US20180237876A1 - Method for producing a grain-oriented electrical steel strip and grain-oriented electrical steel strip - Google Patents

Method for producing a grain-oriented electrical steel strip and grain-oriented electrical steel strip Download PDF

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US20180237876A1
US20180237876A1 US15/754,143 US201615754143A US2018237876A1 US 20180237876 A1 US20180237876 A1 US 20180237876A1 US 201615754143 A US201615754143 A US 201615754143A US 2018237876 A1 US2018237876 A1 US 2018237876A1
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strip
weight
annealing
cold
area
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Christian Hecht
Ludger Lahn
Carsten Schepers
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ThyssenKrupp Electrical Steel GmbH
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ThyssenKrupp Electrical Steel GmbH
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Assigned to THYSSENKRUPP ELECTRICAL STEEL GMBH reassignment THYSSENKRUPP ELECTRICAL STEEL GMBH ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: HECHT, CHRISTIAN, LAHN, LUDGER, SCHEPERS, CARSTEN
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    • 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
    • C21D8/1261—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 following hot rolling
    • 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
    • C21D8/1266—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 between cold rolling steps
    • 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
    • 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
    • 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
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • 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
    • 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
    • C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • 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
    • 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 invention relates to a method of producing a grain-oriented electrical steel strip and to a grain-oriented electrical steel strip.
  • electrical steel strips this means electrical steel sheets and electrical steel strips produced by rolling steels of suitable composition, and circuit boards or blanks that have been divided therefrom, which are intended for the production of parts for electrical engineering applications.
  • Grain-oriented electrical steel strips of the type in question here are especially suitable for uses in which the emphasis is on a particularly low cyclic magnetization loss and high demands are made on permeability or polarization. Such demands exist especially in the case of parts for power transformers, distribution transformers and higher-quality small transformers.
  • a steel comprising (in % by weight) typically 2.5% to 4.0% Si, 0.010% to 0.100% C, up to 0.150% Mn, up to 0.065% Al and up to 0.0150% N, and in each case optionally 0.010% to 0.3% Cu, to 0.060% S, to 0.100% P, and to in each case 0.2%
  • the preliminary material is then, if required, subjected to an annealing treatment and then hot-rolled to give a hot strip.
  • the resultant hot strip is coiled to give a coil and can then, if required, be subjected to annealing and to a likewise optionally executed descaling or pickling treatment. Then a cold strip is rolled from the hot strip in one or more stages, with performance of intermediate annealing if required between the cold rolling steps in a multistage cold rolling operation effected in multiple steps.
  • the resultant cold strip then typically undergoes a decarburization anneal, in order to minimize the carbon content of the cold strip for avoidance of magnetic aging.
  • an annealing separator is applied to the strip surfaces, which typically comprises MgO.
  • the annealing separator prevents the windings of a coil wound from the cold strip from being welded to one another in a subsequently conducted high-temperature anneal.
  • a forsterite layer forms on the strip surfaces during the high-temperature anneal, often also referred to in the technical literature as “glass film”.
  • the steel material is cleaned by diffusion processes that proceed during the high-temperature anneal.
  • the flat steel product having the forsterite layer which is obtained in this way is coated with an insulation layer, thermally aligned and subjected to stress-relief annealing in a concluding “final anneal”.
  • This final anneal can be effected before or after the finishing of the flat steel product produced in the manner described above to give the blanks required for further processing.
  • the additional stresses that have arisen in the course of the dividing operation can be dissipated.
  • Electrical steel strips produced in such a way generally have a thickness of 0.15 mm to 0.5 mm.
  • the domain structure can additionally be improved by the application of an insulation layer which exerts a permanent tensile stress on the sheet substrate, and additionally also that by a treatment in which lines of local stresses are generated transverse or oblique to the rolling direction in the flat steel product, the magnetic properties of grain-oriented electrical steel strips can be further improved.
  • Surface structures of this kind can be generated, for example, by local mechanical deformations (EP 0 409 389 A2), laser or electron beam treatments (EP 0 008 385 B1; EP 0 100 638 B1; EP 0 571 705 A2) or etching of trenches (EP 0 539 236 B1).
  • the forsterite film also has an important influence on essential use properties of electrical steel strips. For example, the losses, the noise characteristics in the transformer or else the bond strength of the insulation are affected by the forsterite film between magnetically active base material and insulation layer.
