US20160102378A1 - Grain oriented electrical steel sheet and method of manufacturing the same - Google Patents

Grain oriented electrical steel sheet and method of manufacturing the same Download PDF

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US20160102378A1
US20160102378A1 US14/971,189 US201514971189A US2016102378A1 US 20160102378 A1 US20160102378 A1 US 20160102378A1 US 201514971189 A US201514971189 A US 201514971189A US 2016102378 A1 US2016102378 A1 US 2016102378A1
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sheet
steel sheet
annealing
subjecting
electron beam
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Takeshi Omura
Hiroi Yamaguchi
Seiji Okabe
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JFE Steel Corp
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JFE Steel Corp
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D1/00General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/74Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
    • C21D1/773Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material under reduced pressure or vacuum
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D10/00Modifying the physical properties by methods other than heat treatment or deformation
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D6/00Heat treatment of ferrous alloys
    • C21D6/001Heat treatment of ferrous alloys containing Ni
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D6/00Heat treatment of ferrous alloys
    • C21D6/005Heat treatment of ferrous alloys containing Mn
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D6/00Heat treatment of ferrous alloys
    • C21D6/008Heat treatment of ferrous alloys containing Si
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/02Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0205Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips of ferrous alloys
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    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/02Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0221Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the working steps
    • C21D8/0226Hot rolling
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    • C21DMODIFYING 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
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/02Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0221Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the working steps
    • C21D8/0236Cold rolling
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    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/02Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0278Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips involving a particular surface treatment
    • C21D8/0284Application of a separating or insulating coating
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    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/02Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0278Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips involving a particular surface treatment
    • C21D8/0289Application of a tension-inducing coating
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1244Modifying 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
    • C21D8/1255Modifying 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
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    • C21DMODIFYING 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
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1244Modifying 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
    • C21D8/1272Final recrystallisation annealing
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    • C21DMODIFYING 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
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1277Modifying 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
    • C21D8/1288Application of a tension-inducing coating
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D9/00Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/46Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for sheet metals
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/001Ferrous alloys, e.g. steel alloys containing N
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/002Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/008Ferrous alloys, e.g. steel alloys containing tin
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/02Ferrous alloys, e.g. steel alloys containing silicon
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/04Ferrous alloys, e.g. steel alloys containing manganese
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/06Ferrous alloys, e.g. steel alloys containing aluminium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/08Ferrous alloys, e.g. steel alloys containing nickel
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/18Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/34Ferrous alloys, e.g. steel alloys containing chromium with more than 1.5% by weight of silicon
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/60Ferrous alloys, e.g. steel alloys containing lead, selenium, tellurium, or antimony, or more than 0.04% by weight of sulfur
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12Magnets 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
    • H01F1/14Magnets 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
    • H01F1/16Magnets 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
    • H01F1/18Magnets 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
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D2201/00Treatment for obtaining particular effects
    • C21D2201/05Grain orientation

Definitions

  • This disclosure relates to a grain oriented electrical steel sheet preferably used for iron core materials such as transformers, and a method of manufacturing the same.
  • Grain oriented electrical steel sheets which are mainly used as iron cores of transformers, are required to have excellent magnetic properties, in particular, less iron loss.
  • JP 57-002252B proposes a technique for reducing iron loss of a steel sheet by irradiating a final product steel sheet with laser, introducing a high dislocation density region to the surface layer of the steel sheet and reducing the magnetic domain width.
  • JP 06-072266B proposes a technique to control the magnetic domain width by electron beam irradiation.
  • the actual transformer may exhibit excellent low noise properties, while maintaining excellent low iron loss properties.
  • FIG. 1 illustrates a cross-section for measuring the thickness of a forsterite film.
  • FIG. 2 illustrates the result of observing magnetic domains of the steel sheet.
  • strain-introduced side indicates the side on which electron beam has been irradiated
  • non-strain-introduced side refers to the side on which electron beam has not been irradiated.
  • the first point is control of the thickness of a forsterite film where strain is introduced. Control of the thickness of a forsterite film is important for the reasons explained below.
  • a forsterite film on a surface of the steel sheet applies tension to the steel sheet.
  • a variation in the thickness of this forsterite film leads to a non-uniform tension distribution of the steel sheet.
  • the non-uniform tension distribution results in a distortion in the magnetostrictive vibration waveform of the steel sheet which causes an increase in noise.
  • noise increases with a superimposed harmonic component. Accordingly, to mitigate this increase in noise, it is important to mitigate a reduction in the thickness of the forsterite film at the time of introduction of thermal strain.
  • a ratio (Wa/Wb) of a film thickness of the forsterite film on a strain-introduced side (Wa) to a film thickness of the forsterite film on a non-strain-introduced side (Wb) should be 0.5 or higher, preferably 0.7 or higher.
  • the thickness of the forsterite film on each side of the steel sheet before the introduction of strain is usually the same.
  • the maximum value of Wa/Wb is about 1.
  • FIG. 1 is a schematic diagram illustrating a cross-section of a steel sheet having a forsterite film.
  • the forsterite film appears to be non-uniform in thickness and has significant irregularities as viewed on a short periodic basis.
  • the thickness of the forsterite film may be determined from an average of thickness measurements by using a sufficiently large measurement distance.
  • the thickness of the forsterite film may be determined by cutting a sample from a cross-section of the steel sheet, determining an area of the forsterite film over a predetermined measurement distance (preferably 1 mm) (using, preferably, SEM observation and image analysis), and calculating an average of thickness measurements of the film on that surface.
  • a good forsterite film means a forsterite film that has fewer gaps due to cracking and thus is highly densified.
