EP4621089A1 - Kornorientiertes elektromagnetisches stahlblech und verfahren zur herstellung davon - Google Patents

Kornorientiertes elektromagnetisches stahlblech und verfahren zur herstellung davon

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Publication number
EP4621089A1
EP4621089A1 EP23891609.2A EP23891609A EP4621089A1 EP 4621089 A1 EP4621089 A1 EP 4621089A1 EP 23891609 A EP23891609 A EP 23891609A EP 4621089 A1 EP4621089 A1 EP 4621089A1
Authority
EP
European Patent Office
Prior art keywords
steel sheet
grain
annealing
content
less
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.)
Pending
Application number
EP23891609.2A
Other languages
English (en)
French (fr)
Other versions
EP4621089A4 (de
Inventor
Takashi Kataoka
Ryutaro Yamagata
Mayuko Kikuzuki
Junki Nakamura
Yoshihiro Suwa
Kazutoshi Takeda
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nippon Steel Corp
Original Assignee
Nippon Steel Corp
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 Nippon Steel Corp filed Critical Nippon Steel Corp
Publication of EP4621089A1 publication Critical patent/EP4621089A1/de
Publication of EP4621089A4 publication Critical patent/EP4621089A4/de
Pending legal-status Critical Current

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    • 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
    • C22C38/60—Ferrous alloys, e.g. steel alloys containing lead, selenium, tellurium, or antimony, or more than 0.04% by weight of sulfur
    • 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
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    • 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
    • C21D1/26—Methods of annealing
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    • C21—METALLURGY OF IRON
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    • 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
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    • 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
    • C21D3/00—Diffusion processes for extraction of non-metals; Furnaces therefor
    • C21D3/02—Extraction of non-metals
    • C21D3/04—Decarburising
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    • C21D6/00—Heat treatment of ferrous alloys
    • C21D6/008—Heat treatment of ferrous alloys containing Si
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    • C21D8/00—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1216—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties characterised by the working steps
    • C21D8/1222—Hot rolling
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    • 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 of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1216—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties characterised by the working steps
    • C21D8/1233—Cold rolling
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    • 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 of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1244—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties characterised by the heat treatment
    • C21D8/1255—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties characterised by the heat treatment 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 of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1244—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties characterised by the heat treatment
    • C21D8/1261—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties characterised by the heat treatment 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 of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1244—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties characterised by the heat treatment
    • 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 of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1277—Modifying the physical properties of ferrous metals or ferrous alloys 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
    • C21D9/46—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for sheet metals
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    • C22C—ALLOYS
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    • C22C38/001—Ferrous alloys, e.g. steel alloys containing N
    • C—CHEMISTRY; METALLURGY
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    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
    • C—CHEMISTRY; METALLURGY
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    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/004—Very low carbon steels, i.e. having a carbon content of less than 0,01%
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22C38/008—Ferrous alloys, e.g. steel alloys containing tin
    • C—CHEMISTRY; METALLURGY
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    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
    • C—CHEMISTRY; METALLURGY
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    • C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
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    • C22C38/08—Ferrous alloys, e.g. steel alloys containing nickel
    • C—CHEMISTRY; METALLURGY
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    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
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    • C22C38/34—Ferrous alloys, e.g. steel alloys containing chromium with more than 1.5% by weight of silicon
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    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/42—Ferrous alloys, e.g. steel alloys containing chromium with nickel with copper
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    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/44—Ferrous alloys, e.g. steel alloys containing chromium with nickel with molybdenum or tungsten
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/50—Ferrous alloys, e.g. steel alloys containing chromium with nickel with titanium or zirconium
    • 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
    • H01F1/147—Alloys characterised by their composition
    • H01F1/14766—Fe-Si based alloys
    • H01F1/14775—Fe-Si based alloys in the form of sheets
    • 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
    • H01F1/147—Alloys characterised by their composition
    • H01F1/14766—Fe-Si based alloys
    • H01F1/14775—Fe-Si based alloys in the form of sheets
    • H01F1/14783—Fe-Si based alloys in the form of sheets with insulating coating
    • 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
    • H01F1/147—Alloys characterised by their composition
    • H01F1/14766—Fe-Si based alloys
    • H01F1/14791—Fe-Si-Al based alloys, e.g. Sendust
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    • 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
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    • C21D2201/00—Treatment for obtaining particular effects
    • C21D2201/05—Grain orientation

Definitions

  • the present disclosure relates to a grain-oriented electrical steel sheet and a method for manufacturing the same.
  • a grain-oriented electrical steel sheet has a three-layer structure of a base steel sheet, a primary coating (sometimes referred to as a glass coating) formed on a surface of the base steel sheet, and a tension-applying insulation secondary coating formed on a surface of the primary coating.
  • a grain-oriented electrical steel sheet is a soft magnetism material and is mainly used as an iron core material of a transformer.
  • the grain-oriented electrical steel sheet is required to have magnetic characteristics such as high magnetization characteristics and a low iron loss.
  • the iron loss is a power loss due to consumption as thermal energy that occurs when the iron core is excited by an AC magnetic field, and the iron loss is required to be as low as possible from the viewpoint of energy saving.
  • the level of iron loss is affected by a magnetic susceptibility, a sheet thickness, a coating tension, an impurity amount, an electric resistivity, a crystal grain size, a magnetic domain size, and the like.
  • the iron loss of the grain-oriented electrical steel sheet is the sum of an eddy-current loss depending on the specific resistance, the sheet thickness, the size of the magnetic domain, and the like and a hysteresis loss depending on crystal orientation, the smoothness of the surface, and the like.
  • thinning the base steel sheet for example, less than 0.22 mm
  • the thinning changes the behavior of the secondary recrystallization itself, and there is a concern that the development degree of the Goss orientation is deteriorated.
  • the development of the Goss orientation occurs through a phenomenon (secondary recrystallization) through advanced control of the texture and the precipitate (inhibitor).
  • the texture is preferably in a state in which there are many Goss orientations (nuclei of secondary recrystallization) and there are many orientations (corresponding orientations) on which the Goss orientation encroaches.
  • the inhibitor is preferably in a state in which the pinning force of the inhibitor gradually decreases (the heat resistance of the inhibitor is high) during the secondary recrystallization annealing. In other words, a rapid decrease in the pinning force of the inhibitor during the secondary recrystallization annealing is not preferable from the viewpoint of promoting growth of the Goss orientation.
  • the cause is not clear, but the heat resistance of the inhibitor decreases, and it is not possible to secure a time for preferential growth of the Goss orientation, and secondary recrystallization becomes unstable.
  • Patent Document 1 and Patent Document 2 disclose techniques for avoiding texture deterioration by optimally controlling a cold rolling ratio by preliminary cold rolling.
  • Patent Document 3 discloses an inhibitor control technique via primary coating control.
  • MgO containing 0.15 to 2.0% of Cl and/or SO 3 as an annealing separator, a formation reaction of glass coating is significantly enhanced, and primary coating is controlled to a form preferable for magnetism.
  • inhibitor control is possible, but texture control is not considered. Therefore, for example, when the present technique is applied to a thin electrical steel sheet with a sheet thickness of a base steel sheet of less than 0.22 mm, there is a high possibility that a high quality secondary recrystallization orientation cannot be obtained.
