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EP3714072B1 - Feuillard magnétique à grains orientés et procédé de fabrication d'un tel feuillard magnétique - Google Patents

Feuillard magnétique à grains orientés et procédé de fabrication d'un tel feuillard magnétique Download PDF

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Publication number
EP3714072B1
EP3714072B1 EP18807895.0A EP18807895A EP3714072B1 EP 3714072 B1 EP3714072 B1 EP 3714072B1 EP 18807895 A EP18807895 A EP 18807895A EP 3714072 B1 EP3714072 B1 EP 3714072B1
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EP
European Patent Office
Prior art keywords
strip
melt
electrical steel
peak
ppm
Prior art date
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EP18807895.0A
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German (de)
English (en)
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EP3714072A1 (fr
Inventor
Christian Hecht
Carsten Schepers
Andreas Allwardt
Ludger Lahn
Heiner Schrapers
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ThyssenKrupp Electrical Steel GmbH
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ThyssenKrupp AG
ThyssenKrupp Electrical Steel GmbH
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1277—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties involving a particular surface treatment
    • C21D8/1283—Application of a separating or insulating coating
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
    • C21D1/76—Adjusting the composition of the atmosphere
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1244—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest
    • C21D8/1255—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest with diffusion of elements, e.g. decarburising, nitriding
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1244—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest
    • C21D8/1272—Final recrystallisation annealing
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1277—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties involving a particular surface treatment
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1277—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties involving a particular surface treatment
    • C21D8/1288—Application of a tension-inducing coating
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/52—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for wires; for strips ; for rods of unlimited length
    • C21D9/54—Furnaces for treating strips or wire
    • C21D9/56—Continuous furnaces for strip or wire
    • C21D9/561—Continuous furnaces for strip or wire with a controlled atmosphere or vacuum
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/001—Ferrous alloys, e.g. steel alloys containing N
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/16—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of sheets
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D2201/00—Treatment for obtaining particular effects
    • C21D2201/05—Grain orientation

Definitions

  • the present invention relates to a grain-oriented electrical steel strip with a magnesium silicate layer on at least one surface, wherein in a DRIFT spectrum of the magnesium silicate layer there is at least one peak in the range 960 to 975 cm-1 (A) and at least one peak in the range 976 to 990 cm-1 (B), wherein the peak height of the at least one peak in the range (A) is higher than the peak height of the at least one peak in the range (B), a method for its production under certain atmospheric conditions in the annealing step and the use of such an electrical steel strip.
  • the invention makes it possible to optimize the nitrogen level during a bell annealing process carried out in the course of the inventive method.
  • EP 1 025 268 B1 discloses a method for producing grain-oriented electrical steel, which is annealed to recrystallize and decarburize after a hot rolling step and a cold rolling step, then provided with an annealing separator and finally annealed.
  • the setting of a specific annealing atmosphere is not disclosed in this document.
  • WO 2017/037019 A1 also discloses a method for producing grain-oriented electrical steel strip.
  • This method includes an annealing step after cold rolling the electrical steel strip, during which an oxide layer forms on the surface. This oxide layer is examined using FTIR spectroscopy. The FTIR examination is then used to determine the area ratio between Fe2SiO4 and ⁇ SiO2 in the layer.
  • a certain ratio of the maximum temperature reached in the annealing step and the dew point of the atmosphere in the annealing step is to be maintained.
  • EP 1752548 A1 and EP 1752549 A1 disclose processes for producing grain-oriented electrical steel strip. These processes also each comprise an annealing step in which the cold-rolled electrical steel strip is annealed to recrystallize and decarburize, and which preferably takes place in an ammonia atmosphere.
  • EP 0 699 771 A1 , CN 102 758 127 B and EP 0947 597 A2 disclose processes for producing grain-oriented electrical steel strip, each of which comprises an annealing step. None of these documents discloses adjusting the annealing conditions in such a way that the high-temperature annealing results in an N content of ⁇ 14/27 x Al sl in the electrical steel strip.
  • nitridic phase When producing grain-oriented electrical steel, it is important to control the nitridic phase during the annealing process, as it can interact with the annealing atmosphere even at temperatures below the secondary crystallization temperature.