  • the tension to be applied to the steel sheet during flattening annealing If this tension is strong, the forsterite film is damaged and cracking occurs, for example.
  • the tension in an annealing furnace where the steel sheet has high temperature and thus is more sensitive to tension, it is necessary to control the tension at 15 MPa (1.5 kgf/mm2) or lower.
  • the degree of vacuum is 0.1 to 5 Pa. If the degree of vacuum is below 0.1 Pa, it is not possible to mitigate the reduction of the forsterite film. Alternatively, if the degree of vacuum is above 5 Pa, it is not possible to apply thermal strain to the steel sheet in an effective manner.
  • the degree of vacuum is more preferably 0.5 to 3 Pa. Control of magnetic domain discontinuous portions in a surface of the steel sheet on the strain-introduced side and in a surface of the steel sheet on the non-strain-introduced side
  • the second point is control of magnetic domain discontinuous portions in a surface of the steel sheet on the strain-introduced side and in a surface of the steel sheet on the non-strain-introduced side, respectively.
  • an average width of a magnetic domain discontinuous portion in a surface of the steel sheet on the strain-introduced side is 150 to 300 ⁇ m; and an average width of a magnetic domain discontinuous portion in a surface of the steel sheet on the non-strain-introduced side is 250 to 500 ⁇ m. That is, we satisfy item (i) by defining an average width of a magnetic domain discontinuous portion in a surface of the steel sheet on the non-strain-introduced side, and satisfy item (ii) by setting the upper limit of each average width. Further, the lower limit of each average width is also set because the magnetic domain refinement effect cannot be obtained for a width smaller than the lower limit.
  • each magnetic domain discontinuous portion affected by such heat usually tends to be wider than the irradiation width. Additionally, for the same reason, each magnetic domain discontinuous portion on the non-strain-introduced side has a width larger than that of each magnetic domain discontinuous portion on the strain-introduced side.
  • the width of a magnetic domain discontinuous portion may be obtained by visualizing a magnetic domain structure by the Bitter method using magnetic colloid so that discontinuous portions formed by the electron beam irradiation can be identified (see FIG. 2 ) and, furthermore, by measuring the widths of magnetic domain discontinuous portions over a predetermined measurement distance (preferably 20 mm) to calculate an average of the width measurements.
  • FIG. 2 is a schematic diagram illustrating the magnetic domain structure of the grain oriented electrical steel sheet after the magnetic domain refinement treatment, where main magnetic domains are oriented in the horizontal direction and an electron beam is irradiated in the vertical direction at the center of the figure at a substantially right angle to the horizontal direction.
  • a magnetic domain discontinuous portion indicates a region where the structure of main magnetic domain is disrupted by electron beam irradiation, and that substantially corresponds to a region affected by the heat caused by the electron beam irradiation.
  • the third point is the high degree of alignment of crystal grains of the material with the easy axis of magnetization.
  • a magnetic flux density B8 which gives an indication of the degree of alignment of crystal grains of the material with the easy axis of magnetization, should be 1.92 T or higher.
  • the magnetic flux density B8 is less than 1.92 T, rotational motion of magnetic domains to align parallel to the excitation magnetic field during the magnetization process causes a large magnetostriction. This results in an increase in transformer noise.
  • the higher the degree of crystal grain alignment the greater the magnetic domain refinement effect.
  • the magnetic flux density B8 should also be 1.92 T or higher in view of iron loss reduction.
  • the strain introduction process is limited to a method by electron beam that may reduce damage to the film at a strain-introduced portion.
  • electron beam should be irradiated in a direction transverse to the rolling direction, preferably at 60° to 90° to the rolling direction, and the irradiation interval of the electron beam is preferably about 3 to 15 mm.
  • a preferred beam diameter is 0.01 to 0.3 mm.
  • a slab for a grain oriented electrical steel sheet may have any chemical composition that allows for secondary recrystallization.
  • Al and N may be contained in an appropriate amount, respectively, while if a MnS/MnSe-based inhibitor is used, Mn and Se and/or S may be contained in an appropriate amount, respectively.
  • MnS/MnSe-based inhibitor e.g., an AlN-based inhibitor
  • Mn and Se and/or S may be contained in an appropriate amount, respectively.
  • these inhibitors may also be used in combination.
  • preferred contents of Al, N, S and Se are: Al: 0.01 to 0.065 mass %; N: 0.005 to 0.012 mass %; S: 0.005 to 0.03 mass %; and Se: 0.005 to 0.03 mass %, respectively.
  • our methods are applicable to a grain oriented electrical steel sheet having limited contents of Al, N, S and Se without using an inhibitor.
  • the amounts of Al, N, S and Se are preferably: Al: 100 mass ppm or less: N: 50 mass ppm or less; S: 50 mass ppm or less; and Se: 50 mass ppm or less, respectively.
  • C is added to improve the texture of a hot-rolled sheet.
  • C content exceeding 0.08 mass % increases the burden to reduce C content to 50 mass ppm or less where magnetic aging will not occur during the manufacturing process.
  • C content is preferably 0.08 mass % or less.
  • it is not necessary to set up a particular lower limit to C content because secondary recrystallization is enabled by a material without containing C.
  • Si is an element that is useful to increase electrical resistance of steel and improve iron loss.
  • An Si content of 2.0 mass % or more has a particularly good effect in reducing iron loss.
  • an Si content of 8.0 mass % or less may offer particularly good formability and magnetic flux density.
  • the Si content is preferably 2.0 to 8.0 mass %.
