CN116559146A - Device for improving detection stability and expansibility of multi-matrix spark direct-reading spectrometer - Google Patents
Device for improving detection stability and expansibility of multi-matrix spark direct-reading spectrometer Download PDFInfo
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- CN116559146A CN116559146A CN202310837061.2A CN202310837061A CN116559146A CN 116559146 A CN116559146 A CN 116559146A CN 202310837061 A CN202310837061 A CN 202310837061A CN 116559146 A CN116559146 A CN 116559146A
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- 239000011159 matrix material Substances 0.000 title claims abstract description 32
- 238000001514 detection method Methods 0.000 title claims abstract description 31
- 230000005284 excitation Effects 0.000 claims abstract description 50
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 28
- 239000010937 tungsten Substances 0.000 claims abstract description 28
- 238000010892 electric spark Methods 0.000 claims description 43
- 238000012360 testing method Methods 0.000 claims description 37
- 239000013307 optical fiber Substances 0.000 claims description 34
- 230000003287 optical effect Effects 0.000 claims description 31
- 238000000295 emission spectrum Methods 0.000 claims description 19
- 238000013461 design Methods 0.000 claims description 12
- 229910052744 lithium Inorganic materials 0.000 claims description 12
- 229910052708 sodium Inorganic materials 0.000 claims description 12
- 230000000630 rising effect Effects 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 claims description 3
- 230000005855 radiation Effects 0.000 claims description 3
- 238000001444 catalytic combustion detection Methods 0.000 description 24
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 22
- 239000011734 sodium Substances 0.000 description 13
- 229910052742 iron Inorganic materials 0.000 description 10
- 229910052782 aluminium Inorganic materials 0.000 description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 230000003595 spectral effect Effects 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 229910000838 Al alloy Inorganic materials 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910001018 Cast iron Inorganic materials 0.000 description 2
- 238000001636 atomic emission spectroscopy Methods 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 125000004436 sodium atom Chemical group 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- KCZFLPPCFOHPNI-UHFFFAOYSA-N alumane;iron Chemical compound [AlH3].[Fe] KCZFLPPCFOHPNI-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
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- 239000000428 dust Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
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- 238000004445 quantitative analysis Methods 0.000 description 1
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- 239000000126 substance Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 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
- 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
- G01N21/66—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence
- G01N21/67—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence using electric arcs or discharges
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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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
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Abstract
The invention relates to a device for improving the detection stability and expansibility of a multi-matrix spark direct-reading spectrometer, which comprises an excitation table, wherein an excitation hole is formed in a workbench of the excitation table, a tungsten needle is connected in the excitation table, the tungsten needle is positioned right below the excitation hole, meanwhile, the tungsten needle is lower than the workbench of the excitation table, the rear side surface of the excitation table is communicated with a Rowland round light chamber through a light passing hole, a front inclined hole, a left inclined hole and a right inclined hole are respectively formed in the front surface, the left side surface and the right side surface of the excitation table, an ARM processor is used for accurately controlling voltage pulse of the tungsten needle spark, CCD acquisition in a Rowland round light chamber and CCD acquisition of four micro spectrometers, and the ARM processor is electrically connected with the excitation table micro spectrometers, wherein the time sequence errors of the voltage pulse of the spark, the CCD acquisition in the Rowland round light chamber are smaller than 10ns. The invention can improve the detection stability and the capability of detecting wave bands.
Description
Technical Field
The invention belongs to the technical field of measuring devices, and particularly relates to a device for improving the detection stability and expansibility of a multi-matrix spark direct-reading spectrometer.
Background
Among the analysis methods for metal materials, an atomic emission spectrometry is the most convenient and rapid analysis method, and a spark direct-reading spectrometry instrument based on an atomic emission spectrometry technology is the most commonly used instrument in the field of material analysis. A photoelectric direct-reading spectrometer performs a qualitative and quantitative analysis on the composition of a substance by receiving characteristic wavelengths emitted from atoms in an excited state through a photoelectric conversion device (PMT or CCD). The requirements on the test precision and stability of the metal materials are higher and higher in the fields of high-end equipment manufacturing, aerospace industry, nuclear industry and the like in China.
