CN115046988A - Melt immersion probe based on LIBS technology, online detection device and detection method - Google Patents
Melt immersion probe based on LIBS technology, online detection device and detection method Download PDFInfo
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- CN115046988A CN115046988A CN202210835486.5A CN202210835486A CN115046988A CN 115046988 A CN115046988 A CN 115046988A CN 202210835486 A CN202210835486 A CN 202210835486A CN 115046988 A CN115046988 A CN 115046988A
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Abstract
The invention relates to a melt immersion probe based on LIBS technology, an online detection device and a detection method, wherein the melt immersion probe comprises a probe body, the probe body is in an inverted cone shape, the top end and the bottom end of the probe body are respectively provided with an opening, the side wall of the probe body is respectively and correspondingly provided with an air inlet pipe and an air outlet pipe, and the air inlet pipe and the air outlet pipe are respectively provided with an air valve; the outer periphery of the opening at the bottom end of the probe body is contracted into a hemisphere shape towards the axis direction of the probe body, and a small hole is formed at the axis, the probe can extend into the molten liquid metal at any depth and position by adopting the technical scheme, the steps of laser ranging and focusing debugging are reduced, the cost and the time are saved, real-time online detection is really realized, accurate detection is provided, the content of each element in the molten liquid metal is accurately mastered, the adjustment is made in real time, and the product performance and the quality are ensured; the potential safety hazard is eliminated, the labor intensity of workers is reduced, the automation and the intellectualization of the smelting process are realized, and the energy waste and the emission are reduced.
Description
Technical Field
The invention relates to the field of remote online monitoring of high-temperature liquid components, in particular to a melt immersion probe based on an LIBS technology, an online detection device and a detection method.
Background
The chemical components and the temperature of molten liquid metal need to be diagnosed in real time in the smelting process of steel and alloy so as to judge the smelting end point, thereby controlling the performance of finished metal materials. The traditional smelting process adopts an off-line detection mode of manual sampling and sample preparation. The off-line detection mode needs to be carried out on an analysis instrument for measurement and analysis after a series of processes such as sampling, cooling, grinding, polishing and the like, the whole process takes 4 minutes, which accounts for 10% of smelting time, the performance of the prepared metallurgical finished product material is difficult to reach the expected standard, and energy waste is caused.
In recent years, more and more equipment manufacturing has put strict requirements on the material performance and quality of key parts (such as high-speed bearings and high-speed railway wheels), so that smelting production has increasingly urgent requirements on an online continuous and stable detection sensor technology and a method for molten metal chemical components and temperature resistance to ultra-high temperature and high reliability, and an online detection device based on a Laser Induced Breakdown Spectroscopy (LIBS) technology begins to appear, wherein the LIBS technology is a technology for exciting plasma by using laser and detecting by using an emission spectrum of the plasma. The LIBS technique does not require sample pretreatment and is applicable to solids, liquids, and gases. Therefore, the method has remarkable application value in the aspects of in-situ, online, real-time and non-contact analysis.
