EP1695068A1 - Procede pour analyser une matiere fondue, dispositif et capteur a immersion - Google Patents

Procede pour analyser une matiere fondue, dispositif et capteur a immersion

Info

Publication number
EP1695068A1
EP1695068A1 EP04803874A EP04803874A EP1695068A1 EP 1695068 A1 EP1695068 A1 EP 1695068A1 EP 04803874 A EP04803874 A EP 04803874A EP 04803874 A EP04803874 A EP 04803874A EP 1695068 A1 EP1695068 A1 EP 1695068A1
Authority
EP
European Patent Office
Prior art keywords
excitation
analyzed
radiation
analysis
immersion
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP04803874A
Other languages
German (de)
English (en)
Inventor
Jacques Plessers
Vittorino Tusset
Marc Schyns
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Heraeus Electro Nite International NV
Original Assignee
Heraeus Electro Nite International NV
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from DE10359447A external-priority patent/DE10359447B4/de
Priority claimed from BE2004/0085A external-priority patent/BE1015940A3/fr
Application filed by Heraeus Electro Nite International NV filed Critical Heraeus Electro Nite International NV
Publication of EP1695068A1 publication Critical patent/EP1695068A1/fr
Withdrawn legal-status Critical Current

Links

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
    • G01N21/69—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 specially adapted for fluids, e.g. molten metal
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
    • C21C5/00—Manufacture of carbon-steel, e.g. plain mild steel, medium carbon steel or cast steel or stainless steel
    • C21C5/28—Manufacture of steel in the converter
    • C21C5/42—Constructional features of converters
    • C21C5/46—Details or accessories
    • C21C5/4673—Measuring and sampling devices
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D19/00—Arrangements of controlling devices
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D21/00—Arrangements of monitoring devices; Arrangements of safety devices
    • 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
    • G01N21/84—Systems specially adapted for particular applications
    • G01N21/85—Investigating moving fluids or granular solids
    • G01N21/8507—Probe photometers, i.e. with optical measuring part dipped into fluid sample
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D19/00—Arrangements of controlling devices
    • F27D2019/0003—Monitoring the temperature or a characteristic of the charge and using it as a controlling value