At present, the light passing hole of the excitation bench can only be used for taking light towards one side of the electric spark, the electric spark is in a divergent spherical shape, the electric spark in the excitation process is affected in multiple aspects, the argon flow, the excitation dust and the tungsten needle height can all influence the stability of the electric spark, and the single-side light taking is easy to cause data instability. If the data can be averaged by taking light from four sides of the electric spark, the stability of the test can be greatly improved.
For multi-matrix test instruments, the position of the via can only be treated as compromise as possible. The main reason is that the wavelength distribution of the electric spark excited is uneven, the light of the upper part of the electric spark is biased to the ultraviolet short wave band, the light of the lower part of the electric spark is biased to the infrared long wave band, and the light of the middle part is positioned between the two parts, as shown in fig. 1.
Light emitted by the electric spark passes through the light passing hole, then passes through the focusing mirror and the slit, then is beaten on the grating, and is received by CCDs at different positions after being diffracted by the grating. The size of the light passing hole cannot be too large, which can cause the receiving of very much stray light, affecting the overall resolution. The size of the through-hole is generally smaller than the overall size of the spark. According to debugging experience, when an instrument of the steel matrix is debugged, the through-hole tends to deviate to the upper edge of an electric spark, because the emission wavelength of nonmetallic elements such as C, P, S in steel deviates to an ultraviolet band, and meanwhile, the nonmetallic elements are core elements for steel detection; when the instrument of the aluminum matrix is debugged, the light-taking hole is deviated to the lower edge of the electric spark, and the emission spectrum of the aluminum matrix core element is deviated to long waves, so that the effective signals of short waves are few. However, if debugging is carried out on a multi-matrix instrument (an iron-aluminum double matrix), only compromise treatment is often carried out, and a light taking hole faces to the middle part of an electric spark, but the capability of the whole machine for testing the iron-based short wave element (C, P, S) and the capability of the aluminum-based long wave element (Zn, si and Cu) are often sacrificed.
Limited by the miniaturization requirement of the direct-reading spectrometer, the current Roland round optical room cannot be made very large, the limit wavelength of the received spectrum signal of the general direct-reading spectrometer on the market is about 500nm, so that the emission signals of elements such as Li element (670.7 nm) and Na element (589.6 nm) in some long wave bands are not received, and the detection of the two elements becomes the focus of the application and development of the direct-reading spectrometer along with the increasing proportion of lithium batteries and sodium batteries in the domestic energy storage field.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a device for improving the detection stability and expansibility of a multi-matrix spark direct-reading spectrometer.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the device for improving the detection stability and expansibility of the multi-matrix spark direct-reading spectrometer comprises an excitation table, wherein an excitation hole is formed in a workbench of the excitation table, a tungsten needle is connected in the excitation table and positioned right below the excitation hole, meanwhile, the tungsten needle is lower than the workbench of the excitation table, the rear side surface of the excitation table is communicated with a Rowland round light chamber through a light passing hole, a front inclined hole, a left inclined hole and a right inclined hole are respectively formed in the front surface, the left side surface and the right side surface of the excitation table, and are communicated to the excitation hole,
one end of the inner side of the front inclined hole is aligned with the lower edge position of the tungsten needle, so that the tungsten needle can receive the emission spectrum of the lower edge of the electric spark, a biconvex lens is embedded at the other end of the front inclined hole, a third optical fiber connecting seat is connected to the outer end of the other side of the front inclined hole, and the third optical fiber connecting seat is respectively connected with a third micro spectrometer for receiving long wave bands and a fourth micro spectrometer for testing Li and Na elements through a third optical fiber and a fourth optical fiber;
one end of the inner side of the left inclined hole is aligned with the lower edge position of the polar plate of the excitation table, so that the polar plate can receive the emission spectrum of the uppermost edge of the electric spark, a biconvex lens is embedded at the other end of the left inclined hole, a first optical fiber connecting seat is connected with the outer end of the other side of the left inclined hole, and the first optical fiber connecting seat is connected with a first micro spectrometer for receiving ultraviolet bands through first light rays;
one end of the inner side of the right side inclined hole is aligned to the middle position of the tungsten needle and the polar plate, so that the tungsten needle and the polar plate can receive the emission spectrum of the middle part of the electric spark, a biconvex lens is embedded at the other end of the right side inclined hole, a second optical fiber connecting seat is connected to the outer end of the other side of the right side inclined hole, and the second optical fiber connecting seat is connected with a second micro spectrometer for receiving wave bands through second light rays;
the ARM processor is used for accurately controlling voltage pulse of electric spark of the tungsten needle, CCD acquisition in the Rowland circle light chamber and CCD acquisition of the four micro spectrometers, and is electrically connected with the excitation bench micro spectrometers, wherein time sequence errors of the voltage pulse of the electric spark, the CCD acquisition in the Rowland circle light chamber and the CCD acquisition of the four micro spectrometers are smaller than 10ns.