At present, there are two types of melt metal online detection devices based on the LIBS technology. The first type mainly uses short-distance and open type optical path detection, optical structures exist on a high-temperature-resistant probe part, the structure is complex, air in an open space strongly absorbs ultraviolet and deep ultraviolet spectrums under high-temperature and smoke severe environments, some nonmetal elements such as C, S, P are the most important elements for quality control and smelting endpoint judgment, plasma characteristic spectrums are mainly distributed in ultraviolet and deep ultraviolet regions, ultraviolet and deep ultraviolet spectrums cannot be effectively detected, in addition, the probe cannot penetrate into liquid metal, and the detection process can also be interfered by slag. The second type mainly comprises an in-situ and on-line detection probe for the components of the remote metallurgical liquid metal, wherein the front-end high-temperature-resistant probe is arranged in the metallurgical liquid metal, a sealed space is formed inside the probe, inert gas is filled in the probe, a light path environment of the inert gas is realized, and an optical element is not arranged inside the probe; the high temperature resistant probe comprises an outer refractory material part and an air charging part, wherein the bottom of the air charging part is of an open structure, but the high temperature resistant probe has the following problems: because the bottom is an open structure, after the probe is placed, because liquid metal at the bottom flows back into the probe, liquid metal laser ranging is needed, then focusing and debugging are carried out, a large amount of time is needed, the delay of optical system focusing generates plasma spectrum real-time disturbance on the current liquid metal acquired by the spectrometer, so that component and temperature measurement deviation is caused, and real-time detection cannot be really realized; secondly, under the condition that liquid metal is in boiling in the smelting process, the metal liquid level can fluctuate, the plasma page is unstable, and the fluctuation of the ion spectral line is uncontrollable, so that the detected component deviation is brought; when the probe extends into the liquid metal again, slag can flow back into the probe along with the liquid metal, interference is caused to the detected components, and the real components of the liquid metal cannot be accurately detected; in addition, due to the material of the probe, the probe cannot be immersed in liquid metal of more than 1700 degrees for too long time, otherwise the probe enables the excitation and collection multiple optical paths to be at high temperature under the action of heat conduction, and the heat radiation generates noise for the spectrum collection at the rear end, so the detection time is shortened.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the melt immersion probe which is not required to adjust laser ranging and focus debugging and can be placed into molten liquid metal to be measured in a metallurgical furnace at any angle and depth based on the LIBS technology.
The invention relates to a melt immersion probe based on LIBS technology, which adopts the following technical scheme: the probe comprises a probe body, wherein the probe body is in an inverted cone shape, the top end and the bottom end of the probe body are respectively provided with an opening, the side wall of the probe body is respectively and correspondingly provided with an air inlet pipe and an air outlet pipe, and the air inlet pipe and the air outlet pipe are respectively provided with an air valve; the periphery of the bottom opening of the probe body is contracted into a hemisphere shape towards the axis direction of the probe body, and a small hole is formed in the axis.
Further, the diameter of the small hole ranges from 1mm to 5 mm.
Further, the diameter of the small hole is 2 mm.
Further, probe body, intake pipe and outlet duct are bilayer structure, and it includes inlayer and skin, the inlayer is by ceramic material shaping, the skin is by high temperature resistant thermal-insulated carbon back ceramic material shaping.
A melt on-line detection device based on LIBS technology adopts the melt immersion probe based on LIBS technology, and further comprises a rear-end console and a sensing unit, wherein the rear-end console is electrically connected with the sensing unit; the sensing unit comprises a box body and an optical system arranged in the box body, the bottom of the box body is connected with the top end of the probe body, an opening corresponding to the opening at the top end of the probe body is formed in the bottom of the box body, and an optical window is arranged at the joint of the opening at the bottom of the box body and the opening at the top end of the probe body.
Further, the box is bilayer structure, and it includes inlayer and skin, the inlayer is by ceramic material shaping, the skin is by high temperature resistant thermal-insulated carbon base ceramic material shaping.
Further, optical system includes laser generator, expands beam focusing module, remote signal collection module, fiber coupling module and fiber optic spectrometer, the fiber optic spectrometer passes through electric connection rear end control platform, laser generator sends laser beam, reaches the aperture of probe body bottom after expanding beam focusing module focuses on, ablates the molten liquid metal that awaits measuring and produces plasma, and plasma cools off the inflation emission signal light under laser induction, and the signal light of plasma conveys the remote signal collection module, again by the fiber coupling module after the coupling in leading-in fiber optic spectrometer again.
Furthermore, the optical system also comprises a first reflector and a second reflector, and a remote beam expanding and focusing module is coaxially arranged in the axial direction of the laser beam emitted by the laser generation module; the first reflector is arranged on the optical axis in the emergent direction of the remote beam expanding and focusing module and forms an angle of 45 degrees with the optical axis, the second reflector is arranged on the optical axis in the incident direction of the remote signal collecting module and forms an angle of 45 degrees with the optical axis, and the central connecting line of the first reflector and the second reflector is vertical to the axes of the remote beam expanding and focusing module and the remote signal collecting module; the optical axis of the remote signal collection module in the emergent direction is provided with an optical fiber coupling module, the optical fiber coupling module is connected with an optical fiber spectrometer through an optical fiber, and the optical fiber spectrometer is electrically connected with a rear end control platform.
