CN1160552C - In-situ metal analyzer - Google Patents
In-situ metal analyzer Download PDFInfo
- Publication number
- CN1160552C CN1160552C CNB021162948A CN02116294A CN1160552C CN 1160552 C CN1160552 C CN 1160552C CN B021162948 A CNB021162948 A CN B021162948A CN 02116294 A CN02116294 A CN 02116294A CN 1160552 C CN1160552 C CN 1160552C
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- Prior art keywords
- spark
- high speed
- links
- speed acquisition
- slit
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- Expired - Lifetime
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- 238000011065 in-situ storage Methods 0.000 title claims abstract description 9
- 239000002184 metal Substances 0.000 title claims abstract description 9
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 9
- 238000004458 analytical method Methods 0.000 claims abstract description 30
- 238000001228 spectrum Methods 0.000 claims abstract description 16
- 230000001360 synchronised effect Effects 0.000 claims abstract description 14
- 230000005284 excitation Effects 0.000 claims abstract description 12
- 238000013019 agitation Methods 0.000 claims description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 230000003595 spectral effect Effects 0.000 claims description 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 5
- 229910052721 tungsten Inorganic materials 0.000 claims description 5
- 239000010937 tungsten Substances 0.000 claims description 5
- 230000003321 amplification Effects 0.000 claims description 4
- 238000003199 nucleic acid amplification method Methods 0.000 claims description 4
- 239000000126 substance Substances 0.000 abstract description 11
- 238000009826 distribution Methods 0.000 abstract description 10
- 239000000203 mixture Substances 0.000 abstract description 10
- 239000007769 metal material Substances 0.000 abstract description 4
- 238000007599 discharging Methods 0.000 abstract 2
- 238000010252 digital analysis Methods 0.000 abstract 1
- 238000005204 segregation Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 5
- 239000011800 void material Substances 0.000 description 5
- 238000000034 method Methods 0.000 description 4
- 239000012769 display material Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000005275 alloying Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000004452 microanalysis Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 235000021110 pickles Nutrition 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000012113 quantitative test Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Classifications
-
- 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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- Health & Medical Sciences (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The present invention relates to the field of the chemical analysis of metal material. An in-situ metal analyzer is composed of an excitation light source system, a light splitting system, a single spark discharging high-speed collecting system, a spark spectrum single discharging digital analysis system and a continuous excitation synchronous scanning and positioning system. The present invention uses synchronous scanning samples to realize sample continuous movement and continuous spark discharge. By light splitting and collection, real time recording is realized in a digital mode. By statistic analysis, the analysis of the chemical composition, the element distribution, the porosity and the inclusion distribution of the samples is carried out, and results are accurate and general.
Description
Technical field
The invention belongs to the field of coming analysis of material by the physical property of measuring material, relate generally to the chemical composition analysis field of metal material.
Background technology
The content of chemical constitution, component segregation, surface imperfection, snotter is most important four contents of quality control in the Iron and Steel Production.In the prior art, adopt sufur printing to test and check segregation or the distribution of alloying element in steel, come the inspection center loose with pickle test, adopt metallographic method check snotter kind, pattern, size and distribution, above-mentioned operated in accordance with conventional methods is cumbersome, analysis speed is slow, required time is long, simultaneously can't quantification (" optical micro analysis " P21-40, Sun Yeying work, publishing house of Tsing-Hua University, in October, 1996).
In the prior art, the spark source Atomic Emission Spectrometer AES can carry out the chemical composition analysis in the material, but can only obtain each element average content, can't carry out the distributional analysis of composition, more can't carry out degree of segregation, fraction void, snotter quantitative test.Trace it to its cause, mainly be that present spark source Atomic Emission Spectrometer AES exists following three major technique defectives: one, static state excites.Keep sample to fix in the analytic process, just excite the spot of a 5mm diameter of fusion at every turn, for static state excites, can not write down the position of impulse discharge, thereby can't carry out the distributional analysis of element and snotter; Two, integrated detected mode.The object of gathering is the integral voltage of several thousand discharge pulses, can't discern each spark character, thereby can't resolve the chemical information of containing in the single spark discharge; Three, high energy pre-burning.Through 20 to 30 seconds pre-burning, most of snotter was heavily melted, thereby can't observe the unusual spark of those reflection snotter information.
Summary of the invention
The object of the present invention is to provide that a kind of chemical constitution that can quick and precisely directly measure metal material, elemental composition distribute, the in-situ metal analyzer of snotter distribution and degree of segregation, fraction void.
Based on above-mentioned purpose, main technical schemes of the present invention is to utilize synchronous scanning platform clamped sample, realize the spark discharge of continuous mobile excited sample, by beam split, by the line strength and the position of the each discharge spark of high-speed data acquistion system collection, with the digital form real time record, and by the statistics parsing, carry out the chemical composition analysis of sample, element distribution analysis (degree of segregation analysis), fraction void analysis and snotter distributional analysis.