Preferably, the device for improving the stability and expansibility of the multi-matrix spark direct-reading spectrometer is characterized in that the first micro spectrometer is responsible for receiving an emission spectrum of the upper edge of the electric spark, and the set parameters are as follows:
reception wavelength: 185-250nm;
CCD pixel: 3648pixels;
optical resolution: 0.1nmFWHM;
optical design: f/4, symmetrically crossing the Czerny-Turner light path.
Preferably, the device for improving the stability and expansibility of the multi-matrix spark direct-reading spectrometer is characterized in that the second micro spectrometer is responsible for receiving the emission spectrum of the middle part of the electric spark, and the set parameters are as follows:
reception wavelength: 250-370nm;
CCD pixel: 3648pixels;
optical resolution: 0.1nmFWHM;
optical design: f/4, symmetrically crossing the Czerny-Turner light path.
Preferably, the device for improving the stability and expansibility of the multi-matrix spark direct-reading spectrometer is characterized in that the third micro spectrometer is responsible for receiving the emission spectrum of the lowest edge of the electric spark, and the set parameters are as follows:
reception wavelength: 370-500m;
CCD pixel: 3648pixels;
optical resolution: 0.1nmFWHM;
optical design: f/4, symmetrically crossing the Czerny-Turner light path.
Preferably, the device for improving the stability and expansibility of the multi-matrix spark direct-reading spectrometer is characterized in that the fourth micro spectrometer is responsible for testing Li and Na elements, and the set parameters are as follows:
reception wavelength: 580-680m;
CCD pixel: 3648pixels;
optical resolution: 0.12nmFWHM;
optical design: f/4, symmetrically crossing the Czerny-Turner light path.
Preferably, the device for improving the detection stability and expansibility of the multi-matrix spark direct-reading spectrometer is characterized in that the apertures of the front inclined hole, the left inclined hole and the right inclined hole are 6mm, and meanwhile, the diameter of the biconvex lens is 6mm and the focal length is 6mm.
Preferably, the device for improving the detection stability and expansibility of the multi-matrix spark direct-reading spectrometer adopts an ultraviolet radiation resistant optical fiber, and the transmission wavelength range of the optical fiber is 185-1100nm.
Preferably, the device for improving the detection stability and expansibility of the multi-matrix spark direct-reading spectrometer starts from the rising edge of square wave voltage, and the acquisition time sequence error is controlled within 10ns.
By means of the scheme, the invention has at least the following advantages:
1. according to the invention, the excitation tables of the spectrum intensities of the upper edge, the middle part and the lower edge of the electric spark can be synchronously detected through the micro spectrometer, and the detection stability is improved and the capability of detecting the whole wave band is enhanced by distributing different weights to different matrixes.
2. The fourth micro spectrometer can ensure that the emission signal of the Li element and the emission signal of the Na element are received, and the detection range of the direct-reading spectrometer is widened.
3. The invention can accurately control the voltage pulse of electric spark, the CCD acquisition in the Rowland round light chamber and the CCD acquisition of a plurality of micro spectrometers by the Arm processor with the performance, and the time sequence error of the three is controlled within 10ns. And can restore the spectrum intensity of the electric spark at 3 different positions (upper edge, middle part and lower edge) at the same moment as far as possible. Meanwhile, each acquisition is started from the rising edge of the square wave voltage, the acquisition time sequence error is controlled within 10ns, and the influence on data acquired at different time sequences of the voltage square wave signal is eliminated.