  • a nitridic phase that is set too low results in too low an inhibition effect and, as a result, higher remagnetization losses, while a nitridic phase that is set too high can shift the secondary crystallization temperature above the inhibitor dissolution temperature and also cause a inhomogeneous forsterite layer is created, which can lead to insufficient interlocking and thus to a deteriorated adhesive strength.
  • the object of the present invention is therefore to provide a grain-oriented electrical steel strip which has an optimized combination of low magnetic reversal losses and good adhesive strength of the forsterite layer on the surface. Furthermore, it is an object of the present invention to provide a method for producing a corresponding grain-oriented electrical steel strip.
  • electrical strip is understood to mean an electrical sheet produced by rolling suitably composed steel, as well as cut pieces thereof, which are intended for the manufacture of parts for electrical engineering applications. Grain-oriented electrical strips of the type in question here are particularly suitable for uses in which a particularly low remagnetization loss is of primary importance and high demands are placed on permeability or polarization. Such requirements exist in particular for parts for power transformers, distribution transformers, high-quality small transformers or in rotating electrical machines.
  • the process according to the invention can include further work steps that are not required in the conventional production of Electrical steel strips can be subjected to various treatments to achieve optimized magnetic properties or properties that are important for practical use. These include, for example, reheating the pre-product obtained after the steel has been cast, descaling the hot strip before cold rolling or, in the case of multi-stage cold rolling, intermediate annealing carried out in the conventional manner between the cold rolling stages.
  • a steel melt is melted which (each in wt. %) optionally contains 0.005 to 0.5 Cu, 0.005 to 0.060 S and also optionally 0 to 0.3 Cr, Mn, Ni, Mo, P, As, Sn, Sb, Se, Te, B or Bi, the remainder being iron and unavoidable impurities.
  • Step (A) of the process according to the invention can be carried out by any method known to the person skilled in the art.
  • a steel melt with a known composition is melted.
  • This melt is then treated using secondary metallurgy.
  • This treatment is preferably initially carried out in a vacuum system in order to adjust the chemical composition of the steel within the required narrow analysis ranges and to achieve preferably low hydrogen contents of a maximum of 10 ppm in order to reduce the risk of strand breakages when pouring the molten steel to a minimum.
  • step (A) it would also be possible to initially use a ladle furnace for slag conditioning, followed by treatment in a vacuum system to adjust the chemical composition of the molten steel within narrow analysis limits.
  • this combination has the disadvantage that in the event of pouring delays, the temperature of the melt drops so far that the molten steel can no longer be poured.
  • step (A) it is also possible to use only the ladle furnace.
  • this has the disadvantage that the accuracy of the analysis is not as good as with treatment in a vacuum system and, in addition, high hydrogen contents can occur in the casting melt with the risk of strand breakages.
  • step (A) it is further preferred to use only the vacuum system in step (A).
  • step (B) of the method according to the invention the steel melt produced in step (A) is then cast to form a starting material.
  • this starting material can be, for example, a slab, a thin slab or a cast strip.
  • a strand is preferably first produced from the melt by casting.
  • the aim is to avoid the formation of nitride precipitations before and during hot rolling as far as possible in order to be able to make extensive use of the possibility of a controlled generation of such precipitations during cooling of the hot strip.
  • it is preferred to carry out an inline thickness reduction of the strand cast from the melt but still in the liquid state.
  • LCR Liquid Core Reduction
  • SR Soft Reduction
  • SR is understood to mean the targeted reduction in the thickness of the strand in the tip of the slurry near the final solidification.
  • the aim of SR is to reduce central segregation and core porosity.
  • the reduction in central silicon segregation in the subsequently hot-rolled pre-products that can be achieved by SR enables the chemical composition to be evened out across the strip thickness, which is beneficial for the magnetic values.
  • Good results from SR are obtained when the thickness reduction achieved when using SR is, for example, 0.5 to 5 mm.
  • the following specification can serve as a guide for the time at which SR is used in connection with the continuous casting carried out according to the invention: start of the SR zone at a degree of solidification fs of 0.2 and end of the SR zone at fs equal to 0.7 to 0.8.
  • thin slabs are preferably produced in step (B) of the method according to the invention.