  • a grain-oriented electrical steel sheet is also required to reduce noise generated when the steel sheet is applied to a transformer or the like.
  • an object of the present disclosure is to provide a grain-oriented electrical steel sheet having good magnetic characteristics and noise characteristics without reducing productivity, and a method for manufacturing the same.
  • the present inventors have conducted studies on a thin material from the viewpoint of controlling both the texture and the precipitate (inhibitor) in order to achieve both good magnetic characteristics due to the development of the Goss orientation through secondary recrystallization and good noise characteristics.
  • the magnetic characteristics were very excellent as compared with the magnetic characteristics of the conventional grain-oriented electrical steel sheet without causing destabilization of secondary recrystallization, and it was also confirmed that the magnetic characteristics were compatible with good noise characteristics.
  • the average dispersion angle ⁇ (°) and the average dispersion angle ⁇ (°) have been known as factors affecting magnetic characteristics.
  • the conventional technique there has been a limit to sufficiently reducing the average dispersion angles ⁇ and ⁇ , and further reduction of these average dispersion angles has been desired.
  • the present inventors have found that by appropriately controlling both the texture and the inhibitor, the average dispersion angle ⁇ can be greatly reduced, and the balance among the average dispersion angles ⁇ , ⁇ , and ⁇ can be achieved. More specifically, the present inventors have found that a dense oxide film capable of sufficiently securing the Goss orientation and stably exhibiting the function of the inhibitor during the secondary recrystallization annealing can be formed by increasing the temperature rising rate in a predetermined temperature range in the temperature-raising step during decarburization annealing.
  • the present inventors have investigated the cause of deterioration of the effect of secondary recrystallization stabilization by an inhibitor in a thin material.
  • the decomposition rate of the inhibitor increases due to a relative increase in the surface area percentage of the steel material itself, and thus secondary recrystallization becomes unstable.
  • the present inventors have found that the trigger for the decomposition of the inhibitor is an interaction between Mg 2 SiO 4 as a primary coating (glass coating) and AlN as an inhibitor.
  • the present inventors have found that deterioration of the secondary recrystallization stabilization effect by the inhibitor can be suppressed by decreasing the formation rate of the primary coating (that is, increasing the formation temperature of the primary coating).
  • an increase in the formation temperature of the primary coating can be achieved by thickening and densifying SiO 2 formed on a surface of a cold-rolled steel sheet during the decarburization annealing (in particular, during the temperature-raising step).
  • the mechanism by which the formation temperature of the primary coating at the time of secondary recrystallization can be increased by thickening and densifying SiO 2 is unknown, but it is considered that the thickened and densified SiO 2 reduces the mobility of Mg ions in SiO 2 .
  • the present inventors have found that the Goss orientation is increased by increasing the temperature rising rate in a predetermined temperature range during the decarburization annealing from the viewpoint of texture. Furthermore, it has been found that by inclusion of P (phosphorus) in the steel, a favorable texture for secondary recrystallization during cold rolling can be obtained.
  • the present invention has been made in view of the above findings.
  • the gist of the present invention is as follows.
  • the grain-oriented electrical steel sheet according to an embodiment of the present disclosure includes a base steel sheet having a predetermined chemical composition described later, a glass coating formed on the base steel sheet, and a tension-applying insulation coating formed on the glass coating. Also, the base steel sheet has a texture oriented in the Goss orientation.
  • an average dispersion angle from an ideal Goss orientation with a rolled surface normal direction ND as the rotation axis is defined as ⁇ (°)
  • an average dispersion angle from the ideal Goss orientation with an orthogonal-to-rolling direction TD as the rotation axis is defined as ⁇ (°)
  • an average dispersion angle from the ideal Goss orientation with a rolling direction RD as the rotation axis is defined as ⁇ (°)
  • the ⁇ , the ⁇ , and the ⁇ satisfy the following formula (1).
  • FIGS. 1A and 1B are diagrams schematically illustrating a structure of the grain-oriented electrical steel sheet according to the present embodiment.
  • a grain-oriented electrical steel sheet 10 includes a base steel sheet 11, a primary coating (glass coating) 13 formed on a surface of the base steel sheet 11, and a secondary coating (tension-applying insulation coating) 15 which is an example of an insulating coating formed on a surface of the glass coating 13.
  • the glass coating 13 and the tension-applying insulation coating 15 may be formed on at least one surface of the base steel sheet 11 but are usually formed on both surfaces of the base steel sheet 11 as schematically illustrated in FIG. 1B .
  • the base steel sheet 11 exhibits excellent noise characteristics and magnetic characteristics by being manufactured from a steel piece containing a chemical composition as described in detail below.
  • the chemical composition of the base steel sheet 11 will be described in detail below.
  • the glass coating 13 is an inorganic coating which is disposed on the surface of the base steel sheet 11 and contains magnesium silicate as a main component.
  • the glass coating 13 is formed by a reaction between an annealing separator containing magnesia (MgO) applied to the surface of the base steel sheet and the component of the surface of the base steel sheet 11 in final annealing. That is, the glass coating 13 has a composition derived from the components of the annealing separator and the base steel sheet (more specifically, a composition containing Mg 2 SiO 4 as a main component).
  • MgO magnesia
  • the tension-applying insulation coating 15 is disposed on the surface of the glass coating 13. By imparting electrical insulation properties to the grain-oriented electrical steel sheet 10 by the tension-applying insulation coating 15, it is possible to reduce eddy-current loss and improve iron loss of the grain-oriented electrical steel sheet 10. Also, the tension-applying insulation coating 15 realizes various properties such as corrosion resistance, heat resistance, and slippage in addition to the electrical insulation properties as described above.
  • the tension-applying insulation coating 15 has a function of applying tension to the grain-oriented electrical steel sheet 10.
  • the tension-applying insulation coating 15 By applying tension to the grain-oriented electrical steel sheet 10 by the tension-applying insulation coating 15 to facilitate the movement of domain walls in the grain-oriented electrical steel sheet 10, the iron loss of the grain-oriented electrical steel sheet 10 can be improved.
  • the surface of the tension-applying insulation coating 15 may be subjected to magnetic domain refining treatment using a continuous-wave laser beam or an electron beam.
  • linear thermal strain forming a predetermined angle ⁇ with the sheet width direction, which is a direction orthogonal to the rolling direction, is periodically formed at predetermined intervals along the rolling direction. Accordingly, in the grain-oriented electrical steel sheet according to the present embodiment, the magnetic characteristics can be further improved.
  • the tension-applying insulation coating 15 is formed, for example, by applying a coating liquid containing a metal phosphate and silica as main components onto the surface of the glass coating 13 and baking the coating liquid.
  • the sheet thickness of the base steel sheet of the grain-oriented electrical steel sheet 10 according to the present embodiment is not particularly limited, and may be, for example, 0.16 mm or more and 0.30 mm or less. Also, in the present embodiment, the smaller the sheet thickness of the cold-rolled sheet (the base steel sheet 11) after the cold rolling, the more sufficiently the effect of reducing iron loss can be obtained. Therefore, the sheet thickness t of the base steel sheet of the grain-oriented electrical steel sheet 10 is preferably 0.24 mm or less, and more preferably 0.23 mm or less.
  • the sheet thickness t of the base steel sheet of the grain-oriented electrical steel sheet 10 is more preferably, for example, less than 0.20 mm from the viewpoint of magnetic characteristics.