Further, optical system still includes real-time imaging module and beam splitter, the beam splitter is established between remote signal collection module and fiber coupling module, and is in on the optical axis of remote signal collection module outgoing direction, real-time imaging module sets up perpendicularly on the optical axis of beam splitter reflection direction, and electric connection rear end control platform.
A detection method of a melt online detection device based on an LIBS technology is applied to the melt online detection device based on the LIBS technology, and comprises the following steps:
the melt immersion probe extends into the metallurgical furnace at any angle, the bottom end of the melt immersion probe penetrates through a slag layer on the surface of molten liquid metal in the metallurgical furnace and is immersed into the molten liquid metal to be detected, the air inlet pipe is filled with inert gas, and air in the probe body flows out from the air outlet pipe, so that a closed inert gas environment is formed in the probe body;
the rear-end control platform controls the laser generation module to emit laser beams, the laser beams are focused by the remote beam expanding and focusing module and reach the small hole at the bottom end of the probe body after passing through the optical window, molten liquid metal to be detected is ablated to generate plasma, the plasma is cooled and expanded under the induction of laser to emit signal light, the signal light of the plasma is transmitted to the remote signal collection module through the inert gas environment in the probe body, then is transmitted to the optical fiber coupling module to be coupled and then is guided into the optical fiber spectrometer to perform optical signal collection and photoelectric conversion, and is fed back to the rear-end control platform to finish the collection of the plasma signal light.
Compared with the prior art, the invention has the following beneficial effects:
1. the periphery of the bottom opening of the probe body is contracted into a hemisphere shape towards the axis direction of the probe body, a small hole is formed at the axis, the molten liquid metal and slag can not flow backwards into the probe body by utilizing the internal surface tension of the molten liquid metal, the molten liquid metal in a boiling state can not be influenced by fluctuation and the molten liquid metal is always attached to the small hole at the bottom of the probe, so that the probe can extend into the molten liquid metal at any depth and any position at any angle, only a laser beam is required to keep focusing on the small hole at the bottom of the probe body, a stable quasi plasma point light source with a certain object distance is provided, the laser distance measurement and focusing debugging steps are reduced, the cost and the time are saved, the real-time online detection is realized in a real sense, the accurate detection is provided, the content of each element in the molten liquid metal is accurately controlled, and the adjustment is made in real time, the product performance and quality are ensured; potential safety hazards are eliminated, the labor intensity of workers is reduced, automation and intellectualization of the smelting process are realized, and energy waste and emission are reduced;
2. the probe and the box body with a double-layer structure are adopted, the inner layer formed by the ceramic material is wrapped with the outer layer formed by the high-temperature-resistant 2300-DEG C heat-insulating carbon-based ceramic material, and the outer layer has the heat-insulating and heat-resisting functions, so that the influence of heat conduction on a duplex light path and an optical element is prevented from causing noise in spectrum collection; the continuous detection time is prolonged, and a temperature adjusting module is not required to be additionally arranged.
Drawings
The accompanying drawings, which are described herein to provide a further understanding of the application, are included in the following description:
fig. 1 is a schematic structural diagram of an embodiment of the present invention.
Detailed Description
Referring to fig. 1, the melt immersion probe based on LIBS technology of the embodiment includes a probe body 3, the probe body 3 is in an inverted cone shape, the top end and the bottom end of the probe body 3 are respectively provided with an opening, the side wall of the probe body 3 is respectively and correspondingly provided with an air inlet pipe 31 and an air outlet pipe 32, and the air inlet pipe 31 and the air outlet pipe 32 are respectively provided with an air valve 33; the bottom opening of the probe body 3 is circumferentially contracted into a hemisphere shape along the axis direction of the probe body 3, and a small hole 34 is formed at the axis.