  • Mn is an element advantageous in improving hot formability. However, Mn content less than 0.005 mass % has a less addition effect. On the other hand, Mn content of 1.0 mass % or less provides a particularly good magnetic flux density to the product sheet. Thus, Mn content is preferably 0.005 to 1.0 mass %.
  • the slab may also contain the following elements as elements to improve magnetic properties:
  • Ni is an element useful to further improve the texture of a hot-rolled sheet to obtain even more improved magnetic properties.
  • an Ni content of less than 0.03 mass % is less effective in improving magnetic properties, whereas an Ni content of 1.5 mass % or less increases, in particular, the stability of secondary recrystallization and provides even more improved magnetic properties.
  • Ni content is preferably 0.03 to 1.5 mass %.
  • Sn, Sb, Cu, P, Mo and Cr are elements useful to improve the magnetic properties, respectively. However, if any of these elements is contained in an amount less than its lower limit described above, it is less effective to improve the magnetic properties, whereas if present in an amount equal to or less than its upper limit described above, it gives the best growth of secondary recrystallized grains. Thus, each of these elements is preferably present in an amount within the above-described range.
  • the balance other than the above-described elements is Fe and incidental impurities that are incorporated during the manufacturing process.
  • the slab having the above-described chemical composition is subjected to heating before hot rolling in a conventional manner.
  • the slab may also be subjected to hot rolling directly after casting, without being subjected to heating.
  • it may be subjected to hot rolling or proceed to the subsequent step, omitting hot rolling.
  • the hot rolled sheet is optionally subjected to hot rolled sheet annealing.
  • a main purpose of the hot rolled sheet annealing is to improve the magnetic properties by dissolving the band texture generated by hot rolling to obtain a primary recrystallization texture of uniformly-sized grains, and thereby further developing a Goss texture during secondary recrystallization annealing.
  • a hot rolled sheet annealing temperature is preferably 800° C. to 1100° C.
  • a hot rolled sheet annealing temperature is lower than 800° C., there remains a band texture resulting from hot rolling, which makes it difficult to obtain a primary recrystallization texture of uniformly-sized grains and impedes a desired improvement of secondary recrystallization.
  • a hot rolled sheet annealing temperature exceeds 1100° C., the grain size after the hot rolled sheet annealing coarsens too much, which makes it difficult to obtain a primary recrystallization texture of uniformly-sized grains.
  • the sheet After the hot rolled sheet annealing, the sheet is preferably subjected to cold rolling once, or twice or more with intermediate annealing performed therebetween, to be finished to a final sheet thickness. The sheet is subjected to subsequent decarburization (combined with recrystallization annealing). Then, an annealing separator is applied to the sheet. After the application of the annealing separator, the sheet is subjected to final annealing for purposes of secondary recrystallization and formation of a forsterite film. It should be noted that the annealing separator is preferably composed mainly of MgO to form forsterite.
  • the phrase “composed mainly of MgO” implies that any well-known compound for the annealing separator and any property improvement compound other than MgO may also be contained within a range without interfering with the formation of a forsterite film intended.
  • Tension coating includes inorganic coating containing silica and ceramic coating by physical vapor deposition, chemical vapor deposition, and so on.
  • the grain oriented electrical steel sheet after final annealing or tension coating as mentioned above is subjected to magnetic domain refining by irradiating the surfaces of the steel sheet with an electron beam.
  • the degree of vacuum during the electron beam irradiation may be controlled as mentioned above to make full use of the thermal strain application effect through the electron beam irradiation, while minimizing damage to the film.
  • Steel slabs each having a chemical composition containing the following elements, were manufactured by continuous casting: C: 0.08 mass %; Si: 3.1 mass %; Mn: 0.05 mass %; Ni: 0.01 mass %; Al: 230 mass ppm; N: 90 mass ppm; Se: 180 mass ppm; S: 20 mass ppm; O: 22 mass ppm; and the balance being Fe and incidental impurities. Then, each of these steel slabs was heated to 1400° C., subjected to hot rolling to be finished to a hot-rolled sheet having a sheet thickness of 2.0 mm, and then subjected to hot rolled sheet annealing at 1100° C. for 120 seconds.
  • each steel sheet was subjected to hydrochloric acid pickling to remove subscales from the surfaces thereof, followed by cold rolling again to be finished to a cold-rolled sheet having a sheet thickness of 0.23 mm.
  • each steel sheet was subjected to decarburization where it was retained at a degree of oxidation PH2O/PH2 of 0.50 and a soaking temperature of 830° C. for 60 seconds. Then, an annealing separator composed mainly of MgO was applied to each steel sheet. Thereafter, each steel sheet was subjected to final annealing for the purposes of secondary recrystallization, formation of a forsterite film and purification under the conditions of 1200° C. and 30 hours. Then, an insulation coating composed of 60% colloidal silica and aluminum phosphate was applied to each steel sheet, which in turn was baked at 800° C. This coating application process also serves as flattening annealing.
  • each steel sheet was subjected to magnetic domain refinement treatment where it was irradiated with electron beam at irradiation width of 0.15 mm and irradiation interval of 5.0 mm in a direction perpendicular to the rolling direction. Then, each steel sheet was evaluated for magnetic properties as a product.
  • the primary recrystallization annealing temperature was varied to obtain materials, each having a value of magnetic flux density B8 of 1.90 to 1.95 T.
  • an electron beam was irradiated under different conditions with different beam current values and beam scanning rates.
  • each product was subjected to oblique shearing to be assembled into a three-phase transformer at 500 kVA, and then measured for its iron loss and noise in a state where it was excited at 50 Hz and 1.7 T.
  • This transformer has design values of iron loss and noise of 55 dB and 0.83 W/kg, respectively. The above-mentioned measurement results on iron loss and noise are shown in Table 1.