  • the main emphasis in the literature is typically on the interdigitation of the forsterite with the steel substrate, since the adhesion of the composite composed of forsterite film and insulation coating which is formed in the subsequent steps is significantly dependent thereon.
  • JP 2004/191217 A1 has proposed improving the bond strength of the insulation layer by optimizing the uppermost oxide layer by means of examinations on the basis of Fourier transform infrared spectrometry “FTIR”.
  • FTIR Fourier transform infrared spectrometry
  • an infrared beam is guided onto the surface at a defined angle and the directed reflection is measured. Since multiple reflections occur within the material, depending on the angle of incidence, it is possible to measure only the uppermost portion of the oxide layer. Therefore, this method can permit only conclusions about the bond strength; it is not possible to use it to determine other properties, for example the later tensile strength.
  • the problem addressed was that of specifying a method of producing grain-oriented electrical steel strips with which the surface constitution of the respective flat steel product can be adjusted in a controlled manner prior to the application of the annealing separator such that a forsterite film with optimal effect in terms of the magnetic properties of the electrical steel strip to be produced is obtained.
  • the invention has solved this problem by following the procedure of the method specified in claim 1 in the production of grain-oriented electrical steel strips.
  • the method of the invention may comprise further steps which are conducted in the conventional production of electrical steel strips in order to achieve optimized magnetic properties or properties that are important for practical use. These include, for example, reheating of the precursor obtained after the casting of the steel, descaling of the hot strip prior to the cold rolling or, in the case of the multistage performance of cold rolling, intermediate annealing conducted in a conventional manner between the cold rolling stages in each case.
  • the invention proceeds here from the finding that, firstly, the bond strength of the forsterite film on the steel substrate is controlled solely by the uppermost atomic layers of the oxide layer, whereas the stress transmitted to the base material can be modified only within certain limits.
  • the oxide layer is characterized by means of “diffuse reflectance Fourier transformation infrared spectroscopy”, also referred to as “DRIFT method” for short.
  • DRIFT method an IR light beam is directed onto the sample surface by means of concave mirrors and the reflected light is also detected by means of concave mirrors (see Beasley et al., “Comparison of transmission FTIR, ATR and DRIFT spectra”, Journal of Archeological Science, Vol. 46, June 2014, pages 16-22). This enables the evaluation of deeper-lying oxide layers and hence a deeper analysis of the molecular components in the oxide layer.
  • the process parameters in the subsequent processing of the flat steel products are then adjusted such that an oxide layer favorable for the formation of an optimally adhering forsterite film that simultaneously exerts optimally high tensile stresses is formed on the steel substrate.
  • the analysis of the DRIFT spectrum of the oxide layer present on the surface of the flat steel product after the cold rolling should be checked continuously in order firstly to detect the quality of the oxide film across the entire surface of the flat steel product in question for each batch of electrical steel strips.
  • the information derived in accordance with the invention from the DRIFT spectrum allows optimization of the results in the production of subsequent batches of electrical steel strips. If the DRIFT spectrum shows that the ratio of the proportions of ⁇ -SiO 2 and fayalite (Fe 2 SiO 4 ) molecules does not meet the specifications of the invention, for this purpose, the process steps in the method of the invention that have been implemented up to the application of the annealing separator are adjusted.
  • the steel analysis, the parameters for the hot strip anneal, the parameters for the cold rolling and the parameters for the oxidation/primary recrystallization anneal are adjusted such that the condition set in accordance with the invention for the molecular proportions that show in the DRIFT spectrum
  • the oxidation/primary recrystallization anneal can be combined in a manner known in practice with a decarburization anneal, in which the carbon content of the steel substrate is minimized, and a nitriding treatment which is likewise optionally conducted in a manner known per se, which has the aim of increasing the nitrogen content of the steel substrate.
  • the area( ⁇ SiO 2 ) and area(Fe 2 SiO 4 ) can be determined here for the peaks representing the proportion of the ⁇ SiO 2 and Fe 2 SiO 4 molecules in a manner known per se (see Foley, “Equations for chromatographic peak modeling and calculation of peak area”, Analytical Chemistry, Vol. 59, Aug. 1, 1987, pages 1984-1985) as the area enclosed by the respective peak and its baseline, the start and end of the baseline being determined by the two foot points F1, F1′; F2, F2′ of the respective peak, i.e. the points where the line of the spectrum gives way to the respective peak (see FIG. 1 ).