Further, the diameter of the small hole 34 ranges from 1mm to 5 mm.
Further, the diameter of the small hole 34 is 2 mm.
Further, probe body 3, intake pipe 31 and outlet duct 32 are bilayer structure, and it includes inlayer 6 and skin 5, inlayer 6 is by ceramic material shaping, skin 5 is by high temperature resistant heat insulation carbon base ceramic material shaping.
A melt on-line detection device based on LIBS technology adopts the melt immersion probe based on LIBS technology, and further comprises a rear-end control platform 1 and a sensing unit, wherein the rear-end control platform 1 is electrically connected with the sensing unit; the sensing unit comprises a box body 2 and an optical system arranged in the box body, the bottom of the box body 2 is connected with the top end of the probe body 3, an opening corresponding to the opening at the top end of the probe body 3 is formed in the bottom of the box body 2, and an optical window 25 is arranged at the joint of the opening at the bottom of the box body 2 and the opening at the top end of the probe body 3.
Further, the box body 2 is of a double-layer structure and comprises an inner layer 6 and an outer layer 5, wherein the inner layer 6 is formed by ceramic materials, and the outer layer 5 is formed by high-temperature-resistant heat-insulation carbon-based ceramic materials. The box body 2 and the probe body 3 can be integrally formed and can also be formed in a split mode, and the split forming is more beneficial to later-period maintenance and part replacement or all the parts are applied to experiments in other fields.
The optical system can be various, and only needs to excite the laser to ablate the molten liquid metal to be detected to generate plasma, and then the emission spectrum of the plasma is used for detecting and measuring the components of the molten liquid metal to be detected.
Furthermore, the optical system comprises a laser generator, a beam expanding focusing module, a remote signal collecting module, an optical fiber coupling module and an optical fiber spectrometer, the optical fiber spectrometer is electrically connected with the rear end control platform, the laser generator emits laser beams, the laser beams reach the small hole at the bottom end of the probe body after being focused by the beam expanding focusing module, molten liquid metal to be measured is ablated to generate plasma, the plasma is cooled and expanded under the induction of laser to emit signal light, the signal light of the plasma is transmitted to the remote signal collecting module, and the signal light is coupled by the optical fiber coupling module and then guided into the optical fiber spectrometer; when the probe is used, the melt immersion probe extends into the metallurgical furnace 4 at any angle, the bottom end of the melt immersion probe penetrates through a slag layer 41 on the surface of molten liquid metal in the metallurgical furnace 4 and is immersed into molten liquid metal 42 to be detected, the air inlet pipe 32 is filled with inert gas, and air in the probe body 3 flows out from the air outlet pipe 31, so that a closed inert gas environment is formed in the probe body 3; the rear-end control platform 1 controls the laser generation module 21 to emit laser beams, the laser beams are focused by the remote beam expanding and focusing module 22, the laser beams pass through the optical window 25 and then reach the small hole 34 at the bottom end of the probe body 3, molten liquid metal 42 to be detected is ablated to generate plasma, the plasma is cooled and expanded under the induction of laser to emit signal light, the signal light of the plasma is transmitted to the remote signal collection module 26 through the inert gas environment in the probe body 3, then is transmitted to the optical fiber coupling module 28 to be coupled and then is guided into the optical fiber spectrometer 29 to be subjected to optical signal collection and photoelectric conversion, and is fed back to the rear-end control platform 1, and the collection of the plasma signal light is completed.