  • each grain oriented electrical steel sheet which was subjected to magnetic domain refining treatment by an electron beam and falls within our range, produces low noise when assembled as an actual transformer and inhibits degradation in iron loss properties.
  • the resulting iron loss and low noise properties are consistent with the design value.
  • Comparative Examples of steel sample IDs 11 and 12 which are outside our range in terms of their magnetic flux densities, all failed to show either low noise properties or low iron loss properties.

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Abstract

A method of manufacturing a grain oriented electrical steel sheet includes subjecting a slab to rolling to a final sheet thickness; subjecting the sheet to subsequent decarburization; applying an annealing separator composed mainly of MgO to a surface of the sheet before subjecting the sheet to final annealing; subjecting the sheet to subsequent tension coating; and subjecting, after the final annealing or the tension coating, the sheet to magnetic domain refining treatment by electron beam irradiation, wherein a degree of vacuum during the electron beam irradiation is 0.1 to 5 Pa, and a tension to be exerted on the steel sheet during flattening annealing is 5 to 15 MPa.

Description

    RELATED APPLICATIONS
  • This is a divisional of U.S. application Ser. No. 13/814,357, filed Feb. 5, 2013, which is a §371 of International Application No. PCT/JP2011/004410, with an international filing date of Aug. 3, 2011 (WO 2012/017655A1, published Feb. 9, 2012), which is based on Japanese Patent Application No. 2010-177619 filed Aug. 6, 2010.
  • TECHNICAL FIELD
  • This disclosure relates to a grain oriented electrical steel sheet preferably used for iron core materials such as transformers, and a method of manufacturing the same.
  • BACKGROUND
  • Grain oriented electrical steel sheets, which are mainly used as iron cores of transformers, are required to have excellent magnetic properties, in particular, less iron loss.
  • To meet this requirement, it is important that secondary recrystallized grains are highly aligned in the steel sheet in the (110)[001] orientation (or so-called the Goss orientation) and impurities in the product steel sheet are reduced. Additionally, there are limitations to control crystal orientation and reduce impurities in terms of balancing with manufacturing cost, and so on. Therefore, some techniques have been developed to introduce non-uniformity to the surfaces of a steel sheet in a physical manner and reducing the magnetic domain width for less iron loss, namely, magnetic domain refining techniques.
  • For example, JP 57-002252B proposes a technique for reducing iron loss of a steel sheet by irradiating a final product steel sheet with laser, introducing a high dislocation density region to the surface layer of the steel sheet and reducing the magnetic domain width. JP 06-072266B proposes a technique to control the magnetic domain width by electron beam irradiation.
  • However, when a grain oriented electrical steel sheet that has been subjected to the above-mentioned magnetic domain refining treatment is assembled into an actual transformer, it may produce significant noise.
  • It could therefore be helpful to provide a grain oriented electrical steel sheet that may exhibit excellent low noise and low iron loss properties when assembled as an actual transformer, along with an advantageous method of manufacturing the same.
  • SUMMARY
  • We thus provide:
      • [1] A grain oriented electrical steel sheet comprising a forsterite film formed on a surface thereof, being subjected to strain introduction by electron beam and having a magnetic flux density B8 of 1.92 T or higher,
        • wherein a ratio (Wa/Wb) of a film thickness of the forsterite film on a strain-introduced side of the steel sheet (Wa) to a film thickness of the forsterite film on a non-strain-introduced side of the steel sheet (Wb) is 0.5 or higher, and
        • wherein a magnetic domain discontinuous portions in a surface of the steel sheet on the strain-introduced side has an average width of 150 to 300 μm, and a magnetic domain discontinuous portion in a surface of the steel sheet on the non-strain-introduced side has an average width of 250 to 500 μm.
      • [2] A method of manufacturing a grain oriented electrical steel sheet, the method comprising:
        • subjecting a slab for a grain oriented electrical steel sheet to rolling to be finished to a final sheet thickness;
        • subjecting the sheet to subsequent decarburization;
        • then applying an annealing separator composed mainly of MgO to a surface of the sheet before subjecting the sheet to final annealing;
        • subjecting the sheet to subsequent tension coating; and
        • subjecting, after the final annealing or the tension coating, the sheet to magnetic domain refining treatment by electron beam irradiation, wherein
        • (1) the degree of vacuum during the electron beam irradiation is 0.1 to 5 Pa, and
        • (2) a tension to be exerted on the steel sheet during flattening annealing is controlled at 5 to 15 MPa.
      • [3] The method of manufacturing a grain oriented electrical steel sheet according to item [2] above, wherein the slab for the grain oriented electrical steel sheet is subjected to hot rolling, and optionally, hot rolled sheet annealing, and subsequently subjected to cold rolling once, or twice or more with intermediate annealing performed therebetween, to be finished to a final sheet thickness.
  • It is possible to provide a grain oriented electrical steel sheet that allows an actual transformer assembled therefrom to effectively maintain the effect of reducing iron loss by magnetic domain refinement using an electron beam. Therefore, the actual transformer may exhibit excellent low noise properties, while maintaining excellent low iron loss properties.
  • BRIEF DESCRIPTION OF THE DRAWINGS
  • Our steel sheets will be further described below with reference to the accompanying drawings, wherein:
  • FIG. 1 illustrates a cross-section for measuring the thickness of a forsterite film.
  • FIG. 2 illustrates the result of observing magnetic domains of the steel sheet.