Definitions

  • the present invention relates to a method of analyzing a high temperature molten material by optical emission spectrometry. It is particularly suitable for the analysis of a molten metal such as cast iron or steel, but is also applicable for the analysis of slag, glass, lava or other liquid high-temperature materials.
  • the invention also relates to a novel apparatus for the use of the method according to the invention for analysis by optical emission spectrometry.
  • the invention relates to an immersion sensor for the analysis of molten materials, in particular metal, slag or lava melts or of glass with an immersion carrier, with a radiation detector and with a radiation guide device for receiving and transmitting radiation and with a arranged on or in the immersion carrier signal interface.
  • the preferred field of application of the invention is the analysis of metal, lavage, glass or slag baths, said substances being in partially or completely molten state, as well as other refractory melts.
  • the areas in which the analysis of the composition of high-temperature melting products, ie with a temperature above 300 ° C, such as liquid steel, liquid aluminum, liquid glass or liquid lava, is carried out, are very far-reaching.
  • the commonly used methods require the removal of a sample, which is first cooled and then subjected to various analytical techniques after partial or complete cooling.
  • Various analysis techniques may be used and are selected depending on the ingredients of the composition to be qualitatively identified or quantitatively metered.
  • emission spectrometry is the most widely used technique, because it is very fast, requires little work in the preparation of samples, and allows the simultaneous dosing of a large number of constituents.
  • Emission spectrometry is based on exciting the material to be analyzed in such a way as to cause ionization of the material of which it is composed. The emitted radiation is then analyzed in a spectrometer, which splits this radiation into different wavelengths that correspond to the existing substances.
  • spectrometer types the most common in the fields in question being equipped with photomultiplier detectors or with CCD (Charged Coupled Device) or CMOS (Complementary Metal Oxide Semi-conductor) systems.
  • the emission spectrometry analyzers are either laboratory equipment or portable equipment for the analysis of solid products.
  • the radiation from the analyzed product can be supplied to the spectrometer in a variety of ways, such as through a glass fiber, through a telescope, and so on.
  • Such techniques are known as immersion sensors for analysis in melts are known from WO 03/081287 A2.
  • a carrier tube is disclosed, which is immersed in an aluminum melt.
  • a lens system is arranged.
  • a light guide is arranged, which with a spectrograph on the one hand and a
  • the laser is connected via an optical system.
  • the radiation emitted by the melt is conducted via the light guide into the spectrograph, where the radiation is analyzed in order to derive analysis results for the composition of the aluminum melt.
  • a method for analyzing a melt by optical emission spectrometry which is particularly intended for the analysis of a molten metal such as cast iron or steel, but also for the analysis of slag, glass, lava or other liquid having a temperature above 300 ° C. and preferably above 500 ° C is applicable, in which a so-called "sensitive element" is used, which contains at least one emission spectrometer, essentially characterized in that
  • a sensitive element having at least one excitation means is used to effect the excitation of the analyte and to enable the partial or complete generation of radiation to be analyzed by a spectrometer present in the sensitive element
  • An information which is referred to as analysis signal and from the sensitive element between the time of its contact with the analyte to be analyzed and its destruction is sent by melting in said substance, is detected, and that the transmitted information contains analysis elements which from a spectrometer present in the sensitive element, and
  • the sensitive element used in the aforementioned method for carrying out the analysis includes not only an emission spectrometer, but also excitation means for effecting the excitation of the substance being analyzed and producing part or all of the radiation analyzed by the existing spectrometer, its use entails Solution to the problems associated with the use of an external excitation device such as a laser, which is to be located in the vicinity of the substance to be analyzed.
  • the method thus consists in employing a system for self-excitation of the material to be analyzed so as to output an emission spectrum that can be analyzed by a field spectrometer, ie a spectrometer present in the element that is to be analyzed Melt is brought into contact.
  • a field spectrometer ie a spectrometer present in the element that is to be analyzed Melt is brought into contact.
  • a modulation technique is used to take into account the practical operating conditions, such as, for example, measurement of the fundamental radiation which is so-called in measurement and control technology.
  • the practical operating conditions such as, for example, measurement of the fundamental radiation which is so-called in measurement and control technology.
  • at least one measurement of the spectrum emitted by the analyte is performed without excitation of that substance.
  • the spectrum of fundamental radiation obtained in this way is then subtracted from the spectrum picked up by the sensitive element after excitation of the analyte. Due to the result of this process, an analysis signal independent of the fundamental radiation is emitted from the sensitive element.
  • At least one measurement of the temperature of the analyzed substance is carried out prior to the process of excitation of the substance to be analyzed in order to correct the signal emitted by the sensitive element.
  • Possible fluctuations (wavelength, amplitude, width) of the emission lines characteristic for the material after excitation of the analyzed substance as a function of the temperature are to be taken into account.
