CN106896099B - Device and method for detecting solid material components by laser - Google Patents
Device and method for detecting solid material components by laser Download PDFInfo
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- CN106896099B CN106896099B CN201710188510.XA CN201710188510A CN106896099B CN 106896099 B CN106896099 B CN 106896099B CN 201710188510 A CN201710188510 A CN 201710188510A CN 106896099 B CN106896099 B CN 106896099B
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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
- G01N21/718—Laser microanalysis, i.e. with formation of sample plasma
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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
- G01N1/286—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
- G01N2001/2866—Grinding or homogeneising
Abstract
A device and a method for detecting components of a solid material by laser belong to the technical field of spectrum analysis detection equipment and method and are used for rapidly detecting the components of the solid material on site. The technical proposal is as follows: the front light path unit is connected to the front end of the laser, the front of the front light path unit is opposite to the drawing type sample bin, the front light path unit is packaged in the right packaging sleeve, the drawing type sample bin is packaged in the left packaging sleeve, the laser, the right packaging sleeve, the left packaging sleeve and the drawing type sample bin are sequentially connected through flanges, two ends of an optical fiber are respectively connected with the front light path unit and the spectrometer, and a vacuum pump is connected with a gas pipeline on the side wall of the left packaging sleeve. Compared with other detection means, the method solves the problems of long time consumption, low precision and the like, realizes the on-site rapid detection and analysis of solid material components such as slag, scrap steel and the like, can particularly realize the accurate determination of C, P, S element components, and plays a remarkable role in improving the product quality and the production efficiency.
Description
Technical Field
The invention relates to a device and a method for rapidly detecting solid material components by using laser-induced breakdown spectroscopy, and belongs to the technical field of spectroscopic analysis detection equipment and methods.
Background
The laser-induced breakdown spectroscopy (laser-Induced break down spectroscopy, LIBS) is to emit high-energy pulse laser to act on a sample to generate plasma, acquire and detect ion signals to obtain corresponding spectral information, and further perform corresponding data processing and analysis to obtain the components of each element in the measured sample. The LIBS technology is a substance component and concentration analysis technology based on atomic emission spectroscopy, has the advantages of no need of sample preparation, short analysis time, strong real-time performance, no damage, quick detection, non-contact measurement, no requirement on the form and specification of a sample to be detected, full-spectrum measurement and the like, and is widely applied to the fields of ferrous metallurgy, biological medicine, environmental monitoring and the like. In particular in the field of ferrous metallurgy, the chemical components in steel in the steelmaking process directly affect the quality and performance of finished steel, and in order to realize the automatic control of a steelmaking system and improve the steelmaking control level and the molten steel quality, the rapid detection and analysis of the steel components are required, so that the development and application of a miniaturized rapid and simple test system are widely focused, and the efficient and simple test means and equipment are developed into industry front hot spots.
At present, in the aspect of detecting solid material components such as slag and the like, technologies such as direct-reading spectrometry, X-ray fluorescence spectrometry, CS chemical analysis, inductively coupled plasma emission spectrometry (ICP-OES), gas chromatography, mass spectrometry (ICP-MS) and the like mainly exist, and although the technologies can detect solid material components such as slag, scrap steel and the like, the processes of the technologies need to undergo processes such as sample preparation, grinding and the like, the whole experimental flow is long, the cost is high, and special technicians are required to operate the technologies. The LIBS technology is utilized to measure solid material components such as slag, scrap steel and the like mainly applied to a laboratory stage, and has no breakthrough research in the aspect of industrial equipment, such as multiple light path integrated installation problem, detection environment, experimental condition consistency problem and the like, so that the problems are urgent to be solved. In the aspect of steel component detection in the metallurgical industry, the LIBS equipment is applied to a lot of researches, but currently, for the detection of C, P, S three elements, the accurate detection of the three elements cannot be basically finished by the LIBS equipment formed at home and abroad at present (wherein the laser power of the miniaturized equipment is insufficient, the light path is compact, and the vacuum and inflation environment is not configured). However, for the steel industry, the C, P, S three major elements have important roles in steel grade identification, quality judgment and the like, so that the LIBS equipment is developed and utilized to detect all elements, and particularly the C, P, S three major element components are accurately detected.
Disclosure of Invention
The invention aims to solve the technical problems of a device and a method for detecting solid material components by laser, which can solve the problems that the existing LIBS technology is difficult to realize industrial field application and popularization, realize the field rapid detection of solid material components such as slag, scrap steel and the like, and particularly realize the accurate determination of C, P, S three difficult-to-detect elements.