  • the strand that usually emerges vertically from the casting mold is bent at lower points and guided in a horizontal direction.
  • the strand cast from the melt is bent and straightened at a temperature of 700 to 1000 °C, preferably 850 to 950 °C, which means that cracks on the surface of the thin slabs separated from the strand can be avoided, which can otherwise occur, in particular as a result of edge cracks in the strand.
  • the steel used according to the invention has good ductility on the surface of the strand or in the edge area, so that it can easily follow the deformations that occur during bending and straightening. Thin slabs are separated from the strand cast in a manner known per se.
  • Step (C) of the method according to the invention comprises hot rolling the starting material from step (B), in particular the thin slabs produced, to form a hot strip.
  • the starting material obtained in step (B), in particular a thin slab is preferably heated in a furnace to the appropriate hot rolling starting temperature and then fed to the hot rolling.
  • the temperature at which the starting material, in particular a thin slab, enters the furnace is preferably above 650 °C.
  • the residence time in the furnace should be less than 60 minutes in order to avoid sticky scale.
  • the hot rolling in step (C) is carried out after the first forming pass in the two-phase region ( ⁇ / ⁇ ).
  • This measure also aims to reduce the formation of nitride precipitations as much as possible during hot rolling in order to be able to control these precipitations in a targeted manner via the cooling conditions on the run-out roller table behind the last rolling stand of the hot strip mill.
  • hot rolling is preferably carried out at temperatures at which austenitic and ferritic components are mixed in the structure of the hot strip. Typical temperatures at which this is the case for the steel alloys used according to the invention are above around 800 °C, in particular in the range from 850 to 1150 °C. In the ⁇ phase, the AIN is kept in solution at these temperatures.
  • Another positive aspect of hot rolling in the two-phase mixed region is the grain refinement effect.
  • austenite By converting the austenite into ferrite after the hot rolling passes, a finer-grained and more homogeneous hot strip structure is achieved, which has a positive effect on the magnetic properties of the end product.
  • the avoidance of nitride precipitation during hot rolling is further supported, for example, by the fact that a degree of deformation of at least 40% is achieved in the first forming pass, so that only relatively small pass reductions are necessary in the last stands to achieve the desired final strip thickness.
  • the total degree of deformation achieved over the first two forming passes is more than 60%, wherein in a further advantageous embodiment of the invention a degree of deformation of more than 40% is achieved in the first stand of the finishing train and the pass reduction in the second stand of the finishing train is more than 30%.
  • the pass reduction in the last stand should preferably be limited to a maximum of 30%, particularly preferably less than 20%, whereby it is also advantageous for an optimal hot rolling result with regard to the desired properties if the pass reduction in the penultimate stand of the finishing train is less than 25%.
  • the cooling of the hot strip can be carried out by methods known to those skilled in the art, for example by means of water and/or air.
  • Step (D) of the method according to the invention comprises the winding of the hot strip obtained in step (C) into a coil.
  • Corresponding methods for winding a hot strip are known per se to the person skilled in the art.
  • the coiling temperature should preferably be in the temperature range of 500 to 780 °C. Temperatures above this would lead to undesirably coarse precipitations and would also impair pickling properties. To set higher coiling temperatures of over 700 °C, a so-called short-distance coiler is preferably used, which is arranged directly after the compact cooling zone.
  • the process according to the invention is preferably carried out in the production of the hot strip in such a way that the hot strip obtained has sulfidic and/or nitridic precipitations with an average particle diameter of less than 150 nm and an average density of at least 0.05 ⁇ m-2.
  • a hot strip of this type has optimal conditions for the effective control of grain growth during the subsequent process steps.
  • the thickness of the hot strip obtained according to the invention is preferably 1.5 to 3.5 mm, particularly preferably 2 to 2.7 mm.
  • the hot strip thus produced can optionally be annealed after coiling or before cold rolling in order to further optimize the microstructure.
  • step (F) the hot strip is rolled into a cold strip in one or more cold rolling steps.
  • intermediate annealing can be carried out between the cold rolling steps if necessary.
  • the thickness of the cold strip obtained according to the invention is preferably 0.10 to 0.35 mm, particularly preferably 0.15 to 0.23 mm.