  • DETAILED DESCRIPTION
  • We analyzed the cause of increases in noise when using a grain oriented electrical steel sheet subjected to magnetic domain refinement treatment as an actual transformer. As a result, we found that an increase in transformer noise is caused by a reduction in the thickness of a forsterite film (a film composed mainly of Mg2SiO4) in the strain-introduced portion when thermal strain is introduced for magnetic domain refinement. In this respect, we also found that noise degradation can be prevented by appropriately adjusting a ratio of a film thickness of the forsterite film on a strain-introduced side of the steel sheet (Wa) to a film thickness of the forsterite film on a non-strain-introduced side of the steel sheet (Wb).
  • Further, we found that both the average width of a magnetic domain discontinuous portion in a surface of the steel sheet on the strain-introduced side and the average width of a magnetic domain discontinuous portion in a surface of the steel sheet on the non-strain-introduced side have to be adjusted within a proper range. As used herein, the term strain-introduced side indicates the side on which electron beam has been irradiated, and non-strain-introduced side refers to the side on which electron beam has not been irradiated.
  • Our steel sheets and methods will be specifically described below.
  • One of the measures to be taken to mitigate an increase in noise when using a grain oriented electrical steel sheet as an actual transformer that has been subjected to strain application and magnetic domain refinement treatment is to satisfy all of the three points given below.
  • Control of the Thickness of a Forsterite Film on the Strain-Introduced Side
  • The first point is control of the thickness of a forsterite film where strain is introduced. Control of the thickness of a forsterite film is important for the reasons explained below.
  • A forsterite film on a surface of the steel sheet applies tension to the steel sheet. A variation in the thickness of this forsterite film leads to a non-uniform tension distribution of the steel sheet. The non-uniform tension distribution results in a distortion in the magnetostrictive vibration waveform of the steel sheet which causes an increase in noise. As a result, noise increases with a superimposed harmonic component. Accordingly, to mitigate this increase in noise, it is important to mitigate a reduction in the thickness of the forsterite film at the time of introduction of thermal strain. That is, a ratio (Wa/Wb) of a film thickness of the forsterite film on a strain-introduced side (Wa) to a film thickness of the forsterite film on a non-strain-introduced side (Wb) should be 0.5 or higher, preferably 0.7 or higher.
  • Besides, the thickness of the forsterite film on each side of the steel sheet before the introduction of strain is usually the same. Thus, the maximum value of Wa/Wb is about 1.
  • FIG. 1 is a schematic diagram illustrating a cross-section of a steel sheet having a forsterite film. The forsterite film appears to be non-uniform in thickness and has significant irregularities as viewed on a short periodic basis. However, the thickness of the forsterite film may be determined from an average of thickness measurements by using a sufficiently large measurement distance. Specifically, the thickness of the forsterite film may be determined by cutting a sample from a cross-section of the steel sheet, determining an area of the forsterite film over a predetermined measurement distance (preferably 1 mm) (using, preferably, SEM observation and image analysis), and calculating an average of thickness measurements of the film on that surface.
  • To satisfy the above-described ratio (Wa/Wb), it is important to mitigate a reduction in the thickness of the forsterite film where thermal strain is applied as mentioned above. Means for mitigating this reduction will be described below. Above all, it is important to form a good forsterite film. As used herein, a good forsterite film means a forsterite film that has fewer gaps due to cracking and thus is highly densified. In addition, what is the most influential factor among those causing damage such as cracking to the forsterite film is the tension to be applied to the steel sheet during flattening annealing. If this tension is strong, the forsterite film is damaged and cracking occurs, for example. Thus, in an annealing furnace where the steel sheet has high temperature and thus is more sensitive to tension, it is necessary to control the tension at 15 MPa (1.5 kgf/mm2) or lower.
  • On the other hand, we control the above-described tension to be 5 MPa (0.5 kgf/mm2) or higher. This is because the tension of less than 5 MPa results in inadequate shape correction of the steel sheet. In addition, it is necessary to control the degree of vacuum during electron beam irradiation. It is generally believed that a higher degree of vacuum is better for electron beam irradiation. However, we found that allowing an adequate amount of oxygen to be left during electron beam irradiation is effective in mitigating reduction of the forsterite film. While the mechanism for this has not been clarified, we believe as follows: oxidation of the steel sheet due to the residual oxygen at the time of introduction of thermal strain might have some influence on maintenance of the film thickness of the forsterite film. To mitigate a reduction in the film thickness of the forsterite film, the degree of vacuum is 0.1 to 5 Pa. If the degree of vacuum is below 0.1 Pa, it is not possible to mitigate the reduction of the forsterite film. Alternatively, if the degree of vacuum is above 5 Pa, it is not possible to apply thermal strain to the steel sheet in an effective manner. The degree of vacuum is more preferably 0.5 to 3 Pa. Control of magnetic domain discontinuous portions in a surface of the steel sheet on the strain-introduced side and in a surface of the steel sheet on the non-strain-introduced side
  • The second point is control of magnetic domain discontinuous portions in a surface of the steel sheet on the strain-introduced side and in a surface of the steel sheet on the non-strain-introduced side, respectively.
  • While this control of the thickness of the forsterite film may somewhat mitigate an increase in noise, an actual transformer is required to exhibit even lower noise properties and still lower iron loss properties.
  • In other words, to reduce the iron loss of a transformer, it is also important to reduce the iron loss of the material. That is, to make full use of the magnetic domain refinement effect in the material, the following are important:
      • (i) To introduce strain until magnetic domain discontinuous portions are also produced in a surface of the steel sheet on the strain-introduced side and in a surface of the steel sheet on the non-strain-introduced side, respectively; and
      • (ii) To minimize the width of each magnetic domain discontinuous portion because strain introduction leads to degradation in hysteresis loss.