The technical scheme for solving the technical problems is as follows:
the utility model provides a device of laser detection solid material composition, it includes the laser instrument, leading light path unit, right side encapsulation sleeve, left side encapsulation sleeve, pull sample storehouse, the vacuum pump, the vacuum gauge, optic fibre and spectrum appearance, leading light path unit connects the front end at the laser instrument, leading light path unit's the place ahead is relative with pull sample storehouse, leading light path unit encapsulation is in right side encapsulation sleeve, pull sample storehouse encapsulation is in left side encapsulation sleeve, right side encapsulation sleeve's one end is connected through the flange with the laser instrument, right side encapsulation sleeve's the other end is connected through the flange with left side encapsulation sleeve's one end, left side encapsulation sleeve's the other end is connected through the flange with pull sample storehouse, leading light path unit is connected with one end of optic fibre, the other end of optic fibre passes the optic fibre derivation hole on the right side encapsulation sleeve and is connected with the spectrum appearance, the vacuum pump is connected with the gas piping on the left side encapsulation sleeve lateral wall, the vacuum gauge is installed on the gas piping.
The device for detecting the solid material components by the laser comprises the front light path unit, the rear light path unit and the rear light path unit, wherein the front light path unit comprises a light path, a dichroic mirror support, a focusing part, an incident lens and an optical fiber support, the light path is of a sleeve structure, the rear end of the light path sleeve is connected with the laser through a flange, the dichroic mirror support is arranged on the side wall of the light path, the focusing part is a sleeve, the sleeve of the focusing part is connected with the front end of the light path sleeve, the incident lens is arranged at the front end of the sleeve of the focusing part, and the optical fiber support is arranged at the front end of the incident lens.
According to the device for detecting the solid material components by the laser, the connection parts of the optical channel and the fixed focus part, the connection parts of the fixed focus part and the incidence lens and the connection parts of the incidence lens and the optical fiber support are all of the connection structures of the boss and the groove, and the connection structures are fixed by the hexagon socket head cap bolts.
According to the device for detecting the solid material components by the laser, the light channel and the laser connecting flange are provided with the light channel flange sealing groove, the side wall of the light channel is provided with the plasma signal output hole, the side wall of the light channel is also provided with the dichroic mirror mounting hole and the dichroic mirror support positioning device which form an angle of 45 degrees with the length direction of the light channel, and the side of the dichroic mirror is provided with the spherical positioning groove.
The device for detecting the solid material components by the laser comprises a dichroic mirror support, wherein the dichroic mirror support is provided with a spherical positioning groove, the dichroic mirror support positioning device comprises a top bead, a top bead spring and a top bead spring base, the top bead spring and the top bead spring base are arranged in the side holes of the optical channel, and the top bead is matched with the spherical positioning groove to play a positioning and limiting role.
The device for detecting the solid material components by the laser comprises a bracket disc, a fiber channel, a fiber joint and a fiber buckle, wherein the bracket disc is provided with a fiber channel hole at a certain angle with an axis, the fiber channel is a hollow cylinder with a threaded end part and is in interference fit with the fiber channel hole, the fiber joint and the fiber are connected with each other through threads and are arranged in the fiber channel, the fiber buckle is a hollow cylinder with a certain taper, threads are arranged in the fiber buckle, and the fiber buckle is in threaded fit connection with the front section of the fiber channel.
The device for detecting the solid material components by the laser comprises a sample stage, a position adjusting device and a substrate flange, wherein the sample stage is of a three-section hollow cylindrical structure, the front section of the sample stage is used as a sample placing stage, the front end surface is of a half-section structure, a flat hole is milled on the front end surface, the middle part of the sample stage is of a hollow cylindrical rod-shaped structure, the tail end of the sample stage is of a hollow cylindrical structure with a flat end surface, and threads are arranged inside the sample stage.
The device for detecting the solid material components by the laser comprises a movable ejector rod, an adjusting handle, an ejector rod spring and an ejector rod spring base, wherein the movable ejector rod, the ejector rod spring and the ejector rod spring base are sequentially connected and placed inside a sample table, a threaded hole is formed in the end of the movable ejector rod, the adjusting handle is matched with the threaded hole in installation, a thread is arranged at the tail end of the ejector rod spring base and used for being matched with the threaded hole at the tail of the sample table to fix the position adjusting device, and quick sample replacement can be achieved by pulling the adjusting handle.
According to the device for detecting the solid material components by the laser, the sample platform adjusting groove, the substrate flange sealing groove, the positioning pin hole and the locking groove are formed in the substrate flange, the fixing threaded hole is formed in the upper portion of the sample platform adjusting groove, and the sample platform adjusting groove is fixedly in contact with the end face of the tail of the sample platform.
According to the device for detecting the solid material components by the laser, the quartz observation window and the three-way gas pipeline are arranged on the left packaging sleeve, the quick clamping mechanism is arranged on the connecting flange of the left packaging sleeve and the drawing sample bin, the two locating pins, the fixing pin holes and the flange locking grooves are arranged on the connecting flange of the left packaging sleeve and the drawing sample bin, the two optical fiber guiding-out holes are arranged on the right packaging sleeve, the protective gas channel is arranged on the right packaging sleeve and the connecting flange of the laser, and the two optical fiber guiding-out holes are respectively provided with the optical fibers of the coaxial optical path and the non-coaxial optical path.