  • Step (G) of the process according to the invention comprises annealing the cold strip at a temperature of 700 to 950 °C, preferably 800 to 900 °C.
  • Step (G) of the process according to the invention can in principle be carried out in all devices known to the person skilled in the art.
  • the annealing in step (G) should take place in an atmosphere in which the dew point DP, given in °C, corresponds to the above equation (1).
  • Alsl here means the content of aluminum in the melt that was used in step (A) of the process according to the invention.
  • the unit of Alsl is ppm.
  • Alsl is 200 to 400 ppm according to the invention.
  • N(melt) means the nitrogen content in the melt that was used in step (A) of the process according to the invention.
  • the unit of N(melt) is ppm.
  • N(melt) is according to the invention 20 to 200 ppm, preferably 40 to 150 ppm, very particularly preferably 60 to 120 ppm.
  • the dew point DP is 20 to 90 °C, particularly preferably 30 to 70 °C.
  • the dew point DP set in step results in the nitrogen concentration N in the material after step (G) according to equation (2) 2 / 3 * Alsl * 14 / 27 ⁇ 0,7 * DP ⁇ N ⁇ Alsl * 14 / 27 + N Schmelze
  • N means the nitrogen content in the material after step (G) in ppm.
  • the unit of N is ppm.
  • the nitrogen content in the material after step (G) is N 70 to 180 ppm, particularly preferably 90 to 160 ppm.
  • Step (G) of the process according to the invention is preferably carried out in a nitrogen-containing atmosphere.
  • step (G) is preferably carried out in the presence of ammonia, nitrogen and/or hydrogen.
  • the corresponding amounts are known per se to the person skilled in the art.
  • the ammonia-containing atmosphere can be present in the entire furnace part, or preferably only in the last furnace part.
  • step (G) of the method according to the invention By carrying out step (G) of the method according to the invention under certain conditions with regard to the dew point of the furnace atmosphere and the nitrogen concentration in the material after step (G), it is possible according to the invention to provide a grain-oriented electrical steel strip which characterized by particularly low magnetic reversal losses and particularly good adhesion of the forsterite layer (magnesium silicate layer) which is formed in step (I) of the process according to the invention.
  • the conditions which are set in step (G) result in a specific nitrogen content in the material after step (G), the relationship being given by formulas (I) and (II).
  • This results in a specific, particularly advantageous nitrogen content of the material in step (I) of the process according to the invention at a temperature of 700 to 900 °C. This is preferably less than 14/27*Alsl of the melt.
  • a grain-oriented electrical steel strip which has a magnesium silicate layer on at least one surface which, in a DRIFT spectrum, shows at least one peak in the range from 960 to 975 cm-1 (A) and at least one peak in the range from 976 to 990 cm-1.
  • the ratio of the peaks to one another is influenced by the denitrification and nitriding processes during step (I), wherein, in the embodiment according to the invention, the peak height of the at least one peak in the range (A) is higher than the peak height of the at least one peak in the range (B).
  • an annealing separator layer is applied to at least one surface of the cold strip from step (G); preferably, such an annealing separator layer is applied to both surfaces of the cold strip from step (G).
  • the annealing separator is typically MgO.
  • the annealing separator prevents the turns of a coil wound from the cold strip from welding together during subsequent high-temperature annealing.
  • Step (I) of the method according to the invention comprises high-temperature annealing of the cold strip coated with the annealing separator to form a forsterite layer on the surface of the annealed cold strip.
  • Step (I) of the method according to the invention is typically carried out in a bell furnace under protective gas, preferably at a temperature of 650 to 950 °C. This creates a microstructure in the cold strip through selective grain growth that contributes significantly to the magnetic properties.
  • a forsterite layer often referred to as a "glass film” in the specialist literature, forms on the strip surfaces during the high-temperature annealing.
  • the steel material is cleaned by diffusion processes that take place during the high-temperature annealing.
  • the nitrogen content of the material after step (G) is set to 200 ppm, for example. According to the invention, however, this nitrogen value is only an auxiliary value; rather, according to the invention, the nitrogen value is controlled in the temperature range from 700 to 900 °C in step (I) and set so that it is below 14/27*Alsl.
