EP2942417B1 - Procédé de production d'une tôle hautement perméable à grains orientés - Google Patents

Procédé de production d'une tôle hautement perméable à grains orientés Download PDF

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Publication number
EP2942417B1
EP2942417B1 EP15159840.6A EP15159840A EP2942417B1 EP 2942417 B1 EP2942417 B1 EP 2942417B1 EP 15159840 A EP15159840 A EP 15159840A EP 2942417 B1 EP2942417 B1 EP 2942417B1
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EP
European Patent Office
Prior art keywords
annealing
strip
cold
hot
nitriding
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.)
Not-in-force
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EP15159840.6A
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German (de)
English (en)
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EP2942417A1 (fr
Inventor
Thorsten Dr. Krenke
Heiner Schrapers
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ThyssenKrupp Electrical Steel GmbH
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ThyssenKrupp Electrical Steel GmbH
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    • 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
    • H01F1/18—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 with 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
    • C21D8/1244—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
    • 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
    • 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
    • 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

Definitions

  • Grain-oriented electrical tapes or sheets are characterized by a particularly sharp ⁇ 110 ⁇ ⁇ 001> texture, which has an easy magnetization direction parallel to the rolling direction. Such a texture is called after their discoverer also "Goss texture”.
  • Goss texture occurs via a selective anomalous grain growth, which is also called secondary recrystallization.
  • grain growth inhibitors which in technical language are also called “inhibitors” or “inhibitor phase” for short.
  • the inhibitor phase consists of very fine and homogeneously distributed particles of one or more foreign phases.
  • the particles in question have at their Interface to the matrix already has a natural interface energy. This obstructs a grain boundary moving across it, because the further savings in interfacial energy in the overall system are greatly reduced.
  • the inhibitor phase therefore has a central importance for the formation of the Goss texture and, consequently, for the magnetic properties of the respective material.
  • the driving force for grain growth during annealing is the grain boundary energy stored in the microstructure. This is essentially determined by the particle size after the primary recrystallization. Due to the weaker inherent inhibition in the low-heating process, the average primary grain size after decarburization annealing is greater than in the conventional process and subject greater fluctuations due to the cold process. The driving force for abnormal grain growth is thus generally lower.
  • the restoring force is determined by the non-magnetic precipitates (inhibitors) precipitated in the cold strip. It is important to have many finely divided particles present.
  • low-heating method One of the methods for producing KO electrical steel is known as "low-heating method".
  • a suitably composite steel is cast into slabs which, after solidification, are annealed at comparatively low slab preheating temperatures below 1300 ° C, typically at 1250 ° C or below.
  • the relevant particles are not produced in the hot strip, but before, after or during the decarburization annealing or during the heating phase of the final annealing with a wide variety of nitriding.
  • nitriding is carried out after the primary recrystallization, but before the onset of abnormal grain growth.
  • the nitration can be carried out here by an atmosphere with nitriding ability or by a nitrogen-donating adhesive protection additive.
  • silicon nitride nitrides are present near the surface after nitriding ( Materials Science Forum 204-206 (1996), 143-154 ). Due to the lower thermodynamic stability they dissolve during the heating of the annealing.
  • the nitrogen diffuses into the steel matrix and recombines with the free aluminum present there to aluminum nitride ( Materials Science Forum 204-206 (1996), 593-598 ).
  • the aluminum nitrides are then the effective inhibitors of secondary grain growth.
  • HGO material H ighly G rain O riented - material
  • HGO material H ighly G rain O riented - material
  • a general disadvantage of all variants of low-heating processes described here, in which the inhibition by ammonia-containing atmospheres is set, is the composition and morphology of the oxide layer obtained after the nitriding process. It is irrelevant at which temperatures previously decarburized and nitrided.
  • nitrides are precipitated in the near-surface layers and in the oxide layer because the solubility limit of nitrogen in Fe-Si is exceeded.
  • the nitrogen excreted in the nitration zone has a high recombination pressure, so that z. T. molecular nitrogen is precipitated in the grain boundaries of the oxide / nitriding layer ( Z. Werkst. michbeh. Manufacturing 63 (2008), 3 ).
  • the consequence of this phenomenon are cracks and pores in the oxide layer, which adversely affect the oxidation during the glass film formation in the course of the cold strip process.
  • the object of the invention was to provide a method which enables the production of grain-oriented electrical steel with improved surface properties and with which, moreover, the dissolution of the nitrides during the heating phase of the high-annealing can be accelerated.