The device for detecting the solid material components by the laser comprises a sliding pin, a fixed sliding block, a compression spring, a spring base and a screwing handle, wherein the rapid clamping mechanism is connected and installed in a flange locking groove of a left packaging sleeve through a fixed pin shaft, a U-shaped groove and a connecting hole are formed in the sliding pin, the fixed sliding block is fixed on the sliding pin through the U-shaped groove, the connecting hole is connected with a fixed pin shaft, threads are arranged on the sliding pin shaft and matched with the threaded holes in the screwing handle.
A method for detecting solid material components by using the device, which comprises the following steps:
a. selecting a proper light path system: the coaxial light path is selected, so that the experimental space can be saved, the non-coaxial light path is selected, and the detection precision is higher;
b. the installation of the front light path unit 2 is completed by selecting an incidence lens 24 with a proper focal length and a fixed focus part 23 with a proper length;
c. after the optical fiber combination is installed, the optical fibers 8 are led out from the optical fiber leading-out holes 31 on the right packaging sleeve 3;
d. installing a sample to be tested in the drawing type sample bin 5, and fixing the base flange 53 and the left packaging sleeve 4 flange by utilizing the quick clamping mechanism 45;
e. starting the laser 1, setting lower pulse energy and frequency, observing the laser focus position through the quartz observation window 41, and performing fine adjustment on the sample stage 51 to enable the laser focus to be converged on the sample surface;
f. after the adjustment of the sample position is completed, the spectrometer 9 is started, and parameters of the laser 1 are adjusted according to experimental requirements: pulse energy and frequency, performing spectrum measurement of a series of samples with known contents, and then measuring the spectrum of an unknown sample;
g. the components of the detected element are analyzed by the spectrum obtained by the test.
The beneficial effects of the invention are as follows:
the invention adopts the structures of a laser, a front light path unit, a right packaging sleeve, a left packaging sleeve, a drawing type sample bin, an optical fiber, a spectrometer and the like, the front light path unit can realize the integrated installation of multiple light paths, can quickly realize the switching of different coaxial light paths and coaxial light paths by combining industrial field conditions, and realizes the adjustment of the length and the length of the whole light path; the sample can be quickly replaced by pulling the sample bin, the operation process is simple, and the labor intensity can be effectively reduced; the right packaging sleeve and the left packaging sleeve are convenient to adjust the installation position of the optical fiber, prevent the optical fiber from being bent, meet the requirements of protective atmosphere and vacuum degree, and facilitate the observation of the focusing position of laser on a sample.
Compared with other detection means, the method solves the problems of long time consumption, low precision and the like, has the advantages of remarkable high efficiency, low energy consumption and the like, and plays a remarkable role in improving the product quality and the production efficiency.
The invention is a breakthrough of LIBS equipment in the steel component detection technology, solves the long-term unsolved problem, realizes the full-element industrial detection by utilizing the LIBS equipment, particularly the accurate detection of the C, P, S three main element components, and opens up a new way for the industrial utilization of the LIBS equipment.
Drawings
FIG. 1 is a schematic diagram of the structure of the present invention;
fig. 2 is a schematic structural view of the front optical path unit;
FIG. 3 is a cross-sectional view of FIG. 2;
fig. 4, 5, 6, and 7 are schematic structural views of a dichroic mirror holder, a focusing member, an incident lens, and an optical fiber holder, respectively, of a front optical path unit;
FIG. 8 is a schematic drawing of a drawing type sample cartridge structure;
FIG. 9 is a cross-sectional view of FIG. 8;
FIG. 10 is a schematic view of the right packaging sleeve;
FIG. 11 is a schematic structural view of a left packaging sleeve;
FIG. 12 is a schematic view of the structure of the quick clamp mechanism;
fig. 13 is a schematic view of the slide pin structure in the quick clamp mechanism.
