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WO2013046005A1 - Procédé de vérification et d'amélioration de la qualité d'un alliage métallique durant le processus de solidification et dispositif approprié pour mettre en œuvre ledit procédé - Google Patents

Procédé de vérification et d'amélioration de la qualité d'un alliage métallique durant le processus de solidification et dispositif approprié pour mettre en œuvre ledit procédé Download PDF

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Publication number
WO2013046005A1
WO2013046005A1 PCT/IB2012/001910 IB2012001910W WO2013046005A1 WO 2013046005 A1 WO2013046005 A1 WO 2013046005A1 IB 2012001910 W IB2012001910 W IB 2012001910W WO 2013046005 A1 WO2013046005 A1 WO 2013046005A1
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WO
WIPO (PCT)
Prior art keywords
metal alloy
electrical
during
electrical quantity
values
Prior art date
Application number
PCT/IB2012/001910
Other languages
English (en)
Inventor
Adrian UDROIU
Mauro DE LISSANDRI
Original Assignee
Tekom S.R.L.
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
Application filed by Tekom S.R.L. filed Critical Tekom S.R.L.
Publication of WO2013046005A1 publication Critical patent/WO2013046005A1/fr

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
    • G01N27/06—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a liquid
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/20—Metals
    • G01N33/205—Metals in liquid state, e.g. molten metals