  • the invention proposes the method specified in claim 1.
  • the invention is therefore based on the conventional processes for the production of KO electrical steel, in which a suitably composed melt is cast into thin slabs and in which the nitration is carried out simultaneously with the decarburization in an ammonia-containing atmosphere at temperatures above 850 ° C.
  • Appropriate procedures are in the EP 1 752 548 A1 , of the EP 1 752 549 A1 , of the EP 0 950 119 B1 and the EP 0 950 120 B1 , the contents of which are hereby incorporated into the present disclosure. From these publications, the usual steps and parameters are known, which is applied and considered by a person skilled in the production of grain-oriented electrical steel and which are also relevant here.
  • the processes described in the above-mentioned publications are supplemented by post-nitriding after nitriding, in which the oxide layer present on the surface and the precipitation zone of the KO electrical strip produced according to the invention are passivated.
  • the cold strip after nitriding (step k) and before application of the annealing separator (step l) undergoes a post-oxidation annealing with an annealing period of 15-180 s and a post-oxidation annealing temperature T NO of 750-900 ° C.
  • FIG. 1 shows schematically according to the invention as a function of the respective Nachoxidationsglühtemperatur for the annealing atmosphere of Nachoxidations opposition to be observed partial pressure range in the stability diagram of the electroband typical oxides fayalite (Fe 2 SiO 4 ) and Wüstit (FeO) (see also ISIJ 9 (1969), 66).
  • nitrides Due to the post-oxidation of the base layer, most of the nitrides are now present in an oxidic environment after annealing.
  • the oxidic environment of the nitrides causes a catalytically driven dissolution during the heating phase of the annealing, whereby a uniform distribution of the nitrogen and thus the inhibitor particles is achieved.
  • the uniform inhibitor distribution has the consequence that the secondary recrystallization is stabilized.
  • the operating parameters set in steps a) to o) of the method according to the invention correspond to the specifications known from the prior art.
  • the temperature of the hot strip during reeling can be 520 - 720 ° C.
  • step j it may be desirable to carry out the recrystallizing and decarburizing annealing and nitriding of the cold strip at a temperature of 800 - 1050 ° C under an annealing atmosphere consisting of 0.1-10% by volume of NH 3 , 30-75% by volume of H 2 and 30-75% by volume of N 2 , the dew point of which is 5-75 ° C. over one Duration of 60 - 300 s is performed.
  • melts S1, S2 have been continuously poured into a 63 mm thick strand.
  • the average residence time was typically 20- 35 minutes.
  • the thin slabs were descaled and hot rolled to a final thickness of 2.3 mm in seven hot rolling steps in a finish hot rolling mill.
  • the hot strips produced from the melt S2 were wound into a coil at a temperature of 630 ° C. and then subjected to a two-stage hot-rolled annealing.
  • the annealing temperature in the first stage of the hot strip annealing was 1100 ° C with an annealing time of 90 s and the annealing temperature in the second stage was 900 ° C with an annealing time of 200 s.
  • a single-stage hot strip annealing at 1050 ° C over a period of 350 s would have been possible.
  • the hot strip was cold rolled in one stage to a cold strip having a final thickness of 0.285 mm.
  • the partial pressure ratio of the annealing atmosphere p H2O / p H2 varies in the range of 0.006-0.44.
  • the oxidation degree changes OO initially obtained in dependence on the partial pressure ratio p H2O / p H2 are in FIG. 3 shown.
  • O initial refers to the oxygen content of the sheets without Nachoxidationsglühung.
  • the post-oxidation annealing has a positive effect on the oxygen content only if the partial pressure ratio p H2O / p H2 is greater than 0.16.
  • Fig. 4a shows by way of example a sectional image of the oxide layer before the post-oxidation treatment
  • the oxide layer becomes more compact through post-oxidation annealing and penetrates into the region of nitridic precipitates.
  • the sheets are then coated with magnesium oxide and finally annealed under an atmosphere consisting of 75% hydrogen and 25% nitrogen.
  • the re-magnetization losses as a function of the partial pressure ratio p H2O / p H2 are in FIG. 5 shown.
  • the 2.3 mm thick hot strips produced from each of the melts S1 and S2 were subjected to a two-stage hot strip annealing after hot rolling.
  • the temperature of the hot strip annealing in the first stage was also in this case at an annealing time of 90 s here 1100 ° C, whereas the annealing temperature in the 200 second second stage of the hot strip annealing was 900 ° C.
  • a single-stage hot strip annealing at 1050 ° C over a period of 350 s would have been possible.
  • the hot strips were cold rolled in one stage to form a cold strip.
  • the final thickness of the cold strip was 0.175 mm.
  • Annealing was then carried out at 900 ° C. for 30 seconds in a moist ammonia / hydrogen / nitrogen mixture, whereby the samples were firstly decarburized and, secondly, nitrided.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electromagnetism (AREA)
  • Manufacturing & Machinery (AREA)
  • Dispersion Chemistry (AREA)
  • Power Engineering (AREA)
  • Manufacturing Of Steel Electrode Plates (AREA)
  • Soft Magnetic Materials (AREA)