  • The following are specific conditions under which the above items (i) and (ii) are satisfied: an average width of a magnetic domain discontinuous portion in a surface of the steel sheet on the strain-introduced side is 150 to 300 μm; and an average width of a magnetic domain discontinuous portion in a surface of the steel sheet on the non-strain-introduced side is 250 to 500 μm. That is, we satisfy item (i) by defining an average width of a magnetic domain discontinuous portion in a surface of the steel sheet on the non-strain-introduced side, and satisfy item (ii) by setting the upper limit of each average width. Further, the lower limit of each average width is also set because the magnetic domain refinement effect cannot be obtained for a width smaller than the lower limit.
  • It should be noted that if the maximum tension during flattening annealing and the degree of vacuum during electron beam irradiation are not satisfied as described earlier in relation to the first point, it is extremely difficult to satisfy the above-described heat-affected width without reducing the thickness of the forsterite film.
  • It should be noted here that what is important is the average widths of magnetic domain discontinuous portions, rather than the average irradiation width. That is, when heat is introduced to the steel sheet, it is diffused in every direction such as the sheet thickness direction or sheet width direction. Accordingly, each magnetic domain discontinuous portion affected by such heat usually tends to be wider than the irradiation width. Additionally, for the same reason, each magnetic domain discontinuous portion on the non-strain-introduced side has a width larger than that of each magnetic domain discontinuous portion on the strain-introduced side.
  • The width of a magnetic domain discontinuous portion may be obtained by visualizing a magnetic domain structure by the Bitter method using magnetic colloid so that discontinuous portions formed by the electron beam irradiation can be identified (see FIG. 2) and, furthermore, by measuring the widths of magnetic domain discontinuous portions over a predetermined measurement distance (preferably 20 mm) to calculate an average of the width measurements. FIG. 2 is a schematic diagram illustrating the magnetic domain structure of the grain oriented electrical steel sheet after the magnetic domain refinement treatment, where main magnetic domains are oriented in the horizontal direction and an electron beam is irradiated in the vertical direction at the center of the figure at a substantially right angle to the horizontal direction. A magnetic domain discontinuous portion indicates a region where the structure of main magnetic domain is disrupted by electron beam irradiation, and that substantially corresponds to a region affected by the heat caused by the electron beam irradiation.
  • High Degree of Alignment of Crystal Grains of the Material with the Easy Axis of Magnetization
  • The third point is the high degree of alignment of crystal grains of the material with the easy axis of magnetization.
  • Regarding the transformer noise, i.e., magnetostrictive vibration, the oscillation amplitude becomes smaller as the degree of alignment of crystal grains of the material with the easy axis of magnetization becomes higher. Therefore, for noise reduction, a magnetic flux density B8, which gives an indication of the degree of alignment of crystal grains of the material with the easy axis of magnetization, should be 1.92 T or higher. In this case, if the magnetic flux density B8 is less than 1.92 T, rotational motion of magnetic domains to align parallel to the excitation magnetic field during the magnetization process causes a large magnetostriction. This results in an increase in transformer noise. In addition, the higher the degree of crystal grain alignment, the greater the magnetic domain refinement effect. The magnetic flux density B8 should also be 1.92 T or higher in view of iron loss reduction.
  • The strain introduction process is limited to a method by electron beam that may reduce damage to the film at a strain-introduced portion. In this case, when electron beam irradiation is performed, electron beam should be irradiated in a direction transverse to the rolling direction, preferably at 60° to 90° to the rolling direction, and the irradiation interval of the electron beam is preferably about 3 to 15 mm. In addition, the electron beam is irradiated in a spot-like or linear fashion under the following conditions: acceleration voltage=10 to 200 kV; current=0.1 to 100 mA; and beam diameter=0.01 to 0.5 mm. A preferred beam diameter is 0.01 to 0.3 mm.
  • Next, the conditions of manufacturing a grain oriented electrical steel sheet will be specifically described below.
  • A slab for a grain oriented electrical steel sheet may have any chemical composition that allows for secondary recrystallization.
  • In addition, if an inhibitor, e.g., an AlN-based inhibitor is used, Al and N may be contained in an appropriate amount, respectively, while if a MnS/MnSe-based inhibitor is used, Mn and Se and/or S may be contained in an appropriate amount, respectively. Of course, these inhibitors may also be used in combination. In this case, preferred contents of Al, N, S and Se are: Al: 0.01 to 0.065 mass %; N: 0.005 to 0.012 mass %; S: 0.005 to 0.03 mass %; and Se: 0.005 to 0.03 mass %, respectively.
  • Further, our methods are applicable to a grain oriented electrical steel sheet having limited contents of Al, N, S and Se without using an inhibitor.
  • In this case, the amounts of Al, N, S and Se are preferably: Al: 100 mass ppm or less: N: 50 mass ppm or less; S: 50 mass ppm or less; and Se: 50 mass ppm or less, respectively.
  • The basic elements and other optionally added elements of the slab for a grain oriented electrical steel sheet will be specifically described below.
  • C: 0.08 Mass % or Less
  • C is added to improve the texture of a hot-rolled sheet. However, C content exceeding 0.08 mass % increases the burden to reduce C content to 50 mass ppm or less where magnetic aging will not occur during the manufacturing process. Thus, C content is preferably 0.08 mass % or less. Besides, it is not necessary to set up a particular lower limit to C content because secondary recrystallization is enabled by a material without containing C.