  • the lower limit of the sheet thickness t may be 0.16 mm or more, or may be 0.17 mm or more.
  • a steel piece for example, a slab
  • a steel piece having the following chemical composition becomes a grain-oriented electrical steel sheet through the manufacturing steps as described in detail below, the same contents as those of the steel piece are maintained for components other than carbon (C), acid-soluble aluminum (sol.Al), nitrogen (N), sulfur (S), and bismuth (Bi) of the base steel sheet 11. That is, the contents of components other than carbon (C), acid-soluble aluminum (sol.Al), nitrogen (N), and sulfur (S) of the base steel sheet 11 are substantially the same as those of the steel piece and the product sheet.
  • the contents of carbon (C), acid-soluble aluminum (sol.Al), nitrogen (N), sulfur (S), and bismuth (Bi) of the base steel sheet 11 change as compared with the composition of the steel piece through the manufacturing steps as described in detail below.
  • silicon (Si), manganese (Mn), chromium (Cr), boron (B), and titanium (Ti) of the base steel sheet 11 are absorbed into the glass coating in the middle of manufacturing, the contents thereof may be slightly reduced as compared with the composition of the steel piece.
  • C Carbon is an element having an effect of increasing the magnetic flux density.
  • the C content of the steel piece is less than 0.020%, the effect of improving the magnetic flux density cannot be obtained.
  • the C content of the steel piece is 0.020% or more.
  • the C content is preferably 0.040% or more, and more preferably 0.050% or more.
  • the C content of the steel piece exceeds 0.150%, the steel undergoes phase transformation in the secondary recrystallization annealing (that is, final annealing), secondary recrystallization does not sufficiently proceed, and a favorable magnetic flux density and iron loss characteristics cannot be obtained.
  • the C content of the steel piece is 0.150% or less.
  • the lower the C content the better for iron loss reduction.
  • the C content is preferably 0.120% or less, and more preferably 0.100% or less.
  • the C content in the steel piece as described above becomes 0.010% (100 ppm) or less in the base steel sheet 11 by forming the grain-oriented electrical steel sheet 10 according to the present embodiment through the steps as described in detail below.
  • the C content in the base steel sheet 11 may be 0%.
  • Si silicon is an extremely effective element for increasing electric resistance (specific resistance) of steel to reduce eddy-current loss constituting a part of iron loss.
  • the Si content of the steel piece is 3.00% or more.
  • the Si content of the steel piece is preferably 3.10% or more, and more preferably 3.20% or more.
  • the Si content of the steel piece exceeds 4.00%, the steel sheet is embrittled, and passability of the sheet in the manufacturing steps is remarkably deteriorated.
  • the Si content of the steel piece is 4.00% or less.
  • the Si content of the steel piece is preferably 3.80% or less, and more preferably 3.50% or less.
  • the Si content in the steel piece as described above may be reduced by forming the grain-oriented electrical steel sheet 10 according to the present embodiment through the steps as described in detail below.
  • the Si content in the base steel sheet 11 may be slightly reduced.
  • the reduced amount is within a range that does not impair the operation and effects of the present embodiment, and the effects of the present embodiment can be obtained by setting the Si content of the steel piece within the above range.
  • the Si content of the base steel sheet 11 may be 2.80 to 3.80%.
  • Sol.Al (acid-soluble aluminum) is a constituent element of a main inhibitor among compounds called inhibitors that influence secondary recrystallization in the grain-oriented electrical steel sheet, and is an essential element from the viewpoint of development of secondary recrystallization in the base steel sheet according to the present embodiment.
  • the sol.Al content of the steel piece is less than 0.010%, AlN functioning as an inhibitor is not sufficiently generated, and secondary recrystallization becomes insufficient, and iron loss characteristics are not improved.
  • the content of sol.Al in the steel piece is 0.010% or more.
  • the content of sol.Al is preferably 0.020% or more.
  • the content of sol.Al of the steel piece is 0.050% or less.
  • the content of sol.Al is preferably 0.040% or less, and more preferably 0.030% or less.
  • the sol.Al content in the steel piece as described above becomes 0.010% (100 ppm) or less in the base steel sheet 11 by forming the grain-oriented electrical steel sheet 10 according to the present embodiment through the steps as described in detail below.
  • the lower limit of the sol.Al content in the base steel sheet 11 is not particularly limited, and may be 0%.
  • Mn manganese
  • MnS manganese
  • the Mn content is preferably 0.03% or more, and more preferably 0.06% or more.
  • the Mn content of the steel piece exceeds 0.50%, the steel undergoes phase transformation in the secondary recrystallization annealing, secondary recrystallization does not sufficiently proceed, and a favorable magnetic flux density and iron loss characteristics cannot be obtained.
  • the Mn content of the steel piece is 0.50% or less.
  • the Mn content is preferably 0.20% or less, and more preferably 0.10% or less.
  • the Mn content in the steel piece as described above may be reduced by forming the grain-oriented electrical steel sheet 10 according to the present embodiment through the steps as described in detail below.
  • the Mn content in the base steel sheet 11 may be slightly reduced.
  • the reduced amount is within a range that does not impair the operation and effects of the present embodiment, and the effects of the present embodiment can be obtained by setting the Mn content of the steel piece within the above range.
  • the Mn content of the base steel sheet 11 may be 0 to 0.40%.
  • N nitrogen
  • the N content of the steel piece is 0.001% or more.
  • the N content is preferably 0.004% or more, and more preferably 0.006% or more.
  • the N content of the steel piece exceeds 0.020%, blisters (pores) are generated in the steel sheet during cold rolling, the strength increases, and passability of the sheet during manufacturing deteriorates.
  • the N content of the steel piece is 0.020% or less.
  • the N content is preferably 0.015% or less, and more preferably 0.010% or less.
  • the N content in the steel piece as described above becomes 0.010% (100 ppm) or less in the base steel sheet 11 by forming the grain-oriented electrical steel sheet 10 according to the present embodiment through the steps as described in detail below.
  • the lower limit of the N content in the base steel sheet 11 is not particularly limited, and may be 0%.
  • Sulfur (S) and Selenium (Se) are important elements that react with the Mn to form an inhibitor MnS or MnSe.
  • S sulfur
  • Se Selenium
  • the total of the S content and the Se content of the steel piece is less than 0.0010%, a sufficient inhibitor effect cannot be obtained.
  • the total of the S content and the Se content in the steel piece is 0.0010% or more.
  • the total of the S content and the Se content is preferably 0.0100% or more, and more preferably 0.0150% or more.
  • the total of the S content and the Se content of the steel piece exceeds 0.0400%, hot embrittlement is caused, and hot rolling is significantly difficult.
  • the total of the S content and the Se content of the steel piece is 0.0400% or less.
  • the total of the S content and the Se content is preferably 0.0300% or less.
  • the S content in the steel piece as described above may be reduced by forming the grain-oriented electrical steel sheet 10 according to the present embodiment through the steps as described in detail below, and in this case, the S content in the base steel sheet 11 may be 0.0100% (100ppm) or less.
  • the lower limit of the total of the S content and the Se content in the base steel sheet 11 is not particularly limited and may be 0.0005%.
  • the lower limit of the total of the S content and the Se content in the base steel sheet 11 may include 0%. It should be noted that identification of S or Se of less than 0.0005% requires careful attention.