Claims (4)

  1. Procédé de fabrication d'une bande d'acier magnétique à grains orientés à base d'une coulée continue de lingot mince, comprenant les étapes suivantes :
    a) la fusion d'un acier constitué par, outre du fer et des impuretés inévitables (en % en masse) : Si : 2,5 à 4,0 % C : 0,01 à 0,10 %
    au choix
    - jusqu'à 0,50 % de Mn,
    - de 0,003 - 0,04 % de S,
    - de 0,003 - 0,04 % de Se,
    - jusqu'à 0,07 % d'Al,
    - jusqu'à 0,015 % de N,
    - jusqu'à 0,05 % de Ti,
    - jusqu'à 0,3 % de P,
    - un ou plusieurs éléments du groupe As, Sn, Sb, Te, Bi en teneurs respectives de jusqu'à 0,2 %,
    - un ou plusieurs éléments du groupe Cu, Ni, Cr, Co, Mo en teneurs respectives de jusqu'à 0,5 %,
    - un ou plusieurs éléments du groupe B, V, Nb en teneurs respectives de jusqu'à 0,012 %,
    b) la coulée continue de la masse fondue en un cordon,
    c) l'obtention de lingots minces à partir du cordon coulé,
    d) le recuit des lingots minces dans un four en ligne à une température comprise entre 1 050 °C et 1 300 °C,
    e) le laminage à chaud continu des lingots minces dans un laminoir à chaud en ligne à plusieurs cages en une bande chaude d'une épaisseur de 0,5 à 4,0 mm,
    f) le refroidissement de la bande chaude,
    g) l'enroulement de la bande chaude en une bobine,
    h) au choix : le recuit de la bande chaude après l'enroulement ou avant le laminage à froid,
    i) le laminage à froid de la bande chaude en une bande froide d'une épaisseur finale de 0,15 mm à 0,50 mm,
    j) le recuit de recristallisation et décarbonisation de la bande froide,
    k) la nitruration de la bande froide ayant lieu pendant ou après le recuit de décarbonisation sous une atmosphère ammoniacale à une température de nitruration comprise entre 850 °C et 1 050 °C,
    l) l'application d'un séparateur de recuit sur la surface de la bande,
    m) le recuit final de la bande froide ayant subi un recuit de recristallisation et décarbonisation pour la formation d'une structure de Goss,
    n) au choix : le revêtement de la bande froide ayant subi un recuit final avec un isolement électrique, puis le recuit de détente de la bande froide revêtue,
    o) au choix : l'affinage des domaines de la bande froide revêtue,
    caractérisé en ce que
    la bande froide après nitruration (étape k) et avant l'application d'un séparateur de recuit (étape 1) est soumise à un recuit de post-oxydation pendant une durée de recuit de 15 à 180 s et à une température de recuit de post-oxydation TNO de 750 °C à 900 °C sous une atmosphère de recuit contenant de l'hydrogène dont le rapport de pression partielle pH20/pH2 appliquée au-delà de la température respective TNO se situe à l'intérieur d'une surface qui est définie par les sommets P1 (TNO = 750 °C ; pH20/pH2 = 0,1), P2 (TNO) = 900 °C ; pH20/pH2 = 0,2), P3 (TNO = 750 °C ; pH20/pH2 = 0,42) et P4 (TNO = 900 °C ; pH20/pH2 = 0,52)
  2. Procédé selon la revendication 1, caractérisé en ce que la température de la bande froide lors du bobinage est comprise entre 520 °C et 720 °C.
  3. Procédé selon l'une des revendications précédentes, caractérisé en ce que le recuit de recristallisation et décarbonisation (étape j) est effectué simultanément au traitement de nitruration (étape k).
  4. Procédé selon la revendication 3, caractérisé en ce que le recuit de recristallisation et décarbonisation et la nitruration simultanée de la bande froide sont effectués à une température comprise entre 800 °C et 1 050 °C sous une atmosphère de recuit se composant de 1 - 10 % en volume de NH3, 30 - 75 % en volume de H2 et 30 - 75 % en volume de N2 et dont le point de rosée se situe entre 5 °C et 75 °C pendant une durée comprise entre 60 et 300 s.
EP15159840.6A 2014-03-25 2015-03-19 Procédé de production d'une tôle hautement perméable à grains orientés Not-in-force EP2942417B1 (fr)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE102014104106.2A DE102014104106A1 (de) 2014-03-25 2014-03-25 Verfahren zur Herstellung von hochpermeablem kornorientiertem Elektroband