  • the optional step (J) of the method according to the invention comprises the application of an insulating layer to the surface having the forsterite layer of the cold strip.
  • Suitable materials that can act as an insulating layer are, for example, phosphates, silicates or mixtures of these.
  • the corresponding processes are known to the person skilled in the art.
  • the cold strip obtained from step (J) of the process according to the invention can be thermally straightened. Appropriate processes for this are also known to the person skilled in the art.
  • the optional step (K) of the method according to the invention comprises a final annealing of the cold strip produced according to the invention.
  • stress relief annealing the cold strip is annealed to relieve stress.
  • This final annealing can take place before or after the flat steel product produced in the manner described above has been made into the blanks required for further processing.
  • the additional stresses that have arisen during the severing process can be reduced by a final annealing, which is carried out after the blanks have been separated.
  • the grain-oriented electrical steel produced according to the invention is characterized in that it has low remagnetization losses and, due to a high degree of interlocking of the forsterite layer with the surface of the electrical steel, a good adhesion of the forsterite layer.
  • the present invention therefore also relates to a grain-oriented electrical steel that can be produced by the method according to the invention.
  • the present invention also relates to grain-oriented electrical steel with a magnesium silicate layer on at least one surface, wherein in a DRIFT spectrum of the magnesium silicate layer there is at least one peak in the range 960 to 975 cm-1 (A) and at least one peak in the range 976 to 990 cm-1 (B), wherein the peak height of the at least one peak in the range (A) is higher than the peak height of the at least one peak in the range (B).
  • the electrical steel according to the invention is obtained by the process according to the invention.
  • DRIFT diffuse reflection Fourier transform infrared spectroscopy
  • an IR light beam is directed onto the sample surface using concave mirrors and the reflected light is also detected using concave mirrors, see for example Beasley et al., "Comparison of transmission FTIR, ATR and DRIFT sprecta,” Journal of Archeological Science, Vol. 46, June 2014, pages 16 to 2 ).
  • This enables the evaluation of deeper oxide layers and thus a more in-depth analysis of the molecular components in the oxide layer.
  • the electrical steel strip according to the invention is characterized in that it has a magnesium silicate layer, i.e. a so-called forsterite layer, which has at least two peaks in a DRIFT spectrum of this layer, firstly at least one peak in a wave number range from 960 to 975 cm-1 (region (A)), and secondly at least one peak in a wave number range from 976 to 990 cm-1 (region (B)). Furthermore, the peak height of the at least one peak in region (A) is higher than the peak height of the at least one peak in region (B). In the context of the present invention, "higher” means that the at least one peak in region (A) is at least 5%, preferably at least 30%, higher than the at least one peak in region (B).
  • the ratio of the peak height of the at least one peak in the region (A) to the peak height of the at least one peak in the region (B) is greater than 1.0, preferably greater than or equal to 1.05, particularly preferably greater than or equal to 1.3.
  • the present invention further preferably relates to the electrical steel strip according to the invention, wherein an annealing separator layer is present on at least one surface, preferably such an annealing separator layer is present on both surfaces.
  • the forsterite layer of the electrical steel strip according to the invention which has at least the two characteristic peaks mentioned, shows an advantageous particularly strong interlocking with the surface of the electrical steel strip. Furthermore, the electrical steel strip according to the invention shows particularly low remagnetization losses
  • the electrical steel strip according to the invention is particularly suitable for use in power transformers, distribution transformers, small transformers or in rotating electrical machines.
  • the present invention therefore further relates to the use of the electrical steel according to the invention in power transformers, distribution transformers, small transformers or in rotating electrical machines.
  • Grain-oriented electrical strips 1 to 14 were produced by the following steps: melting a steel melt containing the alloying elements specified in Table 1, pouring the steel melt into a thin slab, hot rolling the thin slab at a temperature of 1050 °C into a hot strip, coiling the hot strip at a temperature of 700 °C into a coil, cold rolling the hot strip in 5 steps to a thickness between 0.23 and 0.3 mm, annealing the cold rolled strip at a temperature of 700 to 900 °C according to the process parameters given in Table 2.
  • the electrical steel strip according to the invention can be used in power transformers, distribution transformers, small transformers or in rotating electrical machines.