  • the total of the S content and the Se content may be regarded as 0%. In a practical steel sheet, the lower limit of the total of the substantial S content and Se content is 0.0005%.
  • P phosphorus
  • the P content of the steel piece is 0.005% or more.
  • the P content is preferably 0.010% or more.
  • P is an element that lowers the workability in rolling.
  • the P content exceeds 0.100%, rolling workability may be deteriorated, leading to fracture of the steel sheet during manufacturing.
  • the P content is 0.100% or less.
  • the P content is preferably 0.070% or less, and more preferably 0.030% or less.
  • the chemical composition of the steel piece and the base steel sheet 11 according to the present embodiment basically contains the above-described elements (basic elements) with the remainder being Fe and impurities.
  • one or more (optional elements) selected from the group consisting of Sn, Cu, Cr, Sb, Mo, Ni, Nb, B, Ti, and Bi may be further contained in the following ranges.
  • Sn, Cu, Cr, Sb, Mo, Ni, Nb, B, Ti, and Bi are optional elements in the steel piece and the base steel sheet 11 according to the present embodiment, and thus the lower limit of the content thereof is 0%.
  • Sn (tin) is an element having an effect of improving magnetic characteristics.
  • Sn may be contained.
  • the content of Sn is preferably 0.01% or more in order to favorably exhibit the effect of improving magnetic characteristics.
  • the Sn content is more preferably 0.03% or more in consideration of both magnetic characteristics and coating adhesion.
  • the Sn content exceeds 0.50%, adhesion of the glass coating is significantly deteriorated. Therefore, when contained, the Sn content is 0.50% or less.
  • the Sn content is preferably 0.40% or less, and more preferably 0.30% or less.
  • Cu is an element that contributes to an increase in the occupancy rate of the Goss orientation in the secondary recrystallization structure and contributes to an improvement in the glass coating adhesion.
  • the Cu content is preferably 0.01% or more.
  • the Cu content is more preferably 0.05% or more.
  • the Cu content of the steel piece is 0.50% or less.
  • the Cu content is preferably 0.40% or less and more preferably 0.30% or less.
  • Cr Cr
  • Cr chromium
  • the Cr content is preferably set to 0.01% or more.
  • the Cr content is more preferably 0.03% or more.
  • the Cr content exceeds 0.50%, Cr oxide is formed, and the magnetic characteristics are deteriorated.
  • the Cr content is 0.50% or less.
  • the Cr content is preferably 0.40% or less, and more preferably 0.30% or less.
  • Sb antimony is an element having an effect of improving magnetic characteristics.
  • Sb may be contained.
  • the content thereof is preferably 0.01% or more such that Sb favorably exhibits the effect of improving magnetic characteristics.
  • the upper limit of the Sb content is to 0.20%.
  • the Sb content is preferably 0.15% or less and more preferably 0.10% or less.
  • Mo is an element having an effect of improving magnetic characteristics.
  • Mo may be contained.
  • the Mo content is preferably 0.01% or more in order to favorably exhibit the effect of improving magnetic characteristics.
  • the Mo content when the Mo content is more than 0.10%, the cold rolling characteristics may be deteriorated, leading to fracture. Therefore, when contained, the Mo content is 0.10% or less.
  • the Mo content is preferably 0.05% or less, and more preferably 0.03% or less.
  • Ni (nickel) is an effective element that affects crystal orientation rotation occurring during cold rolling and obtains a favorable texture for secondary recrystallization. Ni (nickel) is also an element effective for increasing the specific resistance of the steel sheet and reducing the iron loss. Thus, Ni may be contained. When Ni is contained, the Ni content is preferably 0.01% or more in order to obtain these effects.
  • the Ni content exceeds 0.20%, secondary recrystallization may become unstable.
  • the Ni content is 0.20% or less.
  • the Ni content is preferably 0.15% or less, and more preferably 0.10% or less.
  • Nb (niobium) is an element effective for enhancing the function of the inhibitor to stably obtain secondary recrystallization.
  • Nb may be contained.
  • the Nb content is preferably 0.0005% or more in order to stably obtain secondary recrystallization.
  • the Nb content is more preferably 0.0010% or more.
  • the Nb content exceeds 0.0200%, secondary recrystallization may become unstable.
  • the Nb content is 0.0200% or less.
  • the Nb content is preferably 0.0100% or less, and more preferably 0.0050% or less.
  • B is an element effective for enhancing the function of the inhibitor to stably obtain secondary recrystallization.
  • B may be contained.
  • the B content is preferably 0.0005% or more in order to stably obtain secondary recrystallization.
  • the B content is more preferably 0.0010% or more.
  • the B content exceeds 0.0200%, secondary recrystallization may become unstable.
  • the B content is 0.0200% or less.
  • the B content is preferably 0.0100% or less, and more preferably 0.0050% or less.
  • Ti titanium is an element that increases the development degree of the Goss orientation and improves magnetism. Although the cause is not clear, T may bond to N to form TiN, and function as an inhibitor. When Ti is contained, the Ti content is 0.0005% or more, and preferably 0.0010% or more.
  • Bi bismuth is an element that increases the development degree of the Goss orientation and improves magnetism.
  • the Bi content is 0.0010% or more, and preferably 0.0020% or more.
  • the Bi content is 0.0200% or less.
  • the Bi content is preferably 0.0100% or less.
  • the Bi content in the steel piece as described above becomes 0.0100% (100 ppm) or less in the base steel sheet 11 by forming the grain-oriented electrical steel sheet 10 according to the present embodiment through the steps as described in detail below.
  • the lower limit of the Bi content in the base steel sheet 11 is not particularly limited and may be 0%.
  • the lower limit of the Bi content may exceed 0%.
  • the respective contents of Cr, B, and Ti in the steel piece as described above may be reduced by forming the grain-oriented electrical steel sheet 10 according to the present embodiment through the steps as described in detail below.
  • the content of each of these elements in the base steel sheet 11 may be slightly reduced.
  • any of the reduced amounts is within a range that does not affect the operation and effects of the present embodiment.
  • measurement may be performed using inductively coupled plasma-atomic emission spectrometry (ICP-AES).
  • ICP-AES inductively coupled plasma-atomic emission spectrometry
  • the grain-oriented electrical steel sheet 10 is subjected to a cleaning treatment with an alkaline solution to remove the tension-applying insulation coating 15, and further, the glass coating 13 is removed by pickling, and then measurement is performed using ICP-AES.
  • C and S may be measured by a combustion-infrared absorption method
  • N may be measured by an inert gas fusion-thermal conductivity method
  • O may be measured by an inert gas fusion-non-dispersive infrared absorption method.
  • a method of immersing the grain-oriented electrical steel sheet including the coating in a high-temperature alkaline solution may be applied.
  • the grain-oriented electrical steel sheet including the coating is immersed in a sodium hydroxide aqueous solution (NaOH: 30 to 50 mass% + H 2 O: 50 to 70 mass%) at 80 to 90°C for 5 minutes to 10 minutes, then washed with water, and dried.
  • a sodium hydroxide aqueous solution NaOH: 30 to 50 mass% + H 2 O: 50 to 70 mass%
  • the time of immersion in the sodium hydroxide aqueous solution may be appropriately changed according to the thickness of the tension-applying insulation coating.
