EP2460902A1 - Kornorientiertes magnetstahlblech - Google Patents

Kornorientiertes magnetstahlblech Download PDF

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EP2460902A1
EP2460902A1 EP10804595A EP10804595A EP2460902A1 EP 2460902 A1 EP2460902 A1 EP 2460902A1 EP 10804595 A EP10804595 A EP 10804595A EP 10804595 A EP10804595 A EP 10804595A EP 2460902 A1 EP2460902 A1 EP 2460902A1
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Prior art keywords
precipitates
steel sheet
ppm
annealing
sheets
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French (fr)
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EP2460902A4 (de
EP2460902B1 (de
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Takeshi Imamura
Yukihiro Shingaki
Mineo Muraki
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JFE Steel Corp
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JFE Steel Corp
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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
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1244—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest
    • C21D8/1272—Final recrystallisation annealing
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1277—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties involving a particular surface treatment
    • C21D8/1283—Application of a separating or insulating coating
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/46—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for sheet metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/001—Ferrous alloys, e.g. steel alloys containing N
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/002—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
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/008—Ferrous alloys, e.g. steel alloys containing tin
    • 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
    • C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/12—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
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/20—Ferrous alloys, e.g. steel alloys containing chromium with copper
    • 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
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/34—Ferrous alloys, e.g. steel alloys containing chromium with more than 1.5% by weight of silicon
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/16—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of sheets
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D2201/00—Treatment for obtaining particular effects
    • C21D2201/05—Grain orientation