  • At least one measurement of the spatial position of the analyzed location is furthermore carried out in order to evaluate the relevance of its selection for a measurement. That is to make sure that it is no less interesting, for example, at the borders of that of the tub or near an oxidized surface. There is a risk that the analysis of the substance in question will not be representative of the substance in the vat to be analyzed.
  • At least one excitation device for generating an electrical excitation; said excitation means preferably comprises at least one charged capacitor equipped with an interruption system which may be powered by a battery and capable of generating a number of 1 to 2000 discharges, each discharge lasting at least 10 nsec (nanoseconds) and an intensity of at least 0, 01 amps.
  • At least one excitation device for generating a chemical excitation, preferably with a liquid amount of preferably less than 1000 ml, which is brought into contact with the melt to be analyzed in such a way that a high-energy chemical reaction is produced which stimulates of the analyte and generates radiation which is analyzed by a spectrometer present in the sensitive element, which is preferably an explosive chemical reaction.
  • the excitation means further comprises a container for the liquid, which serves for the excitation by chemical reaction, which has the modulation of the period of contact of the substance to be analyzed and the existing excitation means or the excitation means to the object, possibly through Management of wear and then destruction of one or more components of the on-site spectrometer used to analyze the radiation.
  • a container is used, the latter being provided with a device referred to as explosion valve, which consists of a metal or a metallic alloy whose melting temperature of at least 10 ° C, the melting temperature of exceeds analyzing metal; in the case of ULC steels, for example, a tungsten doped steel may be used as the valve.
  • explosion valve which consists of a metal or a metallic alloy whose melting temperature of at least 10 ° C, the melting temperature of exceeds analyzing metal; in the case of ULC steels, for example, a tungsten doped steel may be used as the valve.
  • the excitation device is mixer design and uses a liquid - preferably water -, wherein the minimum volume of liquid used is preferably 0.01 ml.
  • the present invention also relates to an apparatus for carrying out the method according to the invention.
  • the device is essentially characterized in that the sensitive element brought into contact with the melt to be analyzed contains a shell which at least partially comprises the aforementioned sensitive element, said shell preferably being made of a (under operating conditions) dissolvable material, preferably vermiculite , consists.
  • the sheath is geometrically designed such that the destruction of the sensitive element is delayed by melting, wherein the geometry preferably favors the contacting of the sensitive part of the spectrometer with the melt to be analyzed - preferably a molten metal.
  • the element brought into contact with the molten metal to be analyzed is contained in an enclosure whose internal atmosphere is controlled, consisting of a gas or of a gas mixture, preferably containing nitrogen and / or argon or placed under vacuum is, preferably at a pressure of at least 10 "1 mm Hg +/- 10% in the case of the vacuum.
  • the invention does not require the presence of external systems (laser systems or others) to effect excitation of the material of the object to be analyzed.
  • external systems laser systems or others
  • the facilities for the spectrometric analysis can be simplified and the associated economic costs can be reduced.
  • an immersion sensor for analyzing in particular metal melts with an immersion carrier, with a radiation detector and with a radiation guiding device for receiving and transmitting radiation and with a signal interface arranged on or in the immersion carrier in that on or in the immersion carrier the radiation detector and at least a part of the radiation guidance device are arranged and that the signal interface is connected to the radiation detector.
  • the signal transmission is considerably simplified, since the outgoing of a molten metal optical radiation can be converted already on or in the immersion carrier into electrical signals that can be easily forwarded in many ways.
  • the radiation detector no longer has to be designed for continuous operation, it loses its power after the measurement its function and can therefore be made simple and inexpensive. Maintenance of the radiation detector is no longer necessary.
  • the radiation detector has a device for receiving radiation and for conversion into electrical signals
  • the radiation detector is expediently adapted to receive and convert visible light, ultraviolet radiation, infrared radiation, X-radiation and / or microwave radiation into electrical signals.
  • the immersion carrier is formed as a tube in which the individual parts are arranged, as this protection of the individual parts during transport can be better ensured.
  • the immersion carrier is formed from a material consumable in molten metal, in particular from an organic material.
  • the signal interface is designed as an electrical or optical coupling or as a transmitter (for wireless or wireless transmission of signals). Accordingly, it is possible to couple optical signals coming from the outside into the beam guiding device, to transmit signals coming from the radiation detector (electrical or optical signals) via wire or cable or also via the air by means of transmitters.
  • this makes it possible to easily detach and dispose of the immersion carrier after use of the external equipment and to connect to the external equipment (computer, laser for radiation delivery, spark gap or other facilities) leads connected via the coupling part a new immersion carrier.
  • the immersion carrier is connected to a mechanical coupling, preferably for coupling a carrier lance. Such carrier lances are common in metallurgy for holding measuring devices.
  • the signals emitted by the radiation detector can be transmitted by radio to a computer. It is in principle also possible to provide the signal evaluation already in a unit with the radiation detector, so that only the results are forwarded. It is also conceivable, on or in the immersion carrier to convert incoming electrical signals into optical signals. In this case, the signals arriving at the subcarrier could also be wirelessly or wirelessly transmitted to the subcarrier by radio, converting the radio signals into optical signals. This would make possible a non-contact measurement, a fixed connection between the sensor and the evaluation device or a ready signal. Positioning device would be superfluous, since one is able to provide sufficiently inexpensive, small and powerful units for this purpose.