The figures are labeled as follows:
the device comprises a laser 1, a front light path unit 2, a right packaging sleeve 3, a left packaging sleeve 4, a drawing type sample bin 5, a vacuum pump 6, a vacuum gauge 7, an optical fiber 8 and a spectrometer 9;
a light channel 21, a dichroic mirror holder 22, a focusing member 23, an incidence lens 24, an optical fiber holder 25;
light channel flange seal groove 211, plasma signal output hole 212, dichroic mirror mounting hole 213, dichroic mirror bracket positioning device 214, dichroic mirror 215, light channel side hole 216, spherical positioning groove 2151, top bead 2141, top bead spring 2142, top bead spring mount 2143;
a fixed Jiao Bujian fiber lead-out groove 235 and an incident lens fiber lead-out groove 243;
bracket disc 253, fiber channel 254, fiber splice 255, fiber clasp 256, fiber channel aperture 2531;
optical fiber leading-out holes 31, 32, and a shielding gas passage 33;
the quartz observation window 41, the three-way gas pipeline 42, the positioning pin 411, the fixing pin hole 412, the fixing pin shaft 413 and the flange locking groove 414;
quick clamp mechanism 45, slide pin 451, fixed slide 452, compression spring 453, compression spring mount 454, and screw handle 455;
a sample stage 51, a position adjusting device 52, a base flange 53;
a movable ejector 521, an adjusting handle 522, an ejector spring 523, and an ejector spring base 524;
sample stage adjustment slot 531, base flange seal slot 532, dowel pin hole 533, locking slot 534;
description of the embodiments
The invention comprises a laser 1, a front light path unit 2, a right packaging sleeve 3, a left packaging sleeve 4, a drawing type sample bin 5, a vacuum pump 6, a vacuum gauge 7, an optical fiber 8 and a spectrometer 9.
Fig. 1 shows that the front light path unit 2 is connected to the front end of the laser 1, the front of the front light path unit 2 is opposite to the drawing sample bin 5, the front light path unit 2 is packaged in the right packaging sleeve 3, the drawing sample bin 5 is packaged in the left packaging sleeve 4, one end of the right packaging sleeve 3 is connected with the laser 1 through a flange, the other end of the right packaging sleeve 3 is connected with one end of the left packaging sleeve 4 through a flange, and the other end of the left packaging sleeve 4 is connected with the drawing sample bin 5 through a flange. The front light path unit 2 is connected with one end of an optical fiber 8, the other end of the optical fiber 8 passes through an optical fiber leading-out hole 32 on the right packaging sleeve 3 and is connected with the spectrometer 9, and the spectrometer 9 is connected with a software post-processing unit for spectral data processing and quantitative analysis. The vacuum pump 6 is connected with a gas pipeline on the side wall of the left packaging sleeve 4, and the vacuum gauge 7 is arranged on the gas pipeline.
Fig. 2 and 3 show that the front optical path unit 2 includes an optical channel 21, a dichroic mirror holder 22, a focusing member 23, an incidence lens 24, and an optical fiber holder 25. The light channel 21 is of a sleeve structure, a flange is arranged at the rear end of the sleeve of the light channel 21 and is connected with the laser 1, the dichroic mirror support 22 is arranged on the side wall of the light channel 21, the fixed focus part 23 is a sleeve, the sleeve of the fixed focus part 23 is connected with the front end of the sleeve of the light channel 21, the incidence lens 24 is arranged at the front end of the sleeve of the fixed focus part 23, and the optical fiber support 25 is arranged at the front end of the incidence lens 24.
Fig. 2 and 3 show that the flange of the light channel 21 is provided with a light channel flange sealing groove 211 for ensuring the vacuum degree and the protection atmosphere sealing required by the experiment. The optical channel 21 is laterally open with a plasma signal output aperture 212 from which the plasma signal is directed via a dichroic mirror when a coaxial optical path is used, the signal being input into the spectrometer 9 via a collimator lens. The side wall of the light channel 21 is also provided with a dichroic mirror mounting hole 213 and a dichroic mirror bracket positioning device 214 which form an angle of 45 degrees with the length direction of the light channel 21, thereby facilitating the mounting and positioning of the dichroic mirror 215. A spherical positioning groove 2151 is provided on the side of the dichroic mirror 215.
Fig. 3 and 4 show that dichroic mirror 215 has a spherical positioning groove 2151, and dichroic mirror positioning device 214 includes a top bead 2141, a top bead spring 2142, and a top bead spring mount 2143. The top bead 2141, the top bead spring 2142 and the top bead spring base 2143 are disposed in the side hole 216 of the light channel, and when the dichroic mirror support 22 is installed, the top bead 2141 and the spherical positioning groove 2151 are matched to play a role in positioning and limiting.
Fig. 4, 5, 6 and 7 show that the front ends of the optical channel 21, the focusing component 23 and the incident lens 24 are respectively provided with a boss with the height of 2-3 mm and a screw hole, the tail parts of the focusing component 23 and the optical fiber support 25 are provided with a groove with the height of 2-3 mm and a screw hole, wherein the front ends of the focusing component 23 and the incident lens 24 are respectively provided with a fixed Jiao Bujian optical fiber guiding-out groove 235 and an incident lens optical fiber guiding-out groove 243, and the bosses and the grooves are mutually matched and positioned according to the optical fiber guiding-out grooves and are fixed by means of inner hexagonal cylindrical head screws.