Definitions

  • the present invention relates to a grain oriented electrical steel sheet suitably used as, for example, an iron-core material for transformers and, in particular, is intended to reduce degradation of magnetic characteristics in the case of the sheet being sheared.
  • Electrical steel sheets are a material widely used for iron cores of various transformers, motors, and the like.
  • electrical steel sheets that are referred to as grain oriented electrical steel sheets have crystal grains that are highly oriented in ⁇ 110 ⁇ 001>, which is referred to as the Goss orientation.
  • patent document 1 discloses a method of making Al and S serving as inhibitor-forming elements be present in predetermined amounts, that is, a method of using A1N and MnS as inhibitors.
  • Patent document 2 discloses a method of making at least one of S and Se be present in a predetermined amount, that is, a method of using MnS or MnSe as an inhibitor. These methods are industrially used.
  • patent document 3 a technique of developing Goss oriented grains by the action of secondary recrystallization even in steel sheets having no inhibitor-forming elements has been recently presented.
  • an iron loss characteristic directly relates to energy loss of products and is considered to be the most important characteristic.
  • W 17/50 energy loss at an excitation magnetic flux density of 1.7 T and an excitation frequency of 50 Hz
  • the iron loss characteristic is also considered as an important characteristic. Even after transformers are produced, the transformers that are used need to be periodically measured in terms of iron loss characteristic for the purpose of controlling the iron loss characteristic.
  • electrical steel sheet products have the shape of a sheet and are cut so as to have a predetermined size in the production of transformers.
  • This cutting is generally performed by shearing (also referred to as slit processing) in which two blades vertically press against each other (the blades finally slide over each other) as in a pair of scissors.
  • shearing also referred to as slit processing
  • the processed surfaces are formed by tearing due to a shearing force and a large amount of strain is introduced into the steel sheets. Accordingly, degradation of magnetic characteristics due to the introduced strain tends to occur in sheared electrical steel sheets, which is problematic.
  • stress relief annealing of annealing at 700°C to 900°C for several hours may be performed after shearing.
  • stress relief annealing is performed only for small transformers having a size (length) of 500 mm or less and it cannot be performed for, for example, iron cores of large transformers having a size of several meters. Accordingly, a technique has been demanded that can reduce degradation of magnetic characteristics due to shearing in electrical steel sheets for large transformers having a size of several meters.
  • Grain oriented electrical steel sheets containing, by mass%, 3.30% to 3.34% of Si, 0.06% to 0.07% of Mn, 0.025% to 0.028% of Sb, and 0.03% to 0.04% of Cr; Nb added in various amounts of 4 ppm (on the level of unavoidable impurities), 22 ppm, 48 ppm, 65 ppm, 90 ppm, and 210 ppm; and the balance being Fe and unavoidable impurities were produced by a standard production method having recrystallization annealing (primary recrystallization annealing) and final annealing (purification annealing).
  • the steel sheets were heated at the maximum steel sheet temperature of 1,200°C to dissolve the precipitate-forming element (Nb) therein and then cooled at an average cooling rate of 20°C/hr from 900°C to 500°C and cooled to room temperature.
  • the thus-obtained grain oriented electrical steel sheets were cut into so-called Epstein specimens having a size of 30 mm x 280 mm.
  • Epstein specimens having a size of 30 mm x 280 mm.
  • two types of specimens were prepared by a process of slowly cutting the steel sheets with a wire cutter such that strain was not caused in the steel and by a general cutting process for grain oriented electrical steel sheets in which the steel sheets were cut with a shearing machine employing an upper blade and a lower blade as described above.
  • the resultant samples were measured in terms of iron loss in accordance with a method described in JIS C 2550.
  • Fig. 1 shows the results of a study about the relationship between ⁇ W (ordinate axis: W/kg) and Nb content in steel (abscissa axis: mass ppm), ⁇ W (hereafter, same definition in the present invention) being determined by subtracting the iron loss value of a sample obtained by cutting with the wire cutter from the iron loss value of a sample obtained by cutting with the shearing machine.
  • ⁇ W (hereafter, same definition in the present invention) being determined by subtracting the iron loss value of a sample obtained by cutting with the wire cutter from the iron loss value of a sample obtained by cutting with the shearing machine.
  • ⁇ W substantially represents an iron loss amount equivalent to degradation due to remaining strain.
  • the figure thus shows that the presence of Nb results in reduction of degradation of the iron loss amount due to shearing.
  • Degradation of iron loss due to shearing is caused by accumulation of strain in portions having been subjected to shearing.
  • the accumulation of strain is a phenomenon where iron atoms regularly arranged in iron crystal grains are subjected to an external stress or the like and the arrangement of iron atoms is distorted or becomes irregular.
  • the above-described precipitates are present in such regularly arranged iron atoms.
  • Nb contained in a steel sheet is in two states of forming a solid solution and forming precipitates, as described above, it is probably important that Nb forms precipitates.
  • the sample containing 22 ppm of Nb was measured in terms of Nb precipitation percentage (percentage of Nb content in precipitates with respect to the total Nb content).
  • the total Nb content (content in a steel sheet: mass%) needs to be first determined.
  • the total Nb content can be determined by inductively-coupled plasma optical emission spectrometry (ICP optical emission spectrometry) described in JIS G 1237.
  • ICP optical emission spectrometry inductively-coupled plasma optical emission spectrometry
  • the contents of Ta, V, and Zr can be respectively determined by methods described in JIS G 1236, JIS G 1221, and JIS G 1232.
  • the Nb content in precipitates (content in a steel sheet: mass%) can be determined by melting a steel sheet by electrolysis to capture precipitates only (by filtration), measuring the weight of Nb in the precipitates, and calculating from a decrease in the weight of the steel sheet due to electrolysis and the weight of Nb in the precipitates.
  • the quantitative value of Nb content in precipitates is determined in the following manner. A product sheet is first cut so as to have a size of 50 mm x 20 mm and immersed for 2 minutes in a 10% aqueous solution of HCl heated at 85°C to remove the coating and film of the product. After that, the weight of the product sheet is measured.
  • the product sheet is electrolyzed with a commercially available electrolytic solution (10% AA solution: 10% acetylacetone-1% tetramethylammonium chloride-methanol) such that about 1 g of the product sheet is electrolyzed.
  • a commercially available electrolytic solution (10% AA solution: 10% acetylacetone-1% tetramethylammonium chloride-methanol)
  • the product sheet is immersed in an ethanol solution and subjected to ultrasonic waves.
  • This ethanol solution and the electrolytic solution used in the electrolysis, which contain precipitates, are filtrated through a 0.1 ⁇ m-mesh filter paper (allowing capture of minimum precipitates having a size on the order of nanometers) to capture the precipitates.
  • the precipitates collected by the filtration are placed together with the filter paper in a platinum crucible, heated at 700°C for an hour, mixed with Na 2 B 4 O 7 and NaCO 3 , and heated at 900°C for 15 minutes.
  • the resultant substance is cooled and then heated at 1,000°C for 15 minutes.
  • the substance in the crucible coagulates.
  • the crucible containing the substance is placed into a 25% aqueous solution of HCl and the solution containing the crucible is heated at 90°C for 30 minutes to melt the entirety of the substance.
  • the resultant solution is analyzed by ICP optical emission spectrometry described in JIS G 1237 to determine the weight of Nb in the precipitates.
  • the weight of Nb is divided by a decrease in the weight of the product sheet (steel sheet) due to electrolysis to determine the Nb content (mass%) in the precipitates.
  • the thus-determined Nb content (mass%) in the precipitates is divided by the total Nb content (mass%) to determine the Nb precipitation percentage.
  • the Nb precipitation percentage in the sample was 65%