  • the cold rolling (step f)) is conducted in at least three cold rolling steps, typically with an intermediate anneal between the cold rolling steps in a manner known per se, in order to eliminate the cold solidifications that arise in each preceding cold rolling step and to assure rollability for the subsequent rolling step.
  • the hot strip is likewise optionally subjected to a hot strip anneal in a manner which is likewise known, in order to assure optimal cold rollability.
  • the character of the oxide layer on the cold strip obtained after the cold rolling can then be influenced via the steel composition smelted in step a) and the adjustment of the parameters for the optional hot strip anneal, for the cold rolling and for the oxidation/primary recrystallization anneal, taking account of the inventive measure that follows in each case, where the measures in question can be utilized in combination with one another or alternatively to one another:
  • an index kOx is determined by the formula
  • the parameter ⁇ 1150 is the percentage alpha/gamma conversion, which is elucidated in detail in EP0600181.
  • an oxide layer produced in accordance with the invention enhances the diffusion of nitrogen into the steel base material when the steel substrate processed in accordance with the invention is subjected to a nitriding process as described, for example, in EP 0 950 120 A1.
  • Suitable annealing separators for the purposes of the invention are especially those conventional annealing separators which consist predominantly, i.e. typically to an extent of at least 85% by weight, of MgO.
  • step i a particularly advantageous high-temperature annealing method in relation to the desired optimization of the magnetic properties and the practical utility of electrical steel strips produced in accordance with the invention has been found to be a high-temperature anneal (step i)) conducted in the form of a bell anneal.
  • the temperatures for the high-temperature anneal are typically in the temperature range of 1000-1250° C. known per se for this purpose.
  • a grain-oriented electrical steel strip of the invention comprises a cold-rolled steel substrate consisting of a steel comprising (in % by weight) 2.0-4.0% Si, up to 0.100% C, up to 0.065% Al and up to 0.020% N, and in each case optionally up to 0.5% Cu, up to 0.060% S and likewise optionally in each case up to 0.3% Cr, Mn, Ni, Mo, P, As, Sn, Sb, Se, Te, B or Bi, the balance being iron and unavoidable impurities, wherein a forsterite film present on said steel substrate features a higher peak at the wavenumber of 977 cm ⁇ 1 than at the wavenumber of 984 cm ⁇ 1 in a spectrum recorded by means of diffuse reflectance Fourier transformation infrared spectroscopy.
  • An electrical steel strip of this kind can especially be produced by employing the method of the invention.
  • the carbon content of the electrical steel strip having the characteristics of the invention is typically at least 0.01% by weight, but may also be lower as a result of the process steps implemented in the course of its production, especially in the case of corresponding performance of the optional decarburization anneal.
  • FIG. 1 DRIFT spectra of oxide layers present on an inventive sample and a noninventive sample
  • FIG. 2 DRIFT spectra of forsterite films present on an inventive sample and a noninventive sample.
  • the thin slabs After reheating to a reheating temperature of typically 1170° C., the thin slabs have been hot-rolled to give a hot strip having a thickness of typically 2.3 mm, which has then been coiled to give a coil.
  • the coiling temperature was typically 540° C.
  • the respective hot strip has been subjected to a hot strip anneal in which it has been through-heated in each case at a maximum temperature T max under an atmosphere having a maximum dew point Dp max , and after which it has been cooled to room temperature in each case with a cooling rate K.
  • the hot strips have subsequently been cold-rolled in five passes to give a cold strip in each case.
  • the mean surface temperature T ob of the cold strip during the last three cold rolling passes and the total decrease in thickness Ab achieved over the last three cold rolling passes have been determined here.
  • the cold strips obtained after the cold rolling have been subjected to a combined annealing treatment in which a decarburization under an atmosphere with a maximum dew point Dp dec and a maximum annealing temperature T dec , an oxidation/primary recrystallization at a maximum annealing temperature T ox and a maximum dew point Dp ox , and in some selected samples a nitriding treatment at a maximum temperature T nit under an atmosphere with a maximum dew point Dp nit have been conducted.
  • the cold strips that have thus been coated have been subjected to a high-temperature anneal conducted as a bell anneal, the maximum temperature of which was 1200° C.
  • a high-temperature anneal conducted as a bell anneal, the maximum temperature of which was 1200° C.
  • the cold strips have been kept here under an atmosphere consisting to an extent of 75% by volume of hydrogen and of 25% by volume of nitrogen, and finally in a cleaning phase under an atmosphere consisting to an extent of 100% by volume of hydrogen.
  • the tensile stress exerted on the respective steel substrate by the forsterite film obtained on samples 1-28 was typically 6 MPa for the inventive samples.
  • FIG. 1 shows for the inventive sample 11 as a solid line and for the non-inventive sample 18 as a dotted line the DRIFT spectra determined prior to the application of the annealing separator present oxide layer.
  • FIG. 2 shows for the inventive sample 11 as a solid line and for the non-inventive sample 18 as a dotted line the DRIFT spectra determined after the high-temperature anneal present forsterite layer.