Further, the optical system further includes a first reflector 23 and a second reflector 24, and the remote beam expanding and focusing module 22 is coaxially arranged in the axial direction of the laser beam emitted by the laser generating module 21; the first reflector 23 is arranged on the optical axis of the outgoing direction of the remote beam expanding and focusing module 22 and forms an angle of 45 degrees with the optical axis, the second reflector 24 is arranged on the optical axis of the incoming direction of the remote signal collecting module 26 and forms an angle of 45 degrees with the optical axis, and the central connecting line of the first reflector 23 and the second reflector 24 is vertical to the optical axes of the remote beam expanding and focusing module 22 and the remote signal collecting module 26; an optical fiber coupling module 28 is arranged on an optical axis in the emergent direction of the remote signal collecting module 26, the optical fiber coupling module 28 is connected with an optical fiber spectrometer 29 through an optical fiber, and the optical fiber spectrometer 29 is electrically connected with the rear-end control platform 1; when the probe is used, the melt immersion probe extends into the metallurgical furnace 4 at any angle, the bottom end of the melt immersion probe penetrates through a slag layer 41 on the surface of molten liquid metal in the metallurgical furnace 4 and is immersed into molten liquid metal 42 to be detected, the air inlet pipe 32 is filled with inert gas, and air in the probe body 3 flows out from the air outlet pipe 31, so that a closed inert gas environment is formed in the probe body 3; the rear-end control platform 1 controls the laser generation module 21 to emit laser beams, the laser beams are focused by the remote beam expanding and focusing module 22 and then irradiate the first reflecting mirror 23, the reflected laser beams pass through the second reflecting mirror 24 and then reach the small hole 34 at the bottom end of the probe body 3 through the optical window 25, molten liquid metal 42 to be measured is ablated to generate plasma, the plasma is cooled and expanded under the induction of laser to emit signal light, the signal light of the plasma is transmitted to the remote signal collection module 26 through the inert gas environment in the probe body 3, then is transmitted to the optical fiber coupling module 28 to be coupled and then is guided into the optical fiber spectrometer 29 to be subjected to optical signal collection and photoelectric conversion, and is fed back to the rear-end control platform 1 to finish the collection of the plasma signal light.
Further, the optical system further includes a real-time imaging module 20 and a beam splitter 27, the beam splitter 27 is disposed between the remote signal collecting module 26 and the optical fiber coupling module 28 and is located on the optical axis in the emitting direction of the remote signal collecting module 26, the real-time imaging module 20 is vertically disposed on the optical axis in the reflecting direction of the beam splitter 27 and is electrically connected to the rear-end control platform 1; the real-time imaging module 20 receives part of the signal light and the scene background light reflected by the beam splitter 27, and feeds back the signal light and the scene background light to the back-end control platform 1 to display the state of the molten liquid metal 42 at the melt immersion probe orifice 34 and the stable condition of the plasma formation in real time.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. A melt immersion probe based on an LIBS technology comprises a probe body, wherein the probe body is in an inverted cone shape, the top end and the bottom end of the probe body are respectively provided with an opening, the side wall of the probe body is respectively and correspondingly provided with an air inlet pipe and an air outlet pipe, and the air inlet pipe and the air outlet pipe are respectively provided with an air valve; the method is characterized in that: the periphery of the bottom opening of the probe body is contracted into a hemisphere shape towards the axis direction of the probe body, and a small hole is formed in the axis.
2. The LIBS technology-based melt immersion probe of claim 1, wherein: the diameter range of the small holes is 1mm-5 mm.
3. The LIBS technology-based melt immersion probe of claim 1, wherein: the diameter of the small hole is 2 mm.
4. The melt immersion probe based on LIBS technology as claimed in claim 1, wherein: the probe body, the air inlet pipe and the air outlet pipe are of a double-layer structure and comprise an inner layer and an outer layer, the inner layer is formed by ceramic materials, and the outer layer is formed by high-temperature-resistant heat-insulating carbon-based ceramic materials.
5. An on-line melt detection device based on LIBS technology, which adopts the melt immersion probe based on LIBS technology as claimed in claim 1 or 4, and is characterized in that: the system also comprises a rear end console and a sensing unit, wherein the rear end console is electrically connected with the sensing unit; the sensing unit comprises a box body and an optical system arranged in the box body, the bottom of the box body is connected with the top end of the probe body, an opening corresponding to the opening at the top end of the probe body is formed in the bottom of the box body, and an optical window is arranged at the joint of the opening at the bottom of the box body and the opening at the top end of the probe body.