Fig. 7 shows that the optical fiber support 25 includes a support disc 253, an optical fiber channel 254, an optical fiber connector 255 and an optical fiber buckle 256, wherein the support disc 253 is provided with an optical fiber channel hole 2531 which is 25.27 degrees with the axis, the optical fiber channel 254 is a hollow cylinder with a threaded end portion, the optical fiber channel is in interference fit with the optical fiber channel hole 2531, the optical fiber connector 255 and the optical fiber 8 are connected in the optical fiber channel through threads, the optical fiber buckle 256 is a hollow cylinder with a certain taper, and the inside of the optical fiber connector is provided with threads and is in threaded fit connection with the front section of the optical fiber channel 254.
Fig. 8 and 9 show that the drawing type sample chamber 5 includes a sample stage 51, a position adjusting device 52, and a base flange 53. The sample stage 51 is a three-section hollow cylindrical structure, the front section of the sample stage is a half-section structure, the outer diameter is 42mm, the front end face is milled to be flat, the middle part is a hollow cylindrical rod-shaped structure with the diameter of 20mm, the tail end is a hollow cylindrical structure with a flat end face, and threads are arranged in the hollow cylindrical structure for installing the ejector rod spring base 524.
Fig. 8 and 9 show that the position adjustment device 52 includes a movable plunger 521, an adjustment handle 522, a plunger spring 523, and a plunger spring mount 524. The movable ejector rod 521 is provided with a threaded hole at the end, the adjusting handle 522 is matched with the threaded hole, the movable ejector rod 521, the ejector rod spring 523 and the ejector rod spring base 524 are sequentially connected and arranged inside the sample table 51, the tail part of the ejector rod spring base 524 is provided with threads, the position adjusting device 52 is matched and fixed with the tail end of the sample table 51, and quick sample changing can be realized by pulling the adjusting handle 522.
Fig. 8 and 9 show that the base flange 53 is provided with a sample stage adjusting groove 531, a base flange sealing groove 532, a positioning pin hole 533 and a locking groove 534. The upper part of the sample platform adjusting groove 531 is provided with a fixed threaded hole, and the inner hexagonal flat end surface is contacted and fixed with the tail end surface of the sample platform 51 by screwing the inner hexagonal flat end set screw.
Fig. 10 shows that sleeve flanges are provided at both ends of the right packaging sleeve 3, two optical fiber guiding holes 31, 32 are provided on the right packaging sleeve 3, and the two optical fiber guiding holes 31, 32 are respectively used for guiding out the optical fiber 8 when the optical path is not coaxial and the optical path is coaxial, and a protective gas channel 33 is provided on the right flange of the connection of the right packaging sleeve 3 and the front optical path unit 2.
Fig. 11 shows that sleeve flanges are arranged at two ends of the left packaging sleeve 4, and a quartz observation window 41 and a three-way gas pipeline 42 are arranged on the left packaging sleeve 4. The left end flange that left packaging sleeve 4 and pull sample storehouse 5 are connected is equipped with two locating pins 411, fixed pinhole 412, fixed pin shaft 413 and flange locking groove 414 on, and quick clamping mechanism 45 of pull sample storehouse 5 passes through fixed pin shaft 413 to be installed on the left end flange, and quick clamping mechanism 45 can rotate around fixed pin shaft 413, is convenient for fixed pull sample storehouse 5.
Fig. 12 and 13 show that quick clamp mechanism 45 includes a slide pin 451, a fixed slide 452, a compression spring 453, a compression spring mount 454, and a tightening handle 455. The sliding pin 451 is provided with a U-shaped groove and a connecting hole, the U-shaped groove is used for fixing the position of the sliding block 452 on the sliding pin 451, the position of the U-shaped groove is adjusted according to the thickness of the sample substrate flange 53, the connecting hole is connected with the fixed pin 413, and the quick clamping mechanism 45 is integrally arranged in the flange locking groove 414 of the left packaging sleeve 4, so that the quick clamping mechanism can realize circumferential rotation around the fixed pin 413 through the sliding pin 451. The sliding pin shaft is provided with threads which are matched with the threaded holes in the screwing handle 455, a compression unit formed by the fixed sliding block 452, the compression spring 453 and the compression spring base 454 is fixed, and after the position adjustment of the sample is completed, the drawing sample bin 5 and the left packaging sleeve 4 can be locked and fixed by screwing the handle 455.
The invention uses and works the principle of each part:
use of the front optical path unit 2: according to experimental requirements and the actual volume of a space optical path, firstly, a proper optical path system is selected. When a non-coaxial light path is adopted, the incident laser direction forms a certain angle with the direction of collecting plasma after exciting a sample, a dichroic mirror is not required to be installed at the moment, a fixed focus part 23 which is suitable for the focal length of an incident lens 24 is selected to be installed at the front section of a light channel 21 by using an inner hexagonal bolt, the incident lens 24 is installed at the front section of the fixed focus part 23, an optical fiber 8 is fixed on an optical fiber bracket 25, and then the optical fiber 8 is led out from an optical fiber leading-out hole 31 through the lens bracket, an optical fiber leading-out groove 235 of the fixed focus part 23 and an incident lens optical fiber leading-out groove 243; when the coaxial optical path is adopted, the dichroic mirror 215 is mounted on the optical path 21, the other component mounting position is kept unchanged, and the optical fiber 8 is guided out from the fiber guiding-out hole 32.