  • a signal amplifier and / or a processor for signal evaluation is arranged on or in the immersion carrier
  • the beam guiding device comprises optical and / or magnetic lenses, optical fibers, mirrors, a spark discharge path and / or diaphragms.
  • the device for generating the spark discharge or another radiation emission device may also be arranged on or in the immersion carrier.
  • an optical spectrometer, an X-ray spectrometer and / or a mass spectrometer can be arranged on or in the immersion carrier.
  • the immersion carrier is formed as a tube
  • melting materials such as cryolite melts, iron or steel melts or glass, lava or copper melts can be well analyzed in the manner described above.
  • FIG. 2 shows an alternative construction / method sequence
  • FIG. 3 shows a further embodiment of the method according to the invention
  • FIG. 4 shows a representation of an immersion sensor immersed in a molten metal.
  • Figure 1 illustrates a process under development or in the industrial pilot stage. It is the metal 1 or any solid or liquid to be analyzed substance in a container 7 and to detect the laser device 2, the beam 3 strikes the metal 1 and there causes such heating that a radiation 4 is emitted therefrom, wherein the radiation 4 is at least partially supplied to a spectrometer 5, which is connected to different analysis or signal processing means 6, which allow the interpretation of the information contained in the radiation 4 / analysis signal, to obtain therefrom, the analysis of the metal 1.
  • Figure 2 illustrates an alternative method that can be used in the analysis of a metallic molten bath.
  • the substance to be analyzed which is the metal bath contained in the container 7, and a CCD spectrometer which is brought into contact with the metal bath 1 are to be recognized, the spectrometer 8 being analyzed after a certain time by melting Bad 1 is destroyed.
  • the aforementioned spectrometer 8 is provided with a radiation detector, said radiation being previously possibly divided by a grating or a crystal into different components.
  • the aforesaid detector may be or equivalent to a CCD detector equipped with a transmitting system which transmits the data provided by the detector to an antenna 10 for further analysis and / or operational processing in a suitable analysis or analysis device Signal processing device 6 transmits.
  • the use of the device illustrated in FIG. 2 is to induce excitation in the metal bath 1 to be analyzed via the excitation device 2, which as a rule is a laser emitting the beam 3 which strikes the metal bath 1 at one point which is in the vicinity of the spectrometer 8 such that it detects and analyzes the radiation induced by the beam 3 from the excitation laser 2 and originating from the bath 1.
  • the result of the analysis process by the spectrometer 8 is transmitted by a transmission link 9 (for example wavy by radio or by cable) to a detection device / antenna 10, which may be suitable for storing the information / the analysis signal or for an analysis or analysis Signal processing device 6 forward, which allows a design of the analysis of the induced radiation to determine the chemical composition of the metal bath.
  • a transmission link 9 for example wavy by radio or by cable
  • a detection device / antenna 10 which may be suitable for storing the information / the analysis signal or for an analysis or analysis Signal processing device 6 forward, which allows a design of the analysis of the induced radiation to
  • a sensitive element 11 is inserted, which at least one spectrometer and a System for self-excitation of the metal from which the bath 1 to be analyzed consists.
  • the pickup is triggered manually, automatically or otherwise when the sensitive element 11 is in contact with the bath 1 to be analyzed, and a signal 9 originating from the sensitive element 11 is detected by the detection device / antenna 10, which signal is interpreted by an analysis or signal processing device 6 for the interpretation of the results of a in the sensitive element 11 located spectrometer measurements can be processed.
  • an immersion sensor is partially immersed in a container / crucible 7 with molten iron 1.
  • the immersion carrier 12 is formed as a tube made of cardboard, in which the beam guiding device is arranged with a semitransparent mirror 13 and a lens 14.
  • a spectrometer 8 is further arranged, which receives the coming of the molten iron 1 radiation and converts it into electrical signals.
  • the electrical signals are forwarded by means of signal lines 15 to a coupling 16.
  • the coupling 16 serves to connect the immersion sensor to external supply devices.
  • a laser source is connected to the connector / coupling 16 via a light guide 17, signal cables 18 connect the immersion sensor to a computer and a gas line 19 allows the gas to enter the tube (the immersion carrier 12, the tube itself the gas line between the coupling 16 and the melt 1.
  • the light guide 17 is connected to a light exit 20. Laser light is focused through the light exit 20 through the mirror 13 and the lens 14 onto the molten iron 1. The light reflected by the molten iron 1 is reflected by the mirror 13 directed the signal input of the spectrometer 8. For this purpose, the mirror 13 is formed semi-permeable.
  • a carrier lance can be inserted, at which the tube is held during the immersion process.
  • the industrial areas on which the present analysis method can be used by emission spectrometry are very numerous and are not limited to the Treatments in a steel mill, but can also serve for monitoring by analyzing their composition for other metallurgical baths, possibly for baths for the deposition of metal as in the galvanization.
  • Significant productivity gain can be expected because at no point in time to perform analysis by optical emission spectrometry will disrupt the industrial manufacturing process and thus waste time.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)
  • Spectrometry And Color Measurement (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Investigating And Analyzing Materials By Characteristic Methods (AREA)