The foregoing description is only an overview of the present invention, and is intended to provide a better understanding of the present invention, as it is embodied in the following description, with reference to the preferred embodiments of the present invention and the accompanying drawings.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of an electrical spark at the tip of a tungsten needle in accordance with the present invention;
FIG. 2 is a schematic diagram of the structure of the present invention;
FIG. 3 is a schematic view of the partial connection structure of FIG. 2;
FIG. 4 is a schematic view of the structure of the excitation stage of the present invention;
FIG. 5 is a cross-sectional view of an angled hole directly in front of an excitation stand according to the present invention;
FIG. 6 is a cross-sectional view of a left and right side angled hole of the excitation stand of the present invention;
FIG. 7 is a graph of the intensity at 193nm collected by the Roland circle light chamber of the present invention;
FIG. 8 is a graph of light intensity at 193nm acquired by a first micro-spectrometer of the present invention;
FIG. 9 is a graph of light intensity after the wavelength is measured by the weighted spectrometer of FIG. 8;
FIG. 10 is a graph of the intensity at 481.06nm collected by the Roland circle light chamber of the present invention;
FIG. 11 is a graph of light intensity after the wavelength is measured by the spectrometer after weighting in FIG. 10;
FIG. 12 is a graph of the intensity of Na atoms according to the present invention.
Detailed Description
For the purposes of making the objects, technical solutions and advantages of the embodiments of the present application more clear, the technical solutions of the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is apparent that the described embodiments are some embodiments of the present application, but not all embodiments. The components of the embodiments of the present application, which are generally described and illustrated in the figures herein, may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present application, as provided in the accompanying drawings, is not intended to limit the scope of the application, as claimed, but is merely representative of selected embodiments of the application. All other embodiments, which can be made by one of ordinary skill in the art based on the embodiments herein without making any inventive effort, are intended to be within the scope of the present application.
Examples
As shown in fig. 2 to 6, the device for improving the detection stability and expansibility of the multi-matrix spark direct-reading spectrometer comprises an excitation table 12, wherein an excitation hole 20 is formed in a workbench of the excitation table 12, a tungsten needle 19 is connected in the excitation table 12, the tungsten needle 19 is positioned right below the excitation hole 20, meanwhile, the tungsten needle 19 is lower than the workbench of the excitation table 12, the rear side surface of the excitation table 12 is communicated with a rowland round light chamber 17 through a light passing hole 18, a front inclined hole 3, a left inclined hole 1 and a right inclined hole 2 are respectively formed in the front, left and right sides of the excitation table 12, and are all communicated to the excitation hole 20,
one end of the inner side of the front inclined hole 3 is aligned to the lower edge position of the tungsten needle 19, so that the tungsten needle can receive the emission spectrum of the lower edge of an electric spark, a biconvex lens 13 is embedded at the other end of the front inclined hole 3, a third optical fiber connecting seat 16 is connected to the outer end of the other side of the front inclined hole 3, and the third optical fiber connecting seat 16 is respectively connected with a third micro spectrometer 10 for receiving long wave bands and a fourth micro spectrometer 11 for testing Li and Na elements through a third optical fiber 6 and a fourth optical fiber 7;
one end of the inner side of the left inclined hole 1 is aligned with the upper edge position of the polar plate of the excitation table 12, so that the upper edge position of the polar plate can receive the emission spectrum of the uppermost edge of the electric spark, a biconvex lens 13 is embedded at the other end of the left inclined hole 1, a first optical fiber connecting seat 14 is connected to the outer end of the other side of the left inclined hole 1, and the first optical fiber connecting seat 14 is connected with a first micro spectrometer 8 for receiving ultraviolet wave bands through first light rays 4;
one end of the inner side of the right side inclined hole 2 is aligned to the middle position of the tungsten needle 19 and the polar plate, so that the tungsten needle can receive the emission spectrum of the middle part of the electric spark, the other end of the right side inclined hole 2 is embedded with a biconvex lens 13, the outer end of the other side of the right side inclined hole 2 is connected with a second optical fiber connecting seat 15, and the second optical fiber connecting seat 15 is connected with a second micro spectrometer 9 for receiving wave bands through second light rays 5;
the ARM processor is used for accurately controlling voltage pulse of electric spark of the tungsten needle, CCD collection in the Rowland round optical chamber 17 and CCD collection of the four micro spectrometers, and is electrically connected with the excitation table 12 micro spectrometers, wherein time sequence errors of the voltage pulse of the electric spark, the CCD collection in the Rowland round optical chamber 17 and the CCD collection of the four micro spectrometers are smaller than 10ns.