According to technique scheme, in-situ metal analyzer of the present invention is specifically by excitation light source system, beam splitting system, single spark discharge high speed acquisition system, and spark spectrum impulse discharge digital solution analysis system and continuous agitation synchronous scanning positioning system are formed.Wherein:
Excitation light source system is made up of high-purity argon gas controller, tungsten electrode, sample and spark generator.
Beam splitting system is by entrance slit, and monochrometer and exit slit are formed.
Single spark discharge high speed acquisition system is made up of photomultiplier, hardboard, amplification plate and high speed acquisition board.
Spark spectrum impulse discharge digital solution analysis system is made up of controller, computing machine and printer.
Continuous agitation synchronous scanning positioning system is made up of framework, crotch, connecting cylinder, lifting table, X-axis guide rail, Y-axis guide rail, depression bar and stepper motor.
Now the invention will be further described in conjunction with the accompanying drawings
Description of drawings
Accompanying drawing 1 is the structural representation of in-situ metal analyzer of the present invention.
Accompanying drawing 2 is the structural representation of continuous agitation synchronous scanning positioning system.
Embodiment
Can find out that by accompanying drawing 1 in-situ metal analyzer of the present invention comprises excitation light source system, beam splitting system, single spark discharge high speed acquisition system, spark spectrum impulse discharge digital solution analysis system and continuous agitation synchronous scanning positioning system.The light that excitation light source system excited links to each other with the entrance slit 5 of beam splitting system by catoptron 16, beam splitting system links to each other with the photomultiplier 8 of single spark discharge high speed acquisition system by exit slit 7 emitted line spectrums, the high speed acquisition board 11 of single spark discharge high speed acquisition system links to each other with controller 12 in the spark spectrum impulse discharge digital solution analysis system by lead, and the controller 12 in the spark spectrum impulse discharge digital solution analysis system links to each other with 31 with stepper motor 28 in the continuous agitation synchronous scanning positioning system by lead 17.
Described excitation light source system is made up of high-purity argon gas controller 1, tungsten electrode 2, sample 3 and spark generator 4; Tungsten electrode 2 links to each other with spark generator 4, and vertically relative with sample 3, and the nozzle 18 of high-purity argon gas controller 1 is aimed at the spark center that spark generator 4 is produced.
Described beam splitting system is made up of entrance slit 5, monochrometer 6 and exit slit 7; Entrance slit 5 and exit slit 7 are in the both sides of monochrometer 6 respectively.The width of entrance slit 5 is 60-80um, and the width of exit slit 7 is 20-30 μ m, and the slit number n of exit slit is 3-55, and monochrometer 6 adopts concave grating, Paschen-Long Ge (Paschen-Runge) device.The optics basic parameter of beam splitting system is: grating focal length 750mm, spectral line scope 120-800nm. whole spectral system is under the thermostatic control state.
Described single spark discharge high speed acquisition system is made up of photomultiplier 8, hardboard 9, amplification plate 10 and high speed acquisition board (A/D) 11; With respect to the slit number n of exit slit in the beam splitting system, the corresponding n that also has organizes single spark discharge high speed acquisition system.Photomultiplier 8 in each group single spark discharge acquisition system, amplify plate 10 and high speed acquisition board 11 all by the lead series connection, then parallel with one another between each group, hardboard 9 then communicates with photomultiplier 8 during each is organized by lead 19.
Described spark spectrum impulse discharge digital solution analysis system is made up of controller 12, computing machine 13 and printer 14; The three links to each other by lead.
Described continuous agitation synchronous scanning positioning system is a kind of programmable automated machine device, and it is by framework 21, and crotch 22, connecting cylinder 23, lifting table 25, X-axis guide rail 29, Y-axis guide rail 27, depression bar 32, stepper motor 28 and 31 are formed.Lifting table 25 is fixed on the X-axis guide rail 29, and lifting table 25 links to each other with crotch 22 by connecting cylinder 23, and framework 21 is fixed on the crotch 22, and depression bar 32 screws bolt 24 and also is used for fixing sample 3 by pressure head 33 fastening samples 3; Stepper motor 31 joins with X-axis guide rail 29 by its leading screw 30, and stepper motor 28 is connected with y axis rail 27 by leading screw 26, and both constitute X-Y rectangular coordinate scan track.Controller 12 sends motion command by lead 17 in the spark spectrum impulse discharge digital solution analysis system, control step motor 28 and 31 drives framework 21 and scans in selection area, range of movement and track can be adjusted at any time according to analysis task, accurate position that can real time record spark generator sparking electrode.