  • the grain-oriented electrical steel sheet from which the tension-applying insulation coating has been removed is immersed in hydrochloric acid (concentration: 30 to 40%) at 80 to 90°C for 1 minute to 5 minutes, then washed with water, and dried. Thereby, the glass coating can be removed from the grain-oriented electrical steel sheet.
  • the base steel sheet can be exposed, and the chemical composition of the base steel sheet can be measured.
  • the steel component of the slab may be subjected to composition analysis by collecting a sample from molten steel before casting or subjected to composition analysis by removing a surface oxide film or the like from the slab after casting.
  • the remainder of the chemical composition of the steel piece and the base steel sheet 11 according to the present embodiment other than the above-described elements is basically Fe and impurities.
  • the "impurity" is present in the steel piece and the base steel sheet 11 regardless of the intention of addition. That is, the impurity is an element that is a contaminant derived from ore or scrap as a raw material, a manufacturing environment, or the like when the base steel sheet is industrially manufactured and means an element that is allowed to be contained in a content that does not adversely affect the effect of the grain-oriented electrical steel sheet according to the present embodiment.
  • the base steel sheet 11 of the present embodiment has a secondary recrystallization texture developed in a ⁇ 110 ⁇ 001> orientation (Goss orientation). Moreover, in the base steel sheet 11, when an average dispersion angle from an ideal Goss orientation with a rolled surface normal direction ND as the rotation axis is defined as ⁇ (°), an average dispersion angle from the ideal Goss orientation with an orthogonal-to-rolling direction TD as the rotation axis is defined as ⁇ (°), and an average dispersion angle from the ideal Goss orientation with a rolling direction RD as the rotation axis is defined as ⁇ (°), the ⁇ , the ⁇ , and the ⁇ satisfy the following formula (1).
  • the ⁇ preferably satisfies the following formula (2). 0.0 ⁇ ⁇ ⁇ 2.5 ⁇ ⁇ ⁇ 4.0 ⁇ ⁇ ⁇ 10.0 0.0 ⁇ ⁇ ⁇ 2.0
  • two ⁇ 110 ⁇ 001> orientations of the "actual crystal ⁇ 110 ⁇ 001> orientation” and the "ideal ⁇ 110 ⁇ 001> orientation” are distinguished. This is because, in the present embodiment, it is necessary to distinguishably handle the ⁇ 110 ⁇ 001> orientation when displaying the crystal orientation of the practical steel sheet and the ⁇ 110 ⁇ 001> orientation as an academic crystal orientation.
  • the crystal orientation is defined without strictly distinguishing an angle difference of about ⁇ 2.5°.
  • an angular range of about ⁇ 3.0° centered on a geometrically strict ⁇ 110 ⁇ 001> orientation is defined as a " ⁇ 110 ⁇ 001> orientation”.
  • the deviation between the actual crystal orientation of the grain-oriented electrical steel sheet and the ideal Goss orientation is defined using the following three angles ⁇ , ⁇ , and ⁇ (unit: °).
  • Average dispersion angle (deviation angle) ⁇ a deviation angle around the rolled surface normal direction (ND)
  • the deviation angle ⁇ is an angle formed by the ⁇ 001> direction of crystal projected on the rolled surface and the rolling direction RD when viewed from the rolled surface normal direction ND.
  • the deviation angle ⁇ is an angle formed by the ⁇ 001> direction of crystal projected on L cross section (cross section whose normal direction is the orthogonal-to-rolling direction TD) and the rolling direction RD when viewed from the orthogonal-to-rolling direction TD (sheet width direction).
  • the deviation angle ⁇ is an angle formed by the ⁇ 110> direction of crystal projected on C-section (cross section whose normal direction is the rolling direction RD) and the rolled surface normal direction ND when viewed from the rolling direction RD.
  • the deviation angles ⁇ and ⁇ among the deviation angles ⁇ , ⁇ , and ⁇ affect magnetic characteristics.
  • the deviation angle ⁇ affects magnetostriction.
  • the magnetostriction is a phenomenon in which a shape of magnetic body changes by application of magnetic field.
  • the magnetostriction causes noise, the magnetostriction is required to be small.
  • the crystal orientation is controlled so that the deviation angle ⁇ becomes small (specifically, so that the maximum value and the average value of the absolute value
  • the conventional grain-oriented electrical steel sheet there has been a limit to reduction of the deviation angle ⁇ , and further reduction has been desired.
  • the secondary recrystallization texture of the base steel sheet satisfies the above formula (1), and preferably satisfies the above formula (2).
  • the deviation angle ⁇ exceeds 10.0° in the formula (1), the magnetic characteristics may be deteriorated.
  • the deviation angles ⁇ and ⁇ have a greater influence on the magnetic characteristics than the deviation angle ⁇ . Therefore, the deviation angles ⁇ and ⁇ are made smaller than the deviation angle ⁇ .
  • the deviation angle ⁇ affects noise characteristics, it is not preferable to make the deviation angle ⁇ excessively large. Therefore, in the formula (1), the deviation angle ⁇ is 10.0° or less.
  • the deviation angle ⁇ when the deviation angle ⁇ is controlled to be less than 4.0°, the deviation angle ⁇ may exceed 2.5°. When the deviation angle ⁇ exceeds 2.5°, the noise characteristics may be deteriorated. Therefore, the lower limit of the deviation angle ⁇ is 4.0° or more.
  • the deviation angles ⁇ and ⁇ are preferably less than 3.5°, and more preferably less than 3.0°.
  • the deviation angle ⁇ becomes 2.5° or more.
  • the cause of this is unknown, it is presumed that there is a trade-off relationship between the primary recrystallization texture capable of reducing the deviation angle ⁇ and the primary recrystallization texture capable of reducing the deviation angle ⁇ .
  • the deviation angle ⁇ is 2.5° or more, the noise characteristics may be deteriorated.
  • the lower limit of the deviation angle ⁇ exceeds 2.5°, and the upper limit of the deviation angle ⁇ is less than 2.5°. From the above, from the viewpoint of achieving both the magnetic characteristics and the noise characteristics, it is effective that the deviation angles ⁇ , ⁇ , and ⁇ satisfy the following relationship in the present embodiment. 0.0 ⁇ ⁇ ⁇ 2.5 ⁇ ⁇ ⁇ 4.0 ⁇ ⁇ ⁇ 10.0
  • the deviation angle ⁇ is preferably 2.0° or less, and more preferably 1.8° or less. Since it is more preferable as the deviation angle ⁇ is smaller, the lower limit thereof is not limited.
  • the deviation angle ⁇ may be 0°.
  • the crystal orientation of the grain-oriented electrical steel sheet can be obtained experimentally using, for example, a Laue diffractometer (RIGAKU RASCO-L II V).
  • a grain-oriented electrical steel sheet of 60 mm in the width direction ⁇ 300 mm in the length direction is irradiated with X-rays at intervals of 5 mm in the length direction and 5 mm in the width direction to obtain Laue diffraction spots.
  • analysis software on a PC, Euler angles ⁇ 1, ⁇ , and ⁇ 2 are obtained.
  • the deviation angles ⁇ , ⁇ , and ⁇ are obtained by comparing the orientation angles obtained in the experiment with the angles of the Goss orientation.
  • FIG. 3 is a flowchart illustrating an example of a flow of a method for manufacturing a grain-oriented electrical steel sheet according to the present embodiment.