The first micro spectrometer 8 is responsible for receiving the emission spectrum of the upper edge of the electric spark, and the set parameters are as follows:
reception wavelength: 185-250nm;
CCD pixel: 3648pixels;
optical resolution: 0.1nmFWHM;
optical design: f/4, symmetrically crossing the Czerny-Turner light path.
In the present invention, the second micro spectrometer 9 is responsible for receiving the emission spectrum of the middle part of the electric spark, and the set parameters are as follows:
reception wavelength: 250-370nm;
CCD pixel: 3648pixels (pixels);
optical resolution: 0.1nmFWHM;
optical design: f/4, symmetrically crossing the Czerny-Turner light path.
The third micro spectrometer 10 in the present invention is responsible for receiving the emission spectrum of the lowest edge of the electric spark, and its set parameters are:
reception wavelength: 370-500m;
CCD pixel: 3648pixels;
optical resolution: 0.1nmFWHM;
optical design: f/4, symmetrically crossing the Czerny-Turner light path.
The fourth micro spectrometer 11 in the invention is responsible for testing Li and Na elements, and the set parameters are as follows:
reception wavelength: 580-680m;
CCD pixel: 3648pixels;
optical resolution: 0.12nmFWHM;
optical design: f/4, symmetrically crossing the Czerny-Turner light path.
The apertures of the front inclined hole 3, the left inclined hole 1 and the right inclined hole 2 are 6mm, and the diameter of the lenticular lens 13 is 6mm and the focal length is 6mm.
The optical fiber adopts the ultraviolet radiation resistant optical fiber, and the transmission wavelength range of the optical fiber is 185-1100nm.
In the invention, each acquisition starts from the rising edge of the square wave voltage, the acquisition time sequence error is controlled within 10ns, and the influence on data acquired at different time sequences of the voltage square wave signal can be eliminated.
Under the condition that the testing of Li and Na long wave elements is not considered, the light intensity values tested at present are 4 types, namely the light intensity value I1 collected by a CCD in a traditional Rowland round light chamber, the light intensity value I2 which is received by a first micro spectrometer at the left side and is deviated from an ultraviolet band, the light intensity value I3 which is received by a second micro spectrometer at the right side and is deviated from a normal band, and the light intensity value I4 which is received by a third micro spectrometer at the right front and is deviated from an infrared band.
The weight of the light intensity value collected by the CCD in the conventional rowland circle light chamber 17 is set to a, the weight of the light intensity value received by the first micro-spectrometer at the left side is set to b, the weight of the light intensity value received by the second micro-spectrometer at the right side is set to c, and the weight of the light intensity value received by the third micro-spectrometer at the right front is set to d, wherein a+b+c+d=1.
For the element intensity value of specific wavelength, the device structure can obtain 4 different light intensity values, and the element concentration value calculated by the intensity value needs to be unique, so that the data needs to be normalized, and the final light intensity Is obtained by multiplying I1, I2, I3 and I4 with the corresponding weight coefficients a, b, c, d and then summing the multiplied light intensity Is:
Is= a×I1+b×I2+c×I3+d×I4；
the specific weight value of a, b, c, d in the formula is obtained by analysis according to an experimental result, and the data weight of a is generally about 0.5 because the focal length of the optical chamber is larger, the data reliability is relatively higher and the data weight of the optical chamber 17 is always higher; when the wavelength of the element is measured to be biased to the ultraviolet region, the weight value of b is often higher; when the wavelength of the element is measured to be biased to the infrared region, the weight value of d is always higher; when the measured element wavelength is between ultraviolet and infrared, the weights of c and a are often high.