Abstract

L'invention concerne un procédé et un dispositif pour analyser une matière fondue par spectrométrie d'émission optique, par exemple un métal fondu, tel que de la fonte de fer, de l'acier, un laitier, un verre ou une lave. Selon ladite invention, un élément sensible, comprenant au moins un spectromètre d'émission et au moins un dispositif d'excitation, est utilisé pour induire l'excitation de la matière à analyser et pour permettre la production partielle ou complète d'un rayonnement destiné à être analysé par un spectromètre situé dans l'élément sensible. L'élément sensible susmentionné est mis en contact avec la matière fondue à analyser et transmet une information contenant des éléments d'analyse fournis par un spectromètre. Cette invention concerne également un capteur à immersion.
EP04803874A 2003-12-17 2004-12-15 Procede pour analyser une matiere fondue, dispositif et capteur a immersion Withdrawn EP1695068A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE10359447A DE10359447B4 (de) 2003-12-17 2003-12-17 Eintauchsensor
BE2004/0085A BE1015940A3 (fr) 2004-02-13 2004-02-13 Procede d'analyse par spectrometrie d'emission optique d'une substance en fusion.
PCT/EP2004/014252 WO2005059527A1 (fr) 2003-12-17 2004-12-15 Procede pour analyser une matiere fondue, dispositif et capteur a immersion

Publications (1)

Publication Number Publication Date
EP1695068A1 true EP1695068A1 (fr) 2006-08-30

Family

ID=34701669

Family Applications (1)

Application Number Title Priority Date Filing Date
EP04803874A Withdrawn EP1695068A1 (fr) 2003-12-17 2004-12-15 Procede pour analyser une matiere fondue, dispositif et capteur a immersion

Country Status (11)

Country Link
US (1) US7365841B2 (fr)
EP (1) EP1695068A1 (fr)
JP (2) JP4750717B2 (fr)
KR (2) KR101030103B1 (fr)
AU (4) AU2004299940C1 (fr)
BR (1) BRPI0417748A (fr)
CA (1) CA2539844C (fr)
MX (1) MXPA06006246A (fr)
RU (2) RU2348029C2 (fr)
WO (1) WO2005059527A1 (fr)
ZA (1) ZA200605776B (fr)

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AU2008249182B2 (en) 2011-10-06
RU2006125424A (ru) 2008-01-27
BRPI0417748A (pt) 2007-04-10
RU2348029C2 (ru) 2009-02-27
RU2008133289A (ru) 2010-02-20
JP4750717B2 (ja) 2011-08-17
KR20110038149A (ko) 2011-04-13
KR101030103B1 (ko) 2011-04-20
AU2004299940B2 (en) 2008-12-04
JP5554281B2 (ja) 2014-07-23
KR20060121193A (ko) 2006-11-28
JP2011141293A (ja) 2011-07-21
US7365841B2 (en) 2008-04-29
JP2007514941A (ja) 2007-06-07
MXPA06006246A (es) 2006-08-23
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AU2011201561A1 (en) 2011-04-28
AU2008249182A1 (en) 2008-12-11
CA2539844A1 (fr) 2005-06-30
AU2004299940A1 (en) 2005-06-30
AU2011201560A1 (en) 2011-04-28
AU2004299940C1 (en) 2009-05-14
US20060250614A1 (en) 2006-11-09
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AU2011201560B2 (en) 2011-10-06
CA2539844C (fr) 2012-01-31
WO2005059527A1 (fr) 2005-06-30

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