  • a steel piece such as a slab having the above chemical composition is heated prior to hot rolling.
  • the heating temperature of the steel piece is not particularly limited, but is preferably in the range of 1100 to 1450°C.
  • the heating temperature is more preferably 1300 to 1400°C.
  • the steel piece after the heating step is hot rolled to obtain a hot-rolled steel sheet.
  • the hot rolling conditions are not particularly limited, and is appropriately set on the basis of required characteristics.
  • the thickness of the hot-rolled steel sheet processed by hot rolling is preferably, for example, in a range of 2.0 mm or more and 3.0 mm or less.
  • the hot-band annealing step is a step of annealing the hot-rolled steel sheet manufactured through the hot rolling step to obtain a hot-rolled annealed steel sheet.
  • the hot-rolled steel sheet manufactured through the hot rolling step may be annealed according to a known method.
  • Methods for heating the hot-rolled steel sheet at the time of annealing is not particularly limited, and a known heating method can be adopted.
  • the annealing conditions are also not particularly limited, but for example, the hot-rolled steel sheet can be annealed in a temperature range of 900 to 1200°C for 10 seconds to 5 minutes.
  • the hot-rolled annealed steel sheet is subjected to cold rolling including at least one or more passes to obtain a cold-rolled steel sheet.
  • the cold rolling may not include one or more intermediate annealing between each rolling pass.
  • a plurality of times of cold rolling including an intermediate annealing therebetween may be performed by interrupting the cold rolling and performing at least one or more intermediate annealing before the final pass of the cold rolling step.
  • the intermediate annealing When the intermediate annealing is performed, it is preferable to hold the intermediate annealing at a temperature of 1000 to 1200°C for 5 to 180 seconds.
  • the annealing atmosphere is not particularly limited.
  • the number of times of intermediate annealing is preferably three or less in consideration of manufacturing cost.
  • the surface of the hot-rolled steel sheet may be subjected to pickling under known conditions before rolling.
  • the cold rolling conditions are not limited, but for example, the final rolling reduction can be within a range of 80% or more and 95% or less.
  • the final rolling reduction is less than 80%, there is a high possibility that a Goss nucleus in which the ⁇ 110 ⁇ 001> orientation has a high development degree in a rolling direction cannot be obtained, which is not preferable.
  • the final rolling reduction is a cumulative rolling reduction of cold rolling, and when intermediate annealing is performed, the final rolling reduction is a cumulative rolling reduction of cold rolling after the final intermediate annealing.
  • the sheet thickness of the cold-rolled steel sheet subjected to cold rolling is usually different from the sheet thickness of the grain-oriented electrical steel sheet to be finally manufactured (the product sheet thickness including the thickness of the tension-applying insulation coating).
  • the product sheet thickness of the grain-oriented electrical steel sheet is as described above.
  • the decarburization annealing step (step S107) is a step of subjecting a cold-rolled steel sheet to decarburization annealing to obtain a decarburization-annealed steel sheet, and in the present embodiment, it is an important step for appropriately controlling both the texture and the inhibitor and reducing the average dispersion angle ⁇ .
  • the cold-rolled steel sheet is primarily recrystallized, and C (carbon) that adversely affects magnetic characteristics is removed from the steel sheet.
  • the Goss nuclei are increased, and SiO 2 formed by annealing is thickened and densified.
  • the secondary recrystallization structure can be precisely controlled in the subsequent final annealing step by performing the annealing treatment according to a predetermined heat treatment condition in the decarburization annealing step.
  • the decarburization annealing step according to the present embodiment includes two steps of a temperature-raising step (step S131) and a soaking step (step S133) in order to obtain a desired secondary recrystallization structure.
  • the temperature-raising step (step S131) is a step of raising the temperature of the cold-rolled steel sheet obtained in the cold rolling step from room temperature to a temperature T1 (°C) in a range of 850°C or higher and 950°C or lower (maximum heating temperature) at a predetermined temperature rising rate.
  • the soaking step (step S131) is a step of annealing the cold-rolled steel sheet heated at a predetermined temperature rising rate by cooling the cold-rolled steel sheet to a predetermined temperature and holding the cold-rolled steel sheet in a predetermined temperature range for a predetermined time.
  • the temperature-raising step according to the present embodiment is an important step for precisely controlling the texture of the secondary recrystallized grains.
  • the rolling reduction in cold rolling is increased in order to reduce the sheet thickness, but as the cold rolling ratio increases, the Goss orientation decreases and secondary recrystallization becomes unstable.
  • the average temperature rising rate in the temperature range of 550 to 800°C is set to 400 °C/sec or more to increase the Goss orientation.
  • the temperature range of 550 to 800°C affects the behavior of recrystallization, that is, transition.
  • recrystallization is completed at the maximum attainment temperature through recovery of the structure.
  • This recovery and recrystallization most affect the final annealing step (secondary recrystallization annealing step) which is a subsequent step.
  • secondary recrystallization annealing step which is a subsequent step.
  • the average temperature rising rate in this temperature range is less than 400 °C/sec, the nucleus of the Goss orientation having geometrically strict ⁇ 110 ⁇ 001> cannot be sufficiently increased.
  • the upper limit of the average temperature rising rate in the temperature range of 550 to 800°C is not necessarily limited from the viewpoint of characteristics, but it is not desirable to excessively increase the average temperature rising rate from the viewpoint of a load on equipment and devices to be used. Therefore, the average temperature rising rate in the temperature range of 550 to 800°C is set to 3000 °C/sec or less.
  • the temperature range for controlling the average temperature rising rate is set to 550 to 800°C because this temperature range is an important temperature range for enrichment and recovery of the Goss orientation.
  • This temperature range is a range found by the present inventors by investigating the influence of the staying time at each temperature on the existence frequency and recovery of the Goss orientation.
  • the present inventors have found that the Goss orientation frequency in the primary recrystallization texture decreases due to staying in the temperature range of 550 to 800°C.
  • the existence frequency of the Goss orientation can be increased. If the existence frequency of the Goss orientation can be increased, the coarsening probability of the Goss orientation can be increased in the final annealing step, which leads to an increase in magnetic characteristics.
  • SiO 2 formed on the surface layer of the steel sheet can be thickened and densified by setting the average temperature rising rate in the temperature range of 800 to 850°C to 100 °C/sec or more.
  • the trigger for the decomposition of the inhibitor is an interaction between Mg 2 SiO 4 as a primary coating and AlN.
  • Mg 2 SiO 4 as a primary coating
  • AlN AlN
  • the increase in the formation temperature of the primary coating can be achieved by thickening and densifying SiO 2 formed in the temperature-raising step during the decarburization annealing step.
  • the mechanism by which the formation temperature of the primary coating can be increased by thickening and densifying SiO 2 is unknown, but it is considered that the thickened and densified SiO 2 reduces the mobility of Mg ions in SiO 2 .
  • the form of SiO 2 formed in the temperature-raising step is roughly divided into an "externally oxidized film” formed on the sheet surface and an “internally oxidized film” formed on the surface layer of the steel sheet, and the “internally oxidized film” is further divided into a "spherical oxide” and a “lamellar oxide film”.
  • the present inventors have particularly focused on the "externally oxidized film” among them, and have found that by forming the externally oxidized film thick and dense in the temperature-raising step, the formation rate of the primary coating can be reduced (that is, the formation temperature of the primary coating can be increased) in the subsequent final annealing step, and the stabilization (reduction in the decomposition rate) of the inhibitor can be realized.
