified wavelength range of the spectrum comprises:
the spectral intensities in the wavelength range of 179.23nm-907.64nm of the spectrum are summed.
6. The method of claim 4, wherein the summed P times data form an intensity sum array, the calculating the adjacent difference between the intensity sum array formed by the summed data, and the determining whether the calculated difference satisfies the threshold requirement comprises:
performing adjacent difference operation on the intensity and the array formed by the P times of data, and subtracting the sum of the spectral intensities acquired by the i-1 th excitation laser from the sum of the spectral intensities acquired by the i-1 th excitation laser to obtain an adjacent difference absolute value; carrying out adjacent difference calculation on the intensity formed by the P-time spectral intensity data and an array to obtain P-1 adjacent difference absolute values;
storing the P-1 adjacent difference absolute values into a new array, averaging the new array to obtain U, wherein the judgment threshold range of whether the new array can be used as quantitative analysis is as follows: [ U-Uxn%, U + Uxn% ], wherein U is the mean value of adjacent difference arrays, U is calculated according to each new array, n is a correction coefficient, and n is more than 0 and less than or equal to 5;
and judging whether all the data in the new array are in the threshold range, if so, meeting the threshold requirement, otherwise, not meeting the threshold requirement.
7. The method for nine-point surrounding automatic oxide layer removal of the LIBS stokehole sample according to claim 1, wherein after sequentially removing the oxide layer around the laser focusing point clockwise by a step pitch of 0.5mm from the starting point, returning to the starting point, moving 0.5mm toward the laser focusing point, and exciting the laser pulse at the laser focusing point M times to complete nine-point surrounding oxide layer removal, the method further comprises:
and S104, refocusing the mobile platform to ensure that the data acquisition point is at the laser focusing point, exciting the laser pulse for multiple times at the laser focusing point, and selecting the K-time spectral data as LIBS quantitative analysis data for steel sample component detection.
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| CN114428063A (en) * | 2022-04-01 | 2022-05-03 | 合肥金星智控科技股份有限公司 | Pollution layer spectral data identification method and device, electronic equipment and storage medium |
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