Definitions

  • the invention concerns a method for verifying and improving the quality of a metal alloy during its solidification process, in such a way as to make it possible to plan suitable interventions and reduce the risk of faults being present inside the metallic structure of the same alloy.
  • the invention also concerns a piece of equipment for verifying and improving the quality of a metal alloy comprising a device for measuring the electrical resistance of a metal alloy during its solidification process and a processing device containing a specific software suited to process the input data received, in such a way as to carry out the verification and improvement steps included in said method that is the subject of the invention.
  • every metal alloy is a combination of atoms, ions and molecules of different components, among which there are the already mentioned pure metals.
  • steel is made of iron and carbon, while brass is made of copper and zinc.
  • said components can be divided into solvent and solute, wherein the solvent is present in the alloy in a quantity exceeding the quantity of solute.
  • the entry in and exit from the so-called biphasic zone during the solidification process of an alloy vary not only according to what components make up the metal alloy but also according to the percentage content of the same in the alloy.
  • an alloy constituted by a component A that makes up 60% of it and by a second component B that makes up 40% of it has thresholds of entry and exit in/from the biphasic zone that are different from those of an alloy constituted by 40% of the same component A and 60% of the same component B, as can be seen in the diagram shown in Figure 1.
  • the present invention aims to overcome the drawbacks listed above.
  • the invention has the purpose to define and develop a method and a piece of equipment for verifying and improving the quality of a metal alloy that make it possible to provide information on its tendency to generate faults during the solidification of the same metal alloy.
  • the object of the present invention to define and develop a method and a piece of equipment that make it possible to determine how and to what extent to intervene on the metal alloy during its solidification process.
  • the invention includes also the quality verification and improvement equipment described in claim 8, which makes it possible to carry out the operations belonging to the method of the invention.
  • FIG. 1 shows a typical phase diagram of a generic metal alloy made up of two components A and B;
  • FIG. 2 shows the Cartesian graph of the real curve related to the electrical resistance variation of a specific metal alloy during the solidification process
  • Figure 3 shows the Cartesian graph of the first derivative related to the real curve shown in Figure 2;
  • FIG. 4 shows a schematic view of a first embodiment of the equipment of the invention
  • FIG. 5 shows a schematic view of a second embodiment of the equipment of the invention.
  • the method of the invention for verifying and improving the quality of a metal alloy during the solidification process is based on the concept that the value of the electrical resistance of a given metal alloy is directly related to the chemical composition of the same alloy and to its solidification stage.
  • the applicant has discovered that by measuring the electrical resistance of a metal alloy during the solidification process at short time intervals or continuously it is possible to determine the progress of the latter and, consequently, to intervene to the correct extent and in due time to avoid the formation of faults and improve the quality of the same alloy.
  • the method of the invention includes a first operation that consists in placing a given quantity of metal alloy in the liquid state inside a crucible, where its solidification process will take place.
  • a first constant electrical quantity, selected between electrical current or electrical voltage is provided between a first pair of electrodes immersed in the metal alloy, so that it is possible to measure simultaneously the values of a second electrical quantity, selected between electrical voltage and electrical current, present in said alloy by means of a second pair of electrodes also immersed in the alloy during its solidification.
  • the first electrical quantity is electrical current
  • the second electrical quantity is electrical voltage
  • the measurement of said electrical voltage values is carried out continuously during the solidification process. However, it cannot be excluded that said measurement can be carried out at specific time instants according to regular intervals.
  • the measurement of the electrical voltage values makes it possible to calculate, preferably during the same solidification process, the electrical resistance corresponding to each of them.
  • the values of the electrical resistance are obtained from the ratio between the electrical voltage values measured and the electrical current value provided.
  • the first constant electrical quantity is a constant electrical voltage while the second electrical quantity measured is the electrical current that flows through the metal alloy.
  • these resistance values are used to define a real curve 100 of the variation in the same electrical resistance during the entire solidification process of the metal alloy.
  • said real curve 100 is defined on a Cartesian graph 101 having temperature values on the x-axis and electrical resistance values on the y-axis, as shown in Figure 2.
  • An alternative embodiment of the method of the invention may require that said Cartesian graph is defined indicating on the x-axis, instead of the temperature values, the value of the time necessary for the solidification of the metal alloy.
  • a different embodiment of the invention may require the definition of a Cartesian graph in three dimensions, where the quantities indicated on the three axes are respectively the electrical resistance of the metal alloy that is solidifying, the temperature value and the solidification time.
  • said real curve 100 is defined progressively during the solidification process, as the data are measured and calculated.
  • said interpretation requires that said real curve 100 is compared with reference values related to the variation in the electrical resistance obtained from a plurality of statistical measurements on samples of the same metal alloy being analysed, the defectiveness level of which is known. Said statistical measurements are obviously carried out before implementation of the method of the invention.