According to different matrixes tested, different weight values are determined:
for the iron-based metal test, the wave length of the iron-based metal is biased to ultraviolet short wave within 250nm, and the test result is optimal when a is 0.5, b is 0.35, c is 0.1, and d is 0.05;
for the iron-based metal test, the test results are best when the wave band of 250nm-370nm is tested to obtain a of 0.6, b of 0.05, c of 0.25 and d of 0.1;
for the iron-based metal test, the test results are best when the wave band of 370nm-500nm is tested to obtain a of 0.5, b of 0.05, c of 0.1 and d of 0.35;
for aluminum-based metal test, when the deflection ultraviolet short wave length within 250nm is obtained after the test, a is 0.6, b is 0.2, c is 0.1, and d is 0.1, the test effect is optimal;
for aluminum-based metal test, the test results are best when the wave band of 250nm-370nm is tested to obtain a of 0.6, b of 0.1, c of 0.2 and d of 0.1;
for aluminum-based metal test, the test results are best when the wave band of 370nm-500nm is obtained after test, a is 0.6, b is 0.05, c is 0.05, and d is 0.3.
The capability and test stability of a double-matrix instrument or a multi-matrix instrument in short wave and long wave bands can be improved by plotting the weighted light intensity value I against the element concentration.
When the requirements of the Li and Na long wave elements are tested, the fourth optical fiber head in front of the device can be connected with the fourth miniature spectrometer 11 specially used for testing the Li and Na elements, so that the test of the Li and Na elements is realized, the miniature spectrometer can be customized according to the requirements, and the testing range of the spark direct-reading spectrometer is expanded.
Example 1
The test of the C element is always the difficulty and the key point of the test of the stainless steel in the iron base, the content of the C element in the stainless steel is particularly low, the C element is easily interfered by the spectra at the adjacent positions, and in the actual debugging process, the test C element (193.09 nm) of the multi-matrix direct-reading spectrometer is often interfered by the emission lines (193.03 nm and 193.14 nm) of two Fe elements at the adjacent positions. The multi-matrix direct-reading spectrometer weakens the capability of short wave detection because the light extraction position faces the middle of the electric spark flame, when the sample block is tested 316, before the weighted light intensity is not used, the CCD in the Rowland round light chamber 17 collects the light intensity which deviates to the middle of the electric spark, and the light intensity at 193nm is shown in fig. 7, so that the interference of iron peaks (193.03 nm and 193.14 nm) on the two sides on the stability of the C peak is very large, and the main reason is that the light extraction position deviates to the middle.
While the light intensity at 193nm, which is received by the first micro-spectrometer 8 at the left side and biased toward the upper edge of the spark, is shown in fig. 8, when the light extraction position is only aligned with the upper edge of the spark, the two interference peaks of iron completely disappear, and the spectral intensity of the C element is very stable.
Meanwhile, when the intensities measured by other spectrometers are weighted, as shown in fig. 9, it can be found that the interference of the weighted Fe peak to the C peak is significantly reduced and the stability of the C peak is significantly enhanced.
Stainless steel 316L sample block
The data were tested prior to use and are shown in table 1.
TABLE 1
The data are tested after use and are shown in table 2.
TABLE 2
As can be seen from table 2, the stability and accuracy of the data measured using the weighted spectral intensity values are significantly improved.
For cast iron, the iron content is higher, the interference of iron peaks on two sides to carbon peaks is larger, the test effect of C is poor before the weighted light intensity is not used, but the test effect is obviously improved after the weighted light intensity is used.
Cast iron RG14
The data were tested prior to use and are shown in table 3.
TABLE 3 Table 3
The data are tested after use and are shown in table 4.
TABLE 4 Table 4
Example two
For aluminum substrates, zn element is the key point of detection, the emission wavelength of Zn is longer, a 481.06nm spectral line is generally selected, and the multi-substrate direct-reading spectrometer weakens the capability of long-wave detection due to the fact that the light-taking position faces the middle of electric spark flame, before the weighted light intensity is not used, the CCD in the Rolland round light chamber 17 collects the light intensity of electric spark deflected to the middle, and the light intensity is at 481.06nm, as shown in fig. 10.
When the wavelengths measured by other spectrometers are weighted, the weighted intensities, as shown in fig. 11, can be found that the stability of the intensity of the Zn element emission after weighting is significantly enhanced.