Use of the drawing sample bin 5: the sample to be tested is selected, the adjusting handle 522 is pulled back, the ejector rod spring 523 is contracted, the sample is placed in the sample table 51, the surface of the sample is ensured to be flush with the front end surface, after the sample is installed, the sample table 51 is adjusted to a proper distance according to the fixed focal length, then the sample is fixed through the inner hexagonal flat end set screw, and when the sample is replaced, the quick clamping mechanism 45 is only required to be removed, and the whole drawing of the drawing sample bin 5 is carried out for sample replacement.
Use of right packaging sleeve 3, left packaging sleeve 4: according to experimental requirements, the inside of the right packaging sleeve 3 and the left packaging sleeve 4 is ensured to keep certain vacuum degree or protective atmosphere by connecting a vacuum pump 6 or an argon filling device. The focal position is observed through the quartz observation window 41, and the sample stage 51 is finely adjusted to a certain degree.
Use of the quick clamp mechanism 45: the quick clamping mechanism 45 mainly meets the requirement of quick replacement of samples, firstly, the screwing handle 455 is loosened, the fixing slider 452 is separated from the base flange 53, the drawing type sample bin 5 is drawn out for sample replacement, after the focusing distance is adjusted, the sliding pin 451 is rotated, the base flange 53 is fixed with the left sleeve flange by the fixing slider 452, and finally, the handle 455 is screwed, so that the drawing type sample bin 5 and the left packaging sleeve 4 are locked and fixed, and sealing is ensured.
The method for detecting the solid material components by using the device comprises the following steps:
a. selecting a proper light path system: the coaxial light path is selected, so that the experimental space can be saved, the non-coaxial light path is selected, and the detection precision is higher;
b. the installation of the front light path unit 2 is completed by selecting an incidence lens 24 with a proper focal length and a fixed focus part 23 with a proper length;
c. after the optical fiber combination is installed, the optical fibers 8 are led out from the optical fiber leading-out holes 31 on the right packaging sleeve 3;
d. installing a sample to be tested in the drawing type sample bin 5, and fixing the base flange 53 and the left packaging sleeve 4 flange by utilizing the quick clamping mechanism 45;
e. starting the laser 1, setting lower pulse energy and frequency, observing the laser focus position through the quartz observation window 41, and performing fine adjustment on the sample stage 51 to enable the laser focus to be converged on the sample surface;
f. after the adjustment of the sample position is completed, the spectrometer 9 is started, and parameters of the laser 1 are adjusted according to experimental requirements: pulse energy and frequency, performing spectrum measurement of a series of samples with known contents, and then measuring the spectrum of an unknown sample;
g. the components of the detected element are analyzed by the spectrum obtained by the test.
The following describes the method of using the experimental device of the invention with reference to specific examples:
example 1
The invention is used for measuring elements of a solid steel sample by taking a spark direct-reading spectrum standard sample carbon structural steel as an example.
Before the experiment starts, it is first ensured that the laser 1 is in the ideal working environment (temperature, humidity, etc.).
A non-coaxial optical path system and an incident lens with a focal length of 100mm are selected.
The installation of the front optical path unit 2 is completed by selecting an incident lens 24 having a focal length of 100mm and a focusing member 23 having a length of 40 mm.
After the optical fiber combination is installed, the optical fibers 8 are led out from the optical fiber leading-out holes 31 on the right packaging sleeve 3.
The sample to be tested is arranged in the drawing type sample bin 5, and the base flange 53 is fixed with the flange of the left packaging sleeve 4 by utilizing the quick clamping mechanism 45.
The laser 1 was turned on, the laser focal position was observed through the quartz observation window 41 by setting a low pulse energy (100 mJ) and a low pulse frequency (1 HZ), and the sample stage 51 was fine-tuned to focus the laser focal point on the sample surface.
After the adjustment of the sample position is completed, the spectrometer 9 is started, and parameters of the laser 1 are adjusted according to experimental requirements: pulse energy (130 mJ), frequency (1 HZ), a series of spectral measurements of samples of known content were performed, and then the spectra of the unknown samples were determined.
The linear correlation coefficient of the C element can reach 0.999 and the content of the C element is 0.43 percent (the authentication content of the C element is 0.44 percent) by using an internal standard method.
Example 2
The invention is used for detecting elements of slag.
Before the experiment starts, it is first ensured that the laser 1 is in the ideal working environment (temperature, humidity, etc.).