  • Table 1 Compositions of the melts used, ⁇ /b> remainder Fe and unavoidable impurities No. Si Mn C Cu S Cr P Al sl N [%] [ppm] 1 3.13 0.08 346 152 42 1314 668 263 119 2 3.10 0.27 472 184 119 646 680 272 91 3 2.97 0.12 387 76 78 367 530 292 95 4 3.32 0.31 344 107 36 2274 563 317 79 5 3.16 0.17 444 231 120 1346 555 269 89 6 3.30 0.23 335 149 40 685 308 282 126 7 3.12 0.09 329 86 35 1114 358 276 117 8 3.04 0.09 420 217 98 1711 501 287 73 9 3.12 0.34 336 241 80 1767 772 297 107 10 3.36 0.07 482 212 72

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Claims (10)

  1. Procédé de fabrication d'un feuillard électrique à grains orientés, comprenant au moins les étapes suivantes :
    (A) fusion d'un acier liquide qui contient (respectivement en % en poids) 2,0 à 4,0 de Si, 0,010 à 0,100 de C, 0,0200 à 0,0400 de AIsl (avec AIsl = AI soluble dans l'acide) et 0,0020 jusqu'à 0,02 de N, ainsi que, respectivement éventuellement, jusqu'à 0,5 de Cu, jusqu'à 0,060 de S et, éventuellement également, jusqu'à 0,3 de Cr, Mn, Ni, Mo, P, As, Sn, Sb, Se, Te, B ou Bi, reste de fer et impuretés inévitables,
    (B) coulage de l'acier liquide en un produit primaire, tel qu'une brame, une brame mince ou un feuillard coulé,
    (C) laminage à chaud du produit primaire en un feuillard à chaud,
    (D) dévidage du feuillard à chaud en une bobine,
    (E) recuit éventuel du feuillard à chaud
    (F) laminage à froid du feuillard à chaud en une ou plusieurs étapes de laminage à froid en un feuillard à froid,
    (G) recuit du feuillard à froid de l'étape (F) à une température allant de 700 à 950 °C,
    (H) application d'une couche de séparateur de recuit sur au moins une surface du feuillard à froid de l'étape (G),
    (I) recuit à haute température du feuillard à froid revêtu du séparateur de recuit en réalisant une couche de forstérite sur la surface du feuillard à froid recuit,
    (J) application éventuelle d'une couche isolante sur la surface du feuillard à froid présentant la couche de forstérite, et
    (K) recuit final éventuel du feuillard à froid
    caractérisé en ce que l'étape (G) est effectuée dans une atmosphère dont le point de rosée DP est de 20 °C à 90 °C et qui satisfait à l'équation (1) suivante Alsl / N masse fondue * 10 < DP < Alsl / N masse fondue * 30
    Figure imgb0008
    de sorte qu'une teneur en azote N allant de 70 à 180 ppm est présente dans le produit après l'étape (G), laquelle teneur satisfait à l'équation (2) suivante 2 / 3 * Alsl * 14 / 27 − 0,7 * DP < N < Alsl * 14 / 27 + N masse fondue
    Figure imgb0009
    et, pendant le recuit à haute température selon l'étape de travail (I) dans la plage de températures allant de 700 à 900 °C, la teneur en azote du feuillard électrique est contrôlée de sorte qu'une teneur en azote est présente dans le feuillard électrique, laquelle est inférieure à 14 / 27 x AIsl, où
    Alsl représente la teneur en aluminium (soluble dans l'acide) dans la masse fondue exprimée en ppm,
    N(masse fondue) représente la teneur en azote de la masse fondue exprimée en ppm,
    DP représente le point de rosée exprimé en °C et
    N représente la teneur en azote dans le produit après l'étape (G) exprimée en ppm.
  2. Procédé selon la revendication 1, caractérisé en ce que le point de rosée DP est de 30 à 70 °C.
  3. Procédé selon la revendication 1 ou 2, caractérisé en ce que la teneur en aluminium Alsl est de 240 à 340 ppm.
  4. Procédé selon l'une des revendications 1 à 3, caractérisé en ce que la N(masse fondue) est de 40 à 150 ppm.
  5. Procédé selon la revendication 4, caractérisé en ce que N(masse fondue) est de 60 à 120 ppm.
  6. Procédé selon l'une des revendications 1 à 5, caractérisé en ce que la teneur en azote dans le produit après l'étape (G) est de 90 à 160 ppm.