Aluminum alloy EE411h sample block
The data were tested prior to use and are shown in table 5.
TABLE 5
The data were tested after use and are shown in table 6.
TABLE 6
The data obtained by the Zn element test can be found to be greatly improved in stability and accuracy compared with the prior art from the table 6, and the capability of the multi-matrix direct-reading spectrometer in short-and-short-wave detection can be remarkably improved.
In addition, the fourth optical fiber 7 of the front inclined hole can be connected with a fourth micro spectrometer 11 for testing Li and Na elements, so that the detection range of the direct-reading spectrometer can be expanded, and the spectrometer is used for receiving the emission signal of Na atoms, as shown in fig. 12.
Aluminum alloy AA NA-15 set of standard sample block
TABLE 7
From the above table 7, it is seen that the accuracy and stability of the detection data of Na element meet the standards, and the detection range of the direct-reading spectrometer can be expanded by adopting the fourth micro spectrometer, and meanwhile, the micro spectrometer can be flexibly customized according to the requirements of clients.
In tables 1 to 7 above, wherein RSD is relative standard deviation, 1, 2, 3 … 8 are actual element detection contents; meanwhile, fig. 7 to 12 are only schematic diagrams of light intensity for different test sample blocks, and are only references for table detection data.
It should be noted that: like reference numerals and letters denote like items in the following figures, and thus once an item is defined in one figure, no further definition or explanation thereof is necessary in the following figures.
In the description of the present application, it should be noted that, the terms "vertical," "horizontal," "inner," "outer," and the like indicate an azimuth or a positional relationship based on the azimuth or the positional relationship shown in the drawings, or an azimuth or the positional relationship that the product of the application is conventionally put in use, merely for convenience of description and simplification of the description, and do not indicate or imply that the apparatus or element to be referred to must have a specific azimuth, be configured and operated in a specific azimuth, and therefore should not be construed as limiting the present application. Furthermore, the terms "first," "second," and the like, are used merely to distinguish between descriptions and should not be construed as indicating or implying relative importance.
Furthermore, the terms "horizontal," "vertical," and the like do not denote a requirement that the component be absolutely horizontal or vertical, but rather may be slightly inclined. As "horizontal" merely means that its direction is more horizontal than "vertical", and does not mean that the structure must be perfectly horizontal, but may be slightly inclined.
In the description of the present application, it should also be noted that, unless explicitly specified and limited otherwise, the terms "disposed," "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the terms in this application will be understood by those of ordinary skill in the art in a specific context.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, and it should be noted that it is possible for those skilled in the art to make several improvements and modifications without departing from the technical principle of the present invention, and these improvements and modifications should also be regarded as the protection scope of the present invention.
Claims (8)
1. Promote many base members spark direct-reading spectrometer and detect device of stability and expansibility, including excitation platform (12), excitation hole (20) have been seted up on the workstation of excitation platform (12), excitation platform (12) interconnect has tungsten needle (19), tungsten needle (19) are located the workstation of excitation platform (12) under excitation hole (20), simultaneously tungsten needle (19) are less than excitation platform (12), and the trailing flank of excitation platform (12) is linked together its characterized in that with rowland circle light room (17) through light passing hole (18): the front, left side and right side of the excitation table (12) are respectively provided with a front inclined hole (3), a left side inclined hole (1) and a right side inclined hole (2), which are communicated with the excitation hole (20),
one end of the inner side of the front inclined hole (3) is aligned with the lower edge position of the tungsten needle (19) so that the front inclined hole can receive an emission spectrum of the lower edge of an electric spark, a biconvex lens (13) is embedded in the other end of the front inclined hole (3), a third optical fiber connecting seat (16) is connected to the outer end of the other side of the front inclined hole (3), and the third optical fiber connecting seat (16) is respectively connected with a third micro spectrometer (10) for receiving long wave bands and a fourth micro spectrometer (11) for testing Li and Na elements through a third optical fiber (6) and a fourth optical fiber (7);
one end of the inner side of the left inclined hole (1) is aligned with the lower edge position of a polar plate of the excitation table (12) so that the polar plate can receive the emission spectrum of the uppermost edge of an electric spark, a biconvex lens (13) is embedded in the other end of the left inclined hole (1), a first optical fiber connecting seat (14) is connected to the outer end of the other side of the left inclined hole (1), and the first optical fiber connecting seat (14) is connected with a first micro spectrometer (8) for receiving ultraviolet bands through first light rays (4);
one end of the inner side of the right side inclined hole (2) is aligned to the middle position of the tungsten needle (19) and the polar plate, so that the tungsten needle can receive the emission spectrum of the middle part of an electric spark, a biconvex lens (13) is embedded into the other end of the right side inclined hole (2), a second optical fiber connecting seat (15) is connected to the outer end of the other side of the right side inclined hole (2), and the second optical fiber connecting seat (15) is connected with a second micro spectrometer (9) for receiving wave bands through second light rays (5);
the ARM processor is used for accurately controlling voltage pulse of electric spark of the tungsten needle, CCD collection in the Rowland round optical chamber (17) and CCD collection of the four micro spectrometers, and is electrically connected with the excitation table (12) micro spectrometers, wherein time sequence errors of the voltage pulse of the electric spark, CCD collection in the Rowland round optical chamber (17) and CCD collection of the four micro spectrometers are smaller than 10ns.