Adopting in-situ metal analyzer analysis of metallic materials chemical constitution of the present invention is the content that the intensity of the characteristic spectral line by measuring each element is measured each composition, and the binding site signal, determines the distribution of element, and its concrete course of work is as follows:
1, determines X-Y axle initial point
Move by continuous agitation synchronous scanning positioning system 15 clamped sample 3, determine a relative zero.
2. sample parameters setting.
By computing machine 13 the sample sweep limit is set.
3. excite sampling
Excitation light source system carries out spark discharge at sample surfaces under the control of program, continuous spectrum is gathered, stored by single spark discharge high speed acquisition system after the beam splitting system beam split.
4. data processing
By the relative size of computing machine 13 by each spark discharge energy of controller 12 acceptance, add up parsing, calculate the chemical constitution and the inclusion content of each element, in conjunction with accepted by controller 12 from the spark positional information in the continuous agitation synchronous scanning positioning system, just can calculate the degree of segregation and the fraction void of each composition of material surface, and draw the component distributing and the snotter distribution image of each element, show with two dimension, 3 D stereo mode.And by printer, printout.
Compared with prior art, the present invention has following advantage:
(1) single pass analysis obtains the quantitative analysis results of constituent content in the material, elemental composition distribution, degree of segregation, fraction void and snotter simultaneously.Analytical test information is comprehensive, and contrast property is strong.
(2) chemical constitution of coming calculation sample with the mean value of the constituent content of each point in the sweep limit, the difference of sampling spot when having avoided element segregation and the error brought, analysis result is more reliable.
(3) with each element component content on X-Y scheme display material arbitrfary point, the line, and indicate the position that macrosegregation occurs, the result is quantitatively accurate, and is practical.
(4) with the loose situation on X-Y scheme display material arbitrfary point, the line, and indicate the position of serious loose appearance, the result is quantitatively accurate, and is practical.
(5) with the distribution of elemental composition and snotter in the three-dimensional graph display material, visual in image.
(6) analytical cycle is short, is applicable to the real-time monitoring of production scene.
Claims (3)
1. in-situ metal analyzer is characterized in that:
1. this analyser comprises excitation light source system, beam splitting system, single spark discharge high speed acquisition system, spark spectrum impulse discharge digital solution analysis system and continuous agitation synchronous scanning positioning system; The spectrum that excitation light source system excited links to each other with the entrance slit (5) of beam splitting system by catoptron (16), beam splitting system links to each other with the photomultiplier (8) of single spark discharge high speed acquisition system by the emitted line spectrum of exit slit (7), the high speed acquisition board (11) of single spark discharge high speed acquisition system links to each other by the controller (12) of lead with spark spectrum impulse discharge digital solution analysis system, the controller (12) of spark spectrum impulse discharge digital solution analysis system links to each other by the stepper motor of lead with continuous agitation synchronous scanning positioning system, and the framework (21) that excitation light source system is described positioning system synchronously by sample (3) and continuous agitation links to each other;
2. described excitation light source system is made up of high-purity argon gas controller (1), tungsten electrode (2), sample (3) and spark generator (4), tungsten electrode (2) links to each other with spark generator (4), and vertically relative with sample (3), the nozzle (18) of high-purity argon gas controller (1) is aimed at the spark center that spark generator (4) is produced;
3. described beam splitting system is made up of entrance slit (5) monochrometer (6) and exit slit (7); Entrance slit (5) and exit slit (7) are in the both sides of monochrometer (6) respectively, the width of entrance slit (5) is 60-80 μ m, the width of exit slit (7) is 20-30 μ m, monochrometer (6) adopts concave grating and Paschen one imperial lattice device, and the slit number n of exit slit (7) is 3-55;
4. described single spark discharge high speed acquisition system is made up of photomultiplier (8), hardboard (9), amplification plate (10) and high speed acquisition board (11); Slit number n with respect to exit slit in the beam splitting system (7), the corresponding n that also has organizes single spark discharge high speed acquisition system, photomultiplier (8), amplification plate (10) and high speed acquisition board (11) in each group single spark discharge high speed acquisition system are all connected by lead, it is then parallel with one another that each organizes single spark discharge high speed acquisition system, and hardboard (9) then communicates with the photomultiplier (8) of each group by lead;
5. described spark spectrum impulse discharge digital solution analysis system is made up of controller (12), computing machine (13) and printer (14), and the three links to each other by lead;
6. described continuous agitation synchronous scanning positioning system is made up of framework (21), crotch (22), connecting cylinder (23), lifting table (25), X-axis guide rail (29), Y-axis guide rail (27), depression bar (32), stepper motor; Lifting table (25) is fixed on the X-axis guide rail (29), lifting table (25) links to each other with crotch (22) by connecting cylinder (23), framework (21) is fixed on the crotch (22), depression bar (32) is by the fastening sample of pressure head (33) (3), screw nut (24) and also be used for fixing sample (3), stepper motor links to each other with X-axis guide rail (29) by its leading screw, and stepper motor links to each other with Y-axis guide rail (27) by leading screw, and both constitute X-Y rectangular coordinate scan track.