  7. Feuillard électrique à grains orientés qui peut être obtenu par le procédé selon l'une des revendications 1 à 6, comportant une couche de silicate de magnésium sur au moins une surface, caractérisé en ce que, dans un spectre DRIFT de la couche de silicate de magnésium, au moins un pic est présent dans la plage allant de 960 à 975 cm-1 (A) et au moins un pic est présent dans la plage allant de 976 à 990 cm-1 (B), dans lequel la hauteur de pic de l'au moins un pic dans la plage (A) est supérieure à la hauteur de pic de l'au moins un pic dans la plage (B).
  8. Feuillard électrique selon la revendication 7, caractérisé en ce que le rapport de la hauteur de pic de l'au moins un pic dans la plage (A) à la hauteur de pic de l'au moins un pic dans la plage (B) est supérieur à 1,05.
  9. Feuillard électrique selon l'une des revendications 7 ou 8,
    caractérisé en ce qu'une couche de séparateur de recuit est présente sur au moins une surface.
  10. Utilisation d'un feuillard électrique à grains orientés, procuré selon l'une des revendications 7 à 9, pour la fabrication de pièces pour transformateurs de puissance, transformateurs de distribution, petits transformateurs ou machines électriques rotatives.
EP18807895.0A 2017-11-20 2018-11-12 Feuillard magnétique à grains orientés et procédé de fabrication d'un tel feuillard magnétique Active EP3714072B1 (fr)

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DE102017220714.0A DE102017220714B3 (de) 2017-11-20 2017-11-20 Optimierung des Stickstofflevels während der Haubenglühung
PCT/EP2018/080928 WO2019096736A1 (fr) 2017-11-20 2018-11-12 Feuillard magnétique à grains orientés et procédé de fabrication d'un tel feuillard magnétique

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US5472521A (en) * 1933-10-19 1995-12-05 Nippon Steel Corporation Production method of grain oriented electrical steel sheet having excellent magnetic characteristics
KR0157539B1 (ko) * 1994-05-13 1998-11-16 미노루 다나까 우수한 반응성을 가진 방향성 전기강판용 아닐링 분리제 및 이의 사용방법
JP3390102B2 (ja) * 1995-03-02 2003-03-24 新日本製鐵株式会社 グラス被膜の良好な方向性電磁鋼板の製造方法
DE19745445C1 (de) 1997-10-15 1999-07-08 Thyssenkrupp Stahl Ag Verfahren zur Herstellung von kornorientiertem Elektroblech mit geringem Ummagnetisierungsverlust und hoher Polarisation
DE69923102T3 (de) * 1998-03-30 2015-10-15 Nippon Steel & Sumitomo Metal Corporation Verfahren zur Herstellung eines kornorientierten Elektrobleches mit ausgezeichneten magnetischen Eigenschaften
SI1752548T1 (sl) 2005-08-03 2016-09-30 Thyssenkrupp Steel Europe Ag Metoda za proizvodnjo magnetnega zrnato usmerjenega jeklenega traku
SI1752549T1 (sl) 2005-08-03 2016-09-30 Thyssenkrupp Steel Europe Ag Postopek za proizvodnjo zrnato usmerjene magnetne jeklene vzmeti
CN101768697B (zh) * 2008-12-31 2012-09-19 宝山钢铁股份有限公司 用一次冷轧法生产取向硅钢的方法
CN102758127B (zh) * 2011-04-28 2014-10-01 宝山钢铁股份有限公司 具有优异磁性能和良好底层的高磁感取向硅钢生产方法
CN103695619B (zh) * 2012-09-27 2016-02-24 宝山钢铁股份有限公司 一种高磁感普通取向硅钢的制造方法
DE102015114358B4 (de) 2015-08-28 2017-04-13 Thyssenkrupp Electrical Steel Gmbh Verfahren zum Herstellen eines kornorientierten Elektrobands und kornorientiertes Elektroband

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