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US15/754,143 2015-08-28 2016-08-29 Method for producing a grain-oriented electrical steel strip and grain-oriented electrical steel strip Abandoned US20180237876A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE102015114358.5A DE102015114358B4 (de) 2015-08-28 2015-08-28 Verfahren zum Herstellen eines kornorientierten Elektrobands und kornorientiertes Elektroband
DE102015114358.5 2015-08-28
PCT/EP2016/070316 WO2017037019A1 (de) 2015-08-28 2016-08-29 Verfahren zum herstellen eines kornorientierten elektrobands und kornorientiertes elektroband

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US (1) US20180237876A1 (pl)
EP (1) EP3341500B1 (pl)
JP (1) JP2018532041A (pl)
KR (1) KR20180057632A (pl)
CN (1) CN107922987B (pl)
BR (1) BR112018003100A2 (pl)
DE (1) DE102015114358B4 (pl)
ES (1) ES2781335T3 (pl)
MX (1) MX2018002064A (pl)
PL (1) PL3341500T3 (pl)
PT (1) PT3341500T (pl)
RU (1) RU2719864C2 (pl)
WO (1) WO2017037019A1 (pl)

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US20180274069A1 (en) * 2015-09-25 2018-09-27 Nippon Steel & Sumitomo Metal Corporation Steel sheet
US20220098694A1 (en) * 2019-01-16 2022-03-31 Nippon Steel Corporation Method for manufacturing grain-oriented electrical steel sheet

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DE102017220721A1 (de) 2017-11-20 2019-05-23 Thyssenkrupp Ag Optimierung des Stickstofflevels während der Haubenglühung III
DE102017220718A1 (de) 2017-11-20 2019-05-23 Thyssenkrupp Ag Optimierung des Stickstofflevels während der Haubenglühung II
DE102017220714B3 (de) 2017-11-20 2019-01-24 Thyssenkrupp Ag Optimierung des Stickstofflevels während der Haubenglühung
KR102221606B1 (ko) * 2018-11-30 2021-02-26 주식회사 포스코 방향성 전기강판 및 그의 제조 방법
CN111139407A (zh) * 2020-03-02 2020-05-12 无锡晶龙华特电工有限公司 一种优化的低铁损高磁感取向电工钢生产方法
EP4202067A1 (de) * 2021-12-21 2023-06-28 Thyssenkrupp Electrical Steel Gmbh Verfahren zum erzeugen eines kornorientierten elektrobands und kornorientiertes elektroband
CN115044756A (zh) * 2022-06-14 2022-09-13 无锡普天铁心股份有限公司 一种改善含Bi超高磁感取向硅钢底层附着性的工艺方法

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CN107922987A (zh) 2018-04-17
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CN107922987B (zh) 2020-02-21
WO2017037019A1 (de) 2017-03-09
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BR112018003100A2 (pt) 2018-09-25
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