  • the thick and densely formed externally oxidized film of SiO 2 suppresses the entry of Mg into the steel sheet, and the formation of the primary coating (glass coating) is delayed. It is considered that this is because the reaction between Mg 2 SiO 4 and AlN (that is, the decomposition reaction of AlN) is also delayed as the formation of Mg 2 SiO 4 itself is delayed.
  • the increase in the temperature of the decomposition reaction of AlN leads to the securing of the grain growth rate of the Goss orientation, and thus is a preferable direction as the magnetic characteristics.
  • the temperature of the cold-rolled steel sheet is raised to the temperature T1 (°C) in the range of 850°C or higher and 950°C or lower (maximum heating temperature).
  • the maximum heating temperature T1 is an effective element for suppressing internal oxidation in the subsequent soaking step.
  • the maximum heating temperature T1 is set to 850°C or higher. This makes it possible to suppress the internal oxidation (to suppress the formation of the spherical oxide and the lamellar oxide film) in the soaking step.
  • the maximum heating temperature T1 is preferably 870°C or higher, and more preferably 900°C or higher. On the other hand, since excessively increasing the maximum heating temperature T1 causes an excessive burden on equipment, the maximum heating temperature T1 is set to 950°C or lower.
  • the externally oxidized film of SiO 2 formed on the sheet surface can be formed thick and dense as described above.
  • the average temperature rising rate in the temperature range of 800 to the maximum heating temperature T1 (°C) is less than 100 °C/sec, the thickness of the externally oxidized film of SiO 2 becomes insufficient, and an oxide film other than SiO 2 (for example, Fe 2 SiO 4 or the like) is allowed.
  • the oxide film other than SiO 2 may promote decomposition of the inhibitor during the final annealing step.
  • the average temperature rising rate in the temperature range of 800 to the maximum heating temperature T1 (°C) is set to 100 °C/sec or more, preferably 200 °C/sec or more, and more preferably 400 °C/sec or more.
  • the control range of the average temperature rising rate in the temperature-raising step is preferably set to 550 to the maximum heating temperature T1 (°C).
  • the average temperature rising rate in the temperature range of 550 to the maximum heating temperature T1 (°C) is preferably set to 100 °C/sec or more.
  • a preferable temperature range to be controlled is 600 to the maximum heating temperature T1 (°C), and more preferably 650 to the maximum heating temperature T1 (°C).
  • the upper limit of the average temperature rising rate in the temperature range of 800 to the maximum heating temperature T1 (°C) is not necessarily limited from the viewpoint of characteristics, but since a special device is required to obtain an average temperature rising rate exceeding 1500 °C/sec, the average temperature rising rate is set to 1500 °C/sec or less.
  • the dew point of the atmosphere during the temperature rising in the temperature range from 800°C to the maximum heating temperature T1 (°C) is set to 0°C or less.
  • the dew point in the temperature-raising step also affects the formation of the oxide film other than SiO 2 .
  • the dew point of the atmosphere in the temperature range of 800 to the maximum heating temperature T1 (°C) is set to 0°C or less, preferably -5°C or less, and more preferably -10°C or less.
  • setting the dew point of the atmosphere in the temperature range of room temperature or higher and lower than 800°C to 0°C or lower does not impair the effect of the present invention.
  • a soaking step is performed.
  • the atmosphere at the time of decarburization annealing is usually set to a relatively high oxygen potential in order to reduce the amount of carbon.
  • the oxygen potential of the atmosphere is high, the amount of SiO 2 formation increases, and the primary coating formation rate increases.
  • the annealing atmosphere is performed at a low oxygen potential. Thereby, the formation rate of the primary coating is reduced.
  • the cold-rolled steel sheet is preferably held in an atmosphere having a temperature of 780 to 860°C and an oxygen potential (PH 2 O/PH 2 ) of 0.20 or more and 0.60 or less for 100 seconds to 300 seconds.
  • PH 2 O/PH 2 oxygen potential
  • decarburization is a chemical reaction between carbon in a steel sheet and oxygen in an annealing atmosphere.
  • the low oxygen potential is synonymous with the low oxygen partial pressure and means a situation in which a decarburization reaction is unlikely to occur.
  • the atmospheric dew point temperature may be set to 30 to 80°C as a mixed gas of nitrogen and hydrogen or a nitrogen gas.
  • a nitriding treatment may be performed between the decarburization annealing step and a final annealing step described later.
  • the cold-rolled steel sheet after the decarburization annealing step is maintained at about 700 to 850°C in a nitriding treatment atmosphere (an atmosphere containing a gas having nitriding ability, such as hydrogen, nitrogen, or ammonia).
  • a nitriding treatment atmosphere an atmosphere containing a gas having nitriding ability, such as hydrogen, nitrogen, or ammonia.
  • the steel sheet it is preferable to subject the steel sheet to a nitriding treatment such that the N content of the cold-rolled steel sheet is 40 to 1000 ppm on a mass basis.
  • the N content of the cold-rolled steel sheet after the nitriding treatment is less than 40 ppm, AlN may not be sufficiently precipitated in the cold-rolled steel sheet, and AlN may not function as an inhibitor. Therefore, when AlN is utilized as an inhibitor, the N content of the cold-rolled steel sheet is preferably set to 40 ppm or more.
  • the N content of the cold-rolled steel sheet exceeds 1000 ppm, AlN is excessively present in the steel sheet even after completion of secondary recrystallization in the final annealing. Such AlN causes iron loss deterioration. Therefore, the N content of the steel sheet is preferably set to 1000 ppm or less.
  • step S109 an annealing separator is applied to the decarburization-annealed steel sheet (after the decarburization annealing step or after the nitriding treatment step), and then final annealing is performed to obtain a final-annealed steel sheet.
  • the final annealing conditions are not limited, but the final annealing may be performed, for example, under conditions in which the temperature is raised to 1150 to 1250°C in an atmosphere gas containing hydrogen and nitrogen, and annealing (holding) is performed in the temperature range for 10 to 60 hours.
  • the final annealing is generally performed for a long time in a state where the steel sheet is wound in a coil shape.
  • an annealing separator is applied to the cold-rolled steel sheet and dried for the purpose of preventing seizure inside and outside the winding of the coil.
  • an annealing separator containing MgO as a main component is used as the annealing separator to be applied.
  • a glass coating can be formed on the surface of the base steel sheet.
  • no primary coating glass coating
  • the primary coating is a Mg 2 SiO 4 or a MgAl 2 O 4 compound, and Mg, which is necessary for the formation reaction, is not supplied.
  • the annealing separator applied to the decarburization-annealed steel sheet preferably contains at least one selected from Ti, Sb, Sr, and Cl in a total amount of 0.10 to 10.00% with respect to the weight of MgO.
  • the annealing separator containing MgO as a main component contains one or more selected from Ti, Sb, Sr, and Cl
  • the reactivity between the primary coating and AlN is suppressed, and the magnetic characteristics can be improved.
  • the mechanism is unknown, it is considered that the segregation of these elements at the interface between the primary coating and the base steel sheet suppresses the reaction between the primary coating and AlN.