A coaxial optical path and an entrance lens 24 with a focal length of 40mm are selected.
The slag sample was ground and pressed into a disc shape (direct measurement), and the front optical path was installed by selecting an incident lens 24 having a focal length of 40mm, a focusing member 23 having a length of 100mm, and a dichroic mirror.
After the optical fiber combination is installed, the optical fibers 8 are led out from the optical fiber leading-out holes 32 on the right packaging sleeve 3.
The sample to be tested is arranged in the drawing type sample bin 5, and the base flange 53 is fixed with the flange of the left packaging sleeve 4 by utilizing the quick clamping mechanism 45.
The laser 1 was turned on, the laser focal position was observed through the quartz observation window 41 by setting a low pulse energy (100 mJ) and a low pulse frequency (1 HZ), and the sample stage 51 was fine-tuned to focus the laser focal point on the sample surface.
After the adjustment of the sample position is completed, the spectrometer 9 is started, and parameters of the laser 1 are adjusted according to experimental requirements: pulse energy (130 mJ), frequency (1 HZ), a series of spectral measurements of known content slag flakes samples were performed, followed by measurement of unknown slag samples.
The Si content of the alloy is reversely calculated to be 36.73 percent (the standard sample YSBC28851-98 of blast furnace slag and the certified content of SiO2 is 34.65 percent) by using an internal standard method.
Claims (9)
1. A device for laser detection of solid material components, characterized in that: the device comprises a laser (1), a front light path unit (2), a right packaging sleeve (3), a left packaging sleeve (4), a drawing type sample bin (5), a vacuum pump (6), a vacuum gauge (7), an optical fiber (8) and a spectrometer (9), wherein the front light path unit (2) is connected to the front end of the laser (1), the front of the front light path unit (2) is opposite to the drawing type sample bin (5), the front light path unit (2) is packaged in the right packaging sleeve (3), the drawing type sample bin (5) is packaged in the left packaging sleeve (4), one end of the right packaging sleeve (3) is connected with the laser (1) through a flange, the other end of the right packaging sleeve (3) is connected with one end of the left packaging sleeve (4) through a flange, the other end of the left packaging sleeve (4) is connected with the drawing type sample bin (5) through a flange, the other end of the front light path unit (2) is connected with one end of the optical fiber (8) through a lead-out hole (31) on the right packaging sleeve (3), the other end of the optical fiber (8) is connected with the optical fiber (9) through the flange, and the vacuum gauge is connected with the gas pipe (7) through the side wall of the vacuum gauge;
the front light path unit (2) comprises a light channel (21), a dichroic mirror support (22), a fixed Jiao Bujian (23), an incident lens (24) and an optical fiber support (25), wherein the light channel (21) is of a sleeve structure, the rear end of the sleeve of the light channel (21) is connected with the laser (1) through a flange, the dichroic mirror support (22) is arranged on the side wall of the light channel (21), the fixed Jiao Bujian (23) is a sleeve, the sleeve of the fixed Jiao Bujian (23) is connected to the front end of the sleeve of the light channel (21), the incident lens (24) is arranged at the front end of the sleeve of the fixed Jiao Bujian (23), and the optical fiber support (25) is arranged at the front end of the incident lens (24);
an optical channel flange sealing groove (211) is formed in a connecting flange of the optical channel (21) and the laser (1), a plasma signal output hole (212) is formed in the side wall of the optical channel (21), a dichroic mirror mounting hole (213) and a dichroic mirror support positioning device (214) which form an angle of 45 degrees with the length direction of the optical channel (21) are formed in the side wall of the optical channel (21), and a spherical positioning groove (2151) is formed in the side of the dichroic mirror (215);
the dichroic mirror support positioning device (214) comprises a top bead (2141), a top bead spring (2142) and a top bead spring base (2143), wherein the top bead (2141), the top bead spring (2142) and the top bead spring base (2143) are arranged in the side hole (216) of the light channel.
2. The apparatus for detecting a solid material component by laser light according to claim 1, wherein: the connection part of the light channel (21) and the fixed Jiao Bujian (23), the connection part of the fixed Jiao Bujian (23) and the incident lens (24) and the connection part of the incident lens (24) and the optical fiber bracket (25) are all of a connection structure of a boss and a groove, and are fixed by an inner hexagon bolt.
3. The apparatus for detecting a solid material component by laser light according to claim 1, wherein: the optical fiber bracket (25) comprises a bracket disc (253), an optical fiber channel (254), an optical fiber connector (255) and an optical fiber buckle (256), wherein an optical fiber channel hole (2531) with a certain angle with an axis is formed in the bracket disc (253), the optical fiber channel (254) is a hollow cylinder with a threaded end part and is in interference fit with the optical fiber channel hole (2531), the optical fiber connector (255) is connected with an optical fiber (8) through threads and is arranged in the optical fiber channel (254), the optical fiber buckle (256) is a hollow cylinder with a certain taper, threads are arranged in the optical fiber buckle, and the optical fiber connector is connected with the front section of the optical fiber channel (254) through the threads.