  • the interpretation consists, as first thing, in obtaining from said statistical measurements and defining on the same graph 101 an ideal curve 102 of the variation in the electrical resistance of the metal alloy being analysed, with no faults.
  • the ideal curve 102 is defined using those statistical measurements related to samples of the specific allow being analysed, with no faults.
  • peaks 103 assume an important meaning during the solidification process of a metal alloy, as they indicate the various moments at which the changes of state of the alloy take place.
  • the comparison step requires that the first derivatives 104 of said two curves 100 and 102 are compared, so as to compare the speed of variation in the electrical resistance of the metal alloy being analysed with the speed of variation in the resistance of the ideal alloy, as shown in Figure 3.
  • said statistical measurements referring to samples of the specific metal alloy being analysed, whose level of defectiveness is known, are used to determine a statistical regression equation.
  • said positive peaks 103 of the real curve 100 are determined and the electrical resistance values related to said peaks 103 are used as variables of said regression equation.
  • the result of the equation indicates, at a statistical level, the dissimilarity of the real curve 100 with respect to a metal alloy of the same type with no faults. Said result, therefore, indicates the level of defectiveness of the metal alloy of which the real curve 100 has been defined.
  • the results obtained make it possible to understand how and when it is possible to intervene during the solidification process of the metal alloy to improve its quality.
  • Said interventions represent the final operation of the method of the invention and require that specific additives are introduced in the alloy during the solidification stage in order to reduce said dissimilarities between the two curves 100 and 102 being compared or between the real curve 100 and the statistical data, so that the characteristics of the alloy being analysed become more similar to those of the ideal metal alloy without faults.
  • the invention includes also the equipment 1 , shown in Figures 4 and 5, comprising a device 11 for measuring the electrical resistance of a metal alloy L during the solidification process and a processing device 12 in which a specific software has been loaded that is suited to process the input electrical current and electrical voltage values, so as to carry out the verification and improvement operations belonging to said method of the invention.
  • this is used to obtain the data (the electrical current and voltage values and consequently the electrical resistance values) necessary for comparing the characteristics of the same metal alloy L being analysed with those of the same alloy ideally without faults.
  • the measuring device 11 comprises a crucible 2 suited to contain a given quantity of metal alloy L in the liquid state to be analysed.
  • said crucible 2 in the preferred embodiment of the invention, is of the disposable type and is made of sand.
  • the measuring device 11 comprises a first pair of electrodes 3, each one of which has a first end 31 inserted in the empty space defined inside said crucible 2 so that it can come into contact with the metal alloy L in the solidification stage.
  • the second end 32 of the electrodes belonging to the first pair 3 is connected to a current generator 4 that, as explained above, has the function of providing a constant electrical current to the metal alloy L.
  • the measuring device 11 comprises a second pair of electrodes 5, each one of which, similarly to those belonging to the first pair of electrodes 3, has a first end 51 inserted in the empty space defined inside the crucible 2 so that it can come into contact with the metal alloy L.
  • the second end 52 of the two electrodes of the second pair 5 is connected to a voltage measuring device 6, so as to measure the electrical voltage present in the metal alloy L during said solidification process.
  • the electrical current generator 4 and the electrical voltage measuring device 6 belong to a milliohmmeter 8.
  • the measuring device 11 also comprises, inside the crucible 2, a temperature sensor 9, preferably a thermocouple 91.
  • Said sensor 9 is capable of determining the variation in the temperature of the metal alloy L during its solidification stage.
  • this comprises an input/output system 7 capable of exchanging the data concerning the first electrical quantity provided, the second electrical quantity measured and if necessary the measured temperature with the measuring device 11.
  • the processing device 12 is capable of calculating the variation in the electrical resistance during the solidification process and of defining the graph 101 of the real curve 100, shown in Figure 2, so as to be able to carry out the successive comparison and interpretation operations belonging to the method of the invention.
  • the invention achieves the object to define and implement a method and a piece of equipment for verifying and improving the quality of a metal alloy that make it possible to provide information on its tendency to generate faults during the solidification of the same metal alloy.
  • the invention also achieves the further object to define and develop a method and a piece of equipment that make it possible to determine how and to what extent to intervene in the metal alloy during its solidification process.
  • the invention also achieves the further object to define and develop a method and a piece of equipment that make it possible to determine the chemical composition of the metal alloy during the entire solidification stage of the same alloy and, in the case where the chemical composition of said metal alloy deviates from the reference data, make it possible to identify the types and quantities of additives suited to improve its quality.
  • the invention also achieves the further object to define and implement a method and a piece of equipment that make it possible to identify and predict the final mechanical characteristics of the solidified metal alloy.
  • the invention also achieves the further, and not the least, object to define and implement a method and a piece of equipment that make it possible to predict the shrinkage effects of the metal alloy during the solidification stage and, where said possible shrinkage effects are identified, to indicate the type of operations to be carried out to improve the quality of the metal alloy.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Medicinal Chemistry (AREA)
  • Investigating And Analyzing Materials By Characteristic Methods (AREA)
  • Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)