  • the total amount of Ti, Sb, Sr, and Cl is preferably 0.10 to 10.00% by wt%. When the total amount of Ti, Sb, Sr, and Cl is less than 0.10% with respect to the weight of MgO, the effect of improving the magnetic characteristics may not be sufficiently obtained. On the other hand, when the total amount of Ti, Sb, Sr, and Cl exceeds 10.00%, a sufficient primary coating amount is not formed, a coating tension effective for improving magnetic characteristics cannot be secured, and the iron loss may be poor.
  • the existence form (that is, the addition means) of Ti, Sb, Sr, and Cl in the annealing separator may exist as a compound or may exist alone.
  • Ti when Ti is contained in the annealing separator, Ti may be contained as simple Ti or may be contained as a Ti oxide (for example, TiO 2 ).
  • an insulating coating (a tension-applying insulation coating) is formed on the surface (one surface or both surfaces) of the final-annealed steel sheet.
  • the conditions for forming the insulating coating are not particularly limited.
  • a treatment liquid may be applied and dried by a known method using a known insulating coating treatment liquid.
  • the insulating coating is formed on the sheet surface, the magnetic characteristics of the grain-oriented electrical steel sheet can be further improved.
  • the surface of the steel sheet on which the insulating coating is formed may be a surface that has been subjected to an arbitrary pretreatment such as a degreasing treatment with alkali or the like or a pickling treatment with hydrochloric acid, sulfuric acid, phosphoric acid, or the like, before the treatment liquid is applied; or may be a surface as it is after final annealing, having not been subjected to such a pretreatment.
  • an arbitrary pretreatment such as a degreasing treatment with alkali or the like or a pickling treatment with hydrochloric acid, sulfuric acid, phosphoric acid, or the like
  • the insulating coating formed on the surface of the steel sheet is not particularly limited as long as it is used as an insulating coating for a grain-oriented electrical steel sheet, and a known insulating coating can be used.
  • Examples of such an insulating coating include a coating containing a phosphate and colloidal silica as main components.
  • a composite insulating coating mainly containing an inorganic substance and further containing an organic substance can be exemplified.
  • the composite insulating coating is, for example, an insulating coating mainly made of at least one of a chromate metal salt, a phosphate metal salt, colloidal silica, and an inorganic substance such as a Zr compound and a Ti compound and having a fine organic resin particle dispersed therein.
  • an insulating coating using a metal phosphate, a Zr or Ti coupling agent, or a carbonate or ammonium salt thereof as a starting material may be used.
  • the method for manufacturing a grain-oriented electrical steel sheet according to the present embodiment may include a magnetic domain refinement step after the insulating coating forming step.
  • the surface of the insulating coating is irradiated with energy rays such as laser beam and electron beam at predetermined intervals in the rolling direction, thereby introducing a plurality of linear strains (thermal strains caused by rapid heating by energy ray irradiation and subsequent rapid cooling).
  • the interval at which the plurality of linear strains are formed (that is, the interval between adjacent strains) is preferably 3.0 to 9.0 mm in the rolling direction.
  • the energy ray include a laser beam and an electron beam.
  • the laser beam may be a continuous wave laser or a pulsed laser. Examples of the laser beam type include a fiber laser, a YAG laser, and a CO 2 laser.
  • the electron beam may be a continuous beam or an intermittent beam. Examples
  • the slab was heated to a temperature of 1100 to 1380°C and then hot rolled to prepare a hot-rolled steel sheet with a sheet thickness of 2.3 mm.
  • the obtained hot-rolled steel sheet was subjected to hot-band annealing. Specifically, the hot-rolled steel sheet was annealed under the conditions of an annealing temperature of 1100°C and a holding time of 20 seconds.
  • the hot-rolled steel sheet after the hot-rolled annealing (the hot-band annealed steel sheet) was subjected to surface scale removal by pickling or the like, and then cold rolling including a plurality of passes without intermediate annealing was performed to prepare a cold-rolled steel sheet with a sheet thickness of 0.16 to 0.23 mm.
  • the obtained cold-rolled steel sheet was subjected to decarburization annealing under the conditions shown in Table 3.
  • the retention time in the soaking process was set to 120 seconds in the soaking process.
  • a final annealing step was performed on the decarburization-annealed steel sheet.
  • an annealing separator mainly composed of MgO and containing elements shown in Table 3 was applied to the sheet surface by water slurry application.
  • the components contained in the annealing separator shown in Table 3 indicate the weight fraction of the element alone.
  • the decarburization-annealed steel sheet to which the annealing separator was applied was held at 1200°C for 20 hours to prepare a steel sheet having a primary coating (a glass coating) on the base steel sheet (the final-annealed steel sheet).
  • an insulating coating was formed on the steel sheet. Specifically, an insulating coating forming liquid mainly composed of colloidal silica and phosphate was applied to the surface of the steel sheet (more specifically, the surface of the glass coating as the primary coating) and heat-treated (baked). As a result, a grain-oriented electrical steel sheet including a base steel sheet, a glass coating formed on the base steel sheet, and an insulating coating formed on the glass coating was obtained.
  • the chemical composition of the base steel sheet of the obtained grain-oriented electrical steel sheet is shown in Table 2.
  • the notation "-" in the chemical composition of Table 2 means that a corresponding element content is 0% in the significant digits (numerical value up to the minimum digit) defined in the embodiment. [Table 1] No.
  • the obtained steel sheet sample was cut into a size of 60 mm parallel to the sheet width direction and 300 mm parallel to the rolling direction, and these samples were held at 800 ⁇ 50°C for 2 hours to perform straightening annealing. Thereafter, magnetic domain refinement was performed by laser irradiation.
  • the sample after laser irradiation was subjected to magnetism evaluation by a single sheet tester (SST), and an iron loss (W 17/50 ) was measured.
  • SST single sheet tester
  • W 17/50 iron loss
  • W 17/50 iron loss
  • T magnetic flux density B 8
  • the iron loss (W 17/50 ) was evaluated according to the following criteria. Evaluations A to C were determined to have excellent iron loss characteristics (low iron loss), and evaluation D was determined to have poor iron loss characteristics. Less than 0.70: evaluation A 0.70 or more and less than 0.75: evaluation B 0.75 or more and less than 0.80: evaluation C 0.80 or more: evaluation D
  • a magnetic flux density of 1.88 T or more was defined as acceptable, and a magnetic flux density of less than 1.88 T was defined as unacceptable.
  • the magnetostriction of a sample having a width of 60 mm ⁇ a length of 300 mm subjected to the magnetic domain control was measured by an AC magnetostriction measurement method using a magnetostriction measurement device.
  • the magnetostriction measurement device includes a laser Doppler vibrometer, an exciting coil, an excitation power supply, a magnetic flux detection coil, an amplifier, and an oscilloscope.
  • a correction coefficient ⁇ n values shown in Table 2 of JIS C 1509-1 (2005) were used.
  • the noise characteristics were evaluated according to the following criteria.

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EP23891609.2A 2022-11-15 2023-11-15 Kornorientiertes elektromagnetisches stahlblech und verfahren zur herstellung davon Pending EP4621089A4 (de)

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JP2562254B2 (ja) 1992-04-24 1996-12-11 新日本製鐵株式会社 薄手高磁束密度一方向性電磁鋼板の製造方法
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JP2022182571A (ja) 2021-05-28 2022-12-08 井関農機株式会社 乗用田植機

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