2. The device for improving the detection stability and expansibility of a multi-matrix spark direct-reading spectrometer according to claim 1, wherein: the first micro spectrometer (8) is responsible for receiving an emission spectrum of the upper edge of the electric spark, and the set parameters are as follows:
reception wavelength: 185-250nm;
CCD pixel: 3648pixels;
optical resolution: 0.1nmFWHM;
optical design: f/4, symmetrically crossing the Czerny-Turner light path.
3. The device for improving the detection stability and expansibility of a multi-matrix spark direct-reading spectrometer according to claim 1, wherein: the second micro spectrometer (9) is responsible for receiving an emission spectrum of the middle part of the electric spark, and the set parameters are as follows:
reception wavelength: 250-370nm;
CCD pixel: 3648pixels;
optical resolution: 0.1nmFWHM;
optical design: f/4, symmetrically crossing the Czerny-Turner light path.
4. The device for improving the detection stability and expansibility of a multi-matrix spark direct-reading spectrometer according to claim 1, wherein: the third micro spectrometer (10) is responsible for receiving the emission spectrum of the lowest edge of the electric spark, and the set parameters are as follows:
reception wavelength: 370-500m;
CCD pixel: 3648pixels;
optical resolution: 0.1nmFWHM;
optical design: f/4, symmetrically crossing the Czerny-Turner light path.
5. The device for improving the detection stability and expansibility of a multi-matrix spark direct-reading spectrometer according to claim 1, wherein: the fourth micro spectrometer (11) is responsible for testing Li and Na elements, and the set parameters are as follows:
reception wavelength: 580-680m;
CCD pixel: 3648pixels;
optical resolution: 0.12nmFWHM;
optical design: f/4, symmetrically crossing the Czerny-Turner light path.
6. The device for improving the detection stability and expansibility of a multi-matrix spark direct-reading spectrometer according to claim 1, wherein: the apertures of the front inclined hole (3), the left inclined hole (1) and the right inclined hole (2) are 6mm, and meanwhile, the diameter of the biconvex lens (13) is 6mm and the focal length is 6mm.
7. The apparatus for improving the detection stability and expansibility of a multi-matrix spark direct-reading spectrometer according to any one of claims 1 to 6, wherein: the optical fiber adopts an ultraviolet radiation resistant optical fiber, and the transmission wavelength range of the optical fiber is 185-1100nm.
8. The device for improving the detection stability and expansibility of a multi-matrix spark direct-reading spectrometer of claim 7, wherein: each acquisition starts from the rising edge of the square wave voltage, and the acquisition time sequence error is controlled within 10ns.
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Denomination of invention: A device for improving the detection stability and scalability of multi substrate spark direct reading spectrometer Granted publication date: 20230919 Pledgee: Jiangsu Taicang Rural Commercial Bank Co.,Ltd. Xinmao Branch Pledgor: Jiangsu Aowen Instrument Technology Co.,Ltd. Registration number: Y2024980005091 |