  • Si: 2.0 to 8.0 Mass %
  • Si is an element that is useful to increase electrical resistance of steel and improve iron loss. An Si content of 2.0 mass % or more has a particularly good effect in reducing iron loss. On the other hand, an Si content of 8.0 mass % or less may offer particularly good formability and magnetic flux density. Thus, the Si content is preferably 2.0 to 8.0 mass %.
  • Mn: 0.005 to 1.0 Mass %
  • Mn is an element advantageous in improving hot formability. However, Mn content less than 0.005 mass % has a less addition effect. On the other hand, Mn content of 1.0 mass % or less provides a particularly good magnetic flux density to the product sheet. Thus, Mn content is preferably 0.005 to 1.0 mass %.
  • Further, in addition to the above elements, the slab may also contain the following elements as elements to improve magnetic properties:
      • at least one element selected from: Ni: 0.03 to 1.50 mass %; Sn: 0.01 to 1.50 mass %; Sb: 0.005 to 1.50 mass %; Cu: 0.03 to 3.0 mass %; P: 0.03 to 0.50 mass %; Mo: 0.005 to 0.10 mass %; and Cr: 0.03 to 1.50 mass %.
  • Ni is an element useful to further improve the texture of a hot-rolled sheet to obtain even more improved magnetic properties. However, an Ni content of less than 0.03 mass % is less effective in improving magnetic properties, whereas an Ni content of 1.5 mass % or less increases, in particular, the stability of secondary recrystallization and provides even more improved magnetic properties. Thus, Ni content is preferably 0.03 to 1.5 mass %.
  • Sn, Sb, Cu, P, Mo and Cr are elements useful to improve the magnetic properties, respectively. However, if any of these elements is contained in an amount less than its lower limit described above, it is less effective to improve the magnetic properties, whereas if present in an amount equal to or less than its upper limit described above, it gives the best growth of secondary recrystallized grains. Thus, each of these elements is preferably present in an amount within the above-described range. The balance other than the above-described elements is Fe and incidental impurities that are incorporated during the manufacturing process.
  • Then, the slab having the above-described chemical composition is subjected to heating before hot rolling in a conventional manner. However, the slab may also be subjected to hot rolling directly after casting, without being subjected to heating. In the case of a thin slab, it may be subjected to hot rolling or proceed to the subsequent step, omitting hot rolling.
  • Further, the hot rolled sheet is optionally subjected to hot rolled sheet annealing. A main purpose of the hot rolled sheet annealing is to improve the magnetic properties by dissolving the band texture generated by hot rolling to obtain a primary recrystallization texture of uniformly-sized grains, and thereby further developing a Goss texture during secondary recrystallization annealing. As this moment, to obtain a highly-developed Goss texture in a product sheet, a hot rolled sheet annealing temperature is preferably 800° C. to 1100° C. If a hot rolled sheet annealing temperature is lower than 800° C., there remains a band texture resulting from hot rolling, which makes it difficult to obtain a primary recrystallization texture of uniformly-sized grains and impedes a desired improvement of secondary recrystallization. On the other hand, if a hot rolled sheet annealing temperature exceeds 1100° C., the grain size after the hot rolled sheet annealing coarsens too much, which makes it difficult to obtain a primary recrystallization texture of uniformly-sized grains.
  • After the hot rolled sheet annealing, the sheet is preferably subjected to cold rolling once, or twice or more with intermediate annealing performed therebetween, to be finished to a final sheet thickness. The sheet is subjected to subsequent decarburization (combined with recrystallization annealing). Then, an annealing separator is applied to the sheet. After the application of the annealing separator, the sheet is subjected to final annealing for purposes of secondary recrystallization and formation of a forsterite film. It should be noted that the annealing separator is preferably composed mainly of MgO to form forsterite. As used herein, the phrase “composed mainly of MgO” implies that any well-known compound for the annealing separator and any property improvement compound other than MgO may also be contained within a range without interfering with the formation of a forsterite film intended.
  • After the final annealing, it is effective to subject the sheet to flattening annealing to correct the shape thereof. Insulation coating is applied to the surfaces of the steel sheet before or after the flattening annealing. As used herein, this insulation coating means such coating that may apply tension to the steel sheet to reduce iron loss (hereinafter, referred to as tension coating). Tension coating includes inorganic coating containing silica and ceramic coating by physical vapor deposition, chemical vapor deposition, and so on.
  • The grain oriented electrical steel sheet after final annealing or tension coating as mentioned above is subjected to magnetic domain refining by irradiating the surfaces of the steel sheet with an electron beam. The degree of vacuum during the electron beam irradiation may be controlled as mentioned above to make full use of the thermal strain application effect through the electron beam irradiation, while minimizing damage to the film.
  • Except the above-mentioned steps and manufacturing conditions, it is possible to apply a conventionally known method of manufacturing a grain oriented electrical steel sheet where magnetic domain refining treatment is performed by an electron beam.
  • Experiment 1
  • Steel slabs, each having a chemical composition containing the following elements, were manufactured by continuous casting: C: 0.08 mass %; Si: 3.1 mass %; Mn: 0.05 mass %; Ni: 0.01 mass %; Al: 230 mass ppm; N: 90 mass ppm; Se: 180 mass ppm; S: 20 mass ppm; O: 22 mass ppm; and the balance being Fe and incidental impurities. Then, each of these steel slabs was heated to 1400° C., subjected to hot rolling to be finished to a hot-rolled sheet having a sheet thickness of 2.0 mm, and then subjected to hot rolled sheet annealing at 1100° C. for 120 seconds. Subsequently, each steel sheet was subjected to cold rolling to an intermediate sheet thickness of 0.65 mm, and then to intermediate annealing under the following conditions: degree of oxidation PH2O/PH2=0.32, temperature=1000° C., and duration=60 seconds. Subsequently, each steel sheet was subjected to hydrochloric acid pickling to remove subscales from the surfaces thereof, followed by cold rolling again to be finished to a cold-rolled sheet having a sheet thickness of 0.23 mm.