6. The melt online detection device based on the LIBS technology as claimed in claim 5, wherein: the box is bilayer structure, and it includes inlayer and skin, the inlayer is by ceramic material shaping, the skin is by high temperature resistant thermal-insulated carbon base ceramic material shaping.
7. The melt online detection device based on the LIBS technology as claimed in claim 5, wherein: optical system includes laser generator, expands beam focusing module, remote signal collection module, fiber coupling module and fiber optic spectrometer, the fiber optic spectrometer passes through electric connection rear end control platform, laser generator sends laser beam, reaches the aperture of probe body bottom after expanding beam focusing module focus, and the molten liquid metal that the ablation awaits measuring produces plasma, and plasma cools off the inflation emission signal light under laser induction, and the signal light of plasma conveys remote signal collection module, and the reintroduction fiber optic spectrometer after being coupled by fiber coupling module again.
8. The device for detecting the melt on line based on the LIBS technology as claimed in claim 7, wherein: the optical system also comprises a first reflector and a second reflector, and a remote beam expanding and focusing module is coaxially arranged in the axial direction of the laser beam emitted by the laser generating module; the first reflector is arranged on an optical axis in the emergent direction of the remote beam expanding and focusing module and forms an angle of 45 degrees with the optical axis, the second reflector is arranged on the optical axis in the incident direction of the remote signal collecting module and forms an angle of 45 degrees with the optical axis, and the central connecting line of the first reflector and the second reflector is vertical to the axes of the remote beam expanding and focusing module and the remote signal collecting module; the optical axis of the remote signal collection module in the emergent direction is provided with an optical fiber coupling module, the optical fiber coupling module is connected with an optical fiber spectrometer through an optical fiber, and the optical fiber spectrometer is electrically connected with a rear end control platform.
9. The device for detecting the melt on line based on the LIBS technology as claimed in claim 8, wherein: the optical system further comprises a real-time imaging module and a light splitting piece, the light splitting piece is arranged between the remote signal collecting module and the optical fiber coupling module and is positioned on an optical axis in the emergent direction of the remote signal collecting module, the real-time imaging module is vertically arranged on the optical axis in the reflecting direction of the light splitting piece, and the real-time imaging module is electrically connected with the rear-end control platform.
10. A method for detecting a melt on-line detection device based on LIBS technology, which is applied to the melt on-line detection device based on LIBS technology in claim 7, is characterized in that: which comprises the following steps:
the melt immersion probe extends into the metallurgical furnace at any angle, the bottom end of the melt immersion probe penetrates through a slag layer on the surface of molten liquid metal in the metallurgical furnace and is immersed into the molten liquid metal to be detected, the air inlet pipe is filled with inert gas, and air in the probe body flows out of the air outlet pipe, so that a closed inert gas environment is formed in the probe body;
the rear-end control platform controls the laser generation module to emit laser beams, the laser beams are focused by the remote beam expanding and focusing module and reach the small hole at the bottom end of the probe body after passing through the optical window, molten liquid metal to be detected is ablated to generate plasma, the plasma is cooled and expanded under the induction of laser to emit signal light, the signal light of the plasma is transmitted to the remote signal collection module through the inert gas environment in the probe body, then is transmitted to the optical fiber coupling module to be coupled and then is guided into the optical fiber spectrometer to perform optical signal collection and photoelectric conversion, and is fed back to the rear-end control platform to finish the collection of the plasma signal light.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115468914A (en) * | 2022-11-11 | 2022-12-13 | 中国科学院沈阳自动化研究所 | Signal excitation and sampling probe for high-temperature melt composition analysis |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115468914A (en) * | 2022-11-11 | 2022-12-13 | 中国科学院沈阳自动化研究所 | Signal excitation and sampling probe for high-temperature melt composition analysis |
| CN115468914B (en) * | 2022-11-11 | 2023-03-24 | 中国科学院沈阳自动化研究所 | Signal excitation and sampling probe for high-temperature melt component analysis |
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