2. analyser according to claim 1 is characterized in that the whole spectral system is under the thermostatic control state.
3. analyser according to claim 1 is characterized in that the optics basic parameter of beam splitting system is: grating focal length 750mm, spectral line scope 120-800nm.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021162948A CN1160552C (en) | 2002-04-01 | 2002-04-01 | In-situ metal analyzer |
| EP03007171A EP1351049A3 (en) | 2002-04-01 | 2003-03-28 | Analyzer for metal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021162948A CN1160552C (en) | 2002-04-01 | 2002-04-01 | In-situ metal analyzer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1370987A CN1370987A (en) | 2002-09-25 |
| CN1160552C true CN1160552C (en) | 2004-08-04 |
Family
ID=4744060
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB021162948A Expired - Lifetime CN1160552C (en) | 2002-04-01 | 2002-04-01 | In-situ metal analyzer |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1160552C (en) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1351049A3 (en) * | 2002-04-01 | 2004-02-25 | Central Iron & Steel Research Institute | Analyzer for metal |
| CN100343657C (en) * | 2003-02-25 | 2007-10-17 | 鞍钢股份有限公司 | Spectral analysis method for online detection of grain size distribution of inclusions in steel |
| CN100343656C (en) * | 2003-02-25 | 2007-10-17 | 鞍钢股份有限公司 | Spectral analysis method for online detection of number and content of inclusions in steel |
| CN100447556C (en) * | 2004-12-24 | 2008-12-31 | 北京有色金属研究总院 | Method for analyzeing carbon, sulphur and phosphor in rare metal through emission spectrum, and new light source device |
| CN100489491C (en) * | 2005-11-17 | 2009-05-20 | 钢铁研究总院 | Suspension type scanning method for metal in-situ analyzer and sample clamp therefor |
| CN101294905B (en) * | 2008-05-22 | 2011-05-04 | 浙江沃尔达铜业有限公司 | Method for fast detecting metal composition |
| CN101799415B (en) * | 2010-03-04 | 2011-05-11 | 北京纳克分析仪器有限公司 | All-digital energy-adjustable spark light source |
| CN102221539B (en) * | 2011-03-29 | 2013-05-29 | 钢铁研究总院 | Laser-induced breakdown spectrum in-situ analyzer |
| CN110132942B (en) * | 2019-06-06 | 2021-01-12 | 北京科技大学 | Metal in-situ analyzer based on irregular sample analysis |
| CN113385115A (en) * | 2021-06-08 | 2021-09-14 | 北方工业大学 | Metal sample spark ablation aerosol generating device |
-
2002
- 2002-04-01 CN CNB021162948A patent/CN1160552C/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| CN1370987A (en) | 2002-09-25 |
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Assignee: Beijing NCS Analytical Instruments Co., Ltd. Assignor: Central Iron & Steel Research Institute Contract fulfillment period: 2007.12.15 to 2013.12.15 Contract record no.: 2008990000633 Denomination of invention: Metal in-situ analyzer Granted publication date: 20040804 License type: Exclusive license Record date: 20081008 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2007.12.15 TO 2013.12.15; CHANGE OF CONTRACT Name of requester: BEIJING NAKE ANALYTICAL INSTRUMENT CO., LTD. Effective date: 20081008 |
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Assignee: Beijing NCS Analytical Instruments Co., Ltd. Assignor: Central Iron & Steel Research Institute Contract record no.: 2008990000633 Date of cancellation: 20120828 |
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Owner name: NCS TESTING TECHNOLOGY CO., LTD. Free format text: FORMER OWNER: INST OF IRON + STEEL Effective date: 20121112 |
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Effective date of registration: 20121112 Address after: 100081 Beijing Haidian District sorghum Bridge oblique Street No. 13 Patentee after: NCS Testing Technology Co., Ltd. Address before: 100081 No. 76 South College Road, Beijing Patentee before: Central Iron & Steel Research Institute |
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| CP01 | Change in the name or title of a patent holder |
Address after: No. 13, sorghum Bridge, Beijing, Beijing, Haidian District Patentee after: The detection technology of NCS Limited by Share Ltd Address before: No. 13, sorghum Bridge, Beijing, Beijing, Haidian District Patentee before: NCS Testing Technology Co., Ltd. |
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