4. A device for laser detection of solid material components as claimed in claim 3, wherein: the drawing type sample bin (5) comprises a sample table (51), a position adjusting device (52) and a substrate flange (53), wherein the sample table (51) is of a three-section hollow cylindrical structure, the front section of the sample table (51) is used as a sample placing table, the front end surface is of a half-section structure, the front end surface is provided with a flat hole in a milling mode, the middle part of the sample table is of a hollow cylindrical rod-shaped structure, the tail end of the sample table is of a hollow cylindrical structure with a flat end surface, and threads are arranged inside the sample table.
5. The apparatus for detecting a solid material component by laser light according to claim 4, wherein: the position adjusting device (52) comprises a movable ejector rod (521), an adjusting handle (522), an ejector rod spring (523) and an ejector rod spring base (524), wherein the movable ejector rod (521), the ejector rod spring (523) and the ejector rod spring base (524) are sequentially connected and arranged in the sample table (51), a threaded hole is formed in the end part of the movable ejector rod (521), the adjusting handle (522) is matched with the threaded hole, and threads are formed in the tail end of the ejector rod spring base (524).
6. The apparatus for detecting a solid material component by laser light according to claim 5, wherein: the base flange (53) is provided with a sample stage adjusting groove (531), a base flange sealing groove (532), a positioning pin hole (533) and a locking groove (534), the upper part of the sample stage adjusting groove (531) is provided with a fixing threaded hole, and the sample stage adjusting groove (531) is fixedly contacted with the tail end face of the sample stage (51).
7. The apparatus for detecting a solid material component by laser light according to claim 6, wherein: the novel optical fiber laser is characterized in that a quartz observation window (41) and a three-way gas pipeline (42) are arranged on the left packaging sleeve (4), a quick clamping mechanism (45) is arranged on a connecting flange of the left packaging sleeve (4) and the drawing sample bin (5), two positioning pins (411), a fixing pin hole 412 and a flange locking groove (414) are arranged on the connecting flange of the left packaging sleeve (4) and the drawing sample bin (5), two optical fiber leading-out holes (31) are formed in the right packaging sleeve (3), a protective gas channel (33) is arranged on the right packaging sleeve (3) and the connecting flange of the laser (1), and the two optical fiber leading-out holes (31) are respectively led out by an optical fiber (8) with a coaxial optical path and an optical fiber with a non-coaxial optical path.
8. The apparatus for detecting a solid material component by laser light according to claim 7, wherein: quick clamping mechanism (45) are including smooth round pin (451), fixed slider (452), compression spring (453), compression spring base (454) and handle (455) of screwing, and quick clamping mechanism (45) are installed in flange locking groove (414) of left encapsulation sleeve (4) through fixed round pin axle (413) connection, open on smooth round pin (451) have U type groove and connecting hole, and fixed slider (452) are fixed on smooth round pin (451) through U type groove, and the connecting hole is connected with fixed round pin axle (413), is equipped with the screw thread on the smooth round pin axle, cooperates with the screw hole in handle (455) of screwing.
9. A method for detecting a solid material component using the apparatus for detecting a solid material component according to any one of claims 1 to 8, characterized in that it is carried out by the steps of:
a. selecting a proper light path system: selecting a coaxial light path or a non-coaxial light path;
b. an incidence lens (24) with a proper focal length and a fixed Jiao Bujian (23) with a proper length are selected to finish the installation of the front light path unit (2);
c. after the optical fiber combination is installed, the optical fiber (8) is led out from an optical fiber leading-out hole (31) on the right packaging sleeve (3);
d. installing a sample to be tested in the drawing type sample bin (5), and fixing a base flange (53) and a left packaging sleeve (4) by using a quick clamping mechanism (45);
e. starting a laser (1), firstly setting lower pulse energy and frequency, observing the position of a laser focus through a quartz observation window (41), and finely adjusting a sample stage (51) to enable the laser focus to be converged on the surface of a sample;
f. after the adjustment of the sample position is completed, a spectrometer (9) is started, and parameters of the laser (1) are adjusted according to experimental requirements: pulse energy and frequency, performing spectrum measurement of a series of samples with known contents, and then measuring the spectrum of an unknown sample;
g. the components of the detected element are analyzed by the spectrum obtained by the test.
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| CN110186889A (en) * | 2019-06-03 | 2019-08-30 | 常州星宇车灯股份有限公司 | Laser remote excitation test device and its test method |
| CN113740361B (en) * | 2020-05-29 | 2023-05-23 | 清华大学 | Detection channel, channel assembly and CT detection device |
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