Abstract

La présente invention porte sur un procédé de vérification et d'amélioration de la qualité d'un alliage métallique durant le processus de solidification, comprenant, dans l'ordre donné, les opérations consistant à : placer l'alliage métallique à l'état liquide à l'intérieur d'un creuset ; fournir une première quantité électrique constante, choisie entre un courant électrique et une tension électrique, entre une première paire d'électrodes immergées dans ledit alliage métallique durant l'étape de solidification ; mesurer les valeurs d'une seconde quantité électrique, choisie entre une tension électrique et un courant électrique, pour une pluralité d'instants durant l'étape de solidification, au moyen d'une seconde paire d'électrodes immergées dans l'alliage métallique ; calculer, pour chaque instant, la résistance électrique de l'alliage métallique, obtenue à partir du rapport entre la première quantité électrique constante et chacune des valeurs de la seconde quantité électrique ; définir une courbe réelle de la variation de résistance électrique dans l'alliage métallique durant l'étape de solidification sur un graphe cartésien où des valeurs de température et/ou de temps sont indiquées sur l'axe x et des valeurs de résistance électrique sont indiquées sur l'axe y ; comparer la courbe réelle avec des valeurs de référence associées à la variation de résistance obtenue à partir d'une pluralité de mesures statistiques sur des échantillons de l'alliage métallique dont le niveau de défectuosité est connu, de manière à identifier toute dissimilarité de la courbe réelle par rapport auxdites valeurs de référence ; inclure des additifs dans l'alliage métallique afin de réduire les dissimilarités entre la courbe réelle et les valeurs de référence.
PCT/IB2012/001910 2011-09-29 2012-09-28 Procédé de vérification et d'amélioration de la qualité d'un alliage métallique durant le processus de solidification et dispositif approprié pour mettre en œuvre ledit procédé WO2013046005A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
IT000258A ITVI20110258A1 (it) 2011-09-29 2011-09-29 Metodo di verifica della qualita' di una lega metallica durante il processo di solidificazione e dispositivo atto ad eseguire il suddetto metodo
ITVI2011A000258 2011-09-29

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111965225A (zh) * 2020-07-17 2020-11-20 沈阳广泰真空科技有限公司 一种真空感应熔炼炉中的坩埚监测方法及装置

Citations (5)

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Publication number Priority date Publication date Assignee Title
LU73004A1 (fr) * 1975-07-17 1977-03-21
EP0021316A1 (fr) * 1979-06-20 1981-01-07 Krupp Stahlwerke Südwestfalen AG Procédé et dispositif pour déterminer les teneurs en oxydes de métaux lourds de laitiers liquides
US5432458A (en) * 1990-06-29 1995-07-11 Mitsubishi Materials Corporation Process for determination of phosphorus in molten copper
DE202004014735U1 (de) * 2004-09-22 2004-11-25 Schweiger, Hans-Georg Apparatur zur Bestimmung von Phasenübergängen
US20090101522A1 (en) * 2007-05-29 2009-04-23 Jing Xu High Temperature Electrochemical Characterization of Molten Metal Corrosion

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
LU73004A1 (fr) * 1975-07-17 1977-03-21
EP0021316A1 (fr) * 1979-06-20 1981-01-07 Krupp Stahlwerke Südwestfalen AG Procédé et dispositif pour déterminer les teneurs en oxydes de métaux lourds de laitiers liquides
US5432458A (en) * 1990-06-29 1995-07-11 Mitsubishi Materials Corporation Process for determination of phosphorus in molten copper
DE202004014735U1 (de) * 2004-09-22 2004-11-25 Schweiger, Hans-Georg Apparatur zur Bestimmung von Phasenübergängen
US20090101522A1 (en) * 2007-05-29 2009-04-23 Jing Xu High Temperature Electrochemical Characterization of Molten Metal Corrosion

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
LI X-F ET AL: "Anomalous change of electrical resistivity with temperature in liquid Pb-Sn alloys", PHYSICA B. CONDENSED MATTER, AMSTERDAM, NL, vol. 358, no. 1-4, 15 April 2005 (2005-04-15), pages 126 - 131, XP004809595, ISSN: 0921-4526, DOI: 10.1016/J.PHYSB.2004.12.037 *
WANG QIANG ET AL: "Electrical resistivity of molten indium-antimony alloys", JOURNAL OF APPLIED PHYSICS, AMERICAN INSTITUTE OF PHYSICS. NEW YORK, US, vol. 87, no. 9, 1 May 2000 (2000-05-01), pages 4623 - 4625, XP012049943, ISSN: 0021-8979, DOI: 10.1063/1.373113 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111965225A (zh) * 2020-07-17 2020-11-20 沈阳广泰真空科技有限公司 一种真空感应熔炼炉中的坩埚监测方法及装置
CN111965225B (zh) * 2020-07-17 2023-09-22 沈阳广泰真空科技股份有限公司 一种真空感应熔炼炉中的坩埚监测方法及装置

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