  • Then, each steel sheet was subjected to decarburization where it was retained at a degree of oxidation PH2O/PH2 of 0.50 and a soaking temperature of 830° C. for 60 seconds. Then, an annealing separator composed mainly of MgO was applied to each steel sheet. Thereafter, each steel sheet was subjected to final annealing for the purposes of secondary recrystallization, formation of a forsterite film and purification under the conditions of 1200° C. and 30 hours. Then, an insulation coating composed of 60% colloidal silica and aluminum phosphate was applied to each steel sheet, which in turn was baked at 800° C. This coating application process also serves as flattening annealing.
  • Thereafter, one side of each steel sheet was subjected to magnetic domain refinement treatment where it was irradiated with electron beam at irradiation width of 0.15 mm and irradiation interval of 5.0 mm in a direction perpendicular to the rolling direction. Then, each steel sheet was evaluated for magnetic properties as a product. The primary recrystallization annealing temperature was varied to obtain materials, each having a value of magnetic flux density B8 of 1.90 to 1.95 T. In addition, an electron beam was irradiated under different conditions with different beam current values and beam scanning rates. Then, each product was subjected to oblique shearing to be assembled into a three-phase transformer at 500 kVA, and then measured for its iron loss and noise in a state where it was excited at 50 Hz and 1.7 T. This transformer has design values of iron loss and noise of 55 dB and 0.83 W/kg, respectively. The above-mentioned measurement results on iron loss and noise are shown in Table 1.
  • TABLE 1
    Magnetic Magnetic
    Degree domain domain
    Tension of vacuum discontinuous discontinuous
    in furnace during portion on portion on
    during electron strain- non-strain-i
    flattening beam introduced ntroduced
    Material annealing irradiation side side Transformer
    ID W17/50(W/kg) Bs (T) (MPa) (Pa) Wa/Wb (μm) (μm) W17/50(W/kg) Noise (dBA) Remarks
    1 0.67 1.93 22 0.05 0 290 450 0.80 62 Comparative
    Example
    2 0.67 1.93 16 0.05 0.2 280 440 0.80 62 Comparative
    Example
    3 0.67 1.93 15 1.0 0.3 260 420 0.80 61 Comparative
    Example
    4 0.67 1.93 9 2.0 0.6 250 360 0.81 55 Example
    of Present
    Invention
    5 0.67 1.93 9 1.5 0.8 220 320 0.80 54 Example
    of Present
    Invention
    6 0.73 1.93 9 3.0 0.8 350 270 0.85 54 Comparative
    Example
    7 0.67 1.93 11 2.5 1.0 190 270 0.81 54 Example
    of Present
    Invention
    8 0.76 1.93 11 1.5 1.0 120 200 0.91 54 Comparative
    Example
    9 0.71 1.93 11 1.5 1.0 220 200 0.86 54 Comparative
    Example
    10 0.73 1.93 17 0.03 0 290 550 0.88 62 Comparative
    Example
    11 0.73 1.90 11 1.5 0.9 200 300 0.89 60 Comparative
    Example
    12 0.71 1.91 9 2.5 0.9 200 300 0.87 59 Comparative
    Example
    13 0.69 1.92 7 3.0 0.9 200 300 0.82 55 Example
    of Present
    Invention
    14 0.67 1.93 7 1.5 0.9 200 300 0.81 54 Example
    of Present
    Invention
    15 0.66 1.94 11 2.5 0.9 200 300 0.80 53 Example
    of Present
    Invention
    16 0.65 1.95 11 2.5 0.9 200 300 0.79 53 Example
    of Present
    Invention
  • As shown in Table 1, each grain oriented electrical steel sheet, which was subjected to magnetic domain refining treatment by an electron beam and falls within our range, produces low noise when assembled as an actual transformer and inhibits degradation in iron loss properties. The resulting iron loss and low noise properties are consistent with the design value.
  • In contrast, Comparative Examples of steel sample IDs 11 and 12, which are outside our range in terms of their magnetic flux densities, all failed to show either low noise properties or low iron loss properties. In addition, Comparative Examples of steel sample IDs 1 to 3 and 10, each of which has a value of (Wa/Wb) less than 0.5, did not offer low noise properties. Further, Comparative Examples of steel sample IDs 6, 8 and 9, which are outside our range in terms of the average width of a magnetic domain discontinuous portion in a surface of the steel sheet either on the strain-introduced side or non-strain-introduced side, proved to exhibit inferior iron loss properties.

Claims (2)

1. A method of manufacturing a grain oriented electrical steel sheet comprising:
subjecting a slab to rolling to a final sheet thickness;
subjecting the sheet to subsequent decarburization;
applying an annealing separator composed mainly of MgO to a surface of the sheet before subjecting the sheet to final annealing;
subjecting the sheet to subsequent tension coating; and
subjecting, after the final annealing or the tension coating, the sheet to magnetic domain refining treatment by electron beam irradiation, wherein
(1) a degree of vacuum during the electron beam irradiation is 0.1 to 5 Pa, and
(2) a tension to be exerted on the steel sheet during flattening annealing is 5 to 15 MPa.
2. The method according to claim 1, wherein the slab for the grain oriented electrical steel sheet is subjected to hot rolling and, optionally, hot rolled sheet annealing, and subsequently subjected to cold rolling once, or twice or more with intermediate annealing performed therebetween, to be finished to a final sheet thickness.
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