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Publication Number Publication Date
EP2942417A1 EP2942417A1 (fr) 2015-11-11
EP2942417B1 true EP2942417B1 (fr) 2016-08-24

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Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102017220718A1 (de) * 2017-11-20 2019-05-23 Thyssenkrupp Ag Optimierung des Stickstofflevels während der Haubenglühung II
KR102142511B1 (ko) * 2018-11-30 2020-08-07 주식회사 포스코 방향성 전기강판 및 그의 제조방법

Family Cites Families (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6240315A (ja) * 1985-08-15 1987-02-21 Nippon Steel Corp 磁束密度の高い一方向性珪素鋼板の製造方法
US4897131A (en) * 1985-12-06 1990-01-30 Nippon Steel Corporation Grain-oriented electrical steel sheet having improved glass film properties and low watt loss
JPH083125B2 (ja) 1991-01-08 1996-01-17 新日本製鐵株式会社 磁束密度の高い方向性電磁鋼板の製造方法
IT1290172B1 (it) * 1996-12-24 1998-10-19 Acciai Speciali Terni Spa Procedimento per la produzione di lamierino magnetico a grano orientato, con elevate caratteristiche magnetiche.
IT1290171B1 (it) 1996-12-24 1998-10-19 Acciai Speciali Terni Spa Procedimento per il trattamento di acciaio al silicio, a grano orientato.
PL1752549T3 (pl) 2005-08-03 2017-08-31 Thyssenkrupp Steel Europe Ag Sposób wytwarzania taśmy elektrotechnicznej o zorientowanych ziarnach
SI1752548T1 (sl) 2005-08-03 2016-09-30 Thyssenkrupp Steel Europe Ag Metoda za proizvodnjo magnetnega zrnato usmerjenega jeklenega traku
DE102011119395A1 (de) * 2011-06-06 2012-12-06 Thyssenkrupp Electrical Steel Gmbh Verfahren zum Herstellen eines kornorientierten, für elektrotechnische Anwendungen bestimmten Elektrostahlflachprodukts
DE102011107304A1 (de) * 2011-07-06 2013-01-10 Thyssenkrupp Electrical Steel Gmbh Verfahren zum Herstellen eines kornorientierten, für elektrotechnische Anwendungen bestimmten Elektrostahlflachprodukts

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EP2942417A1 (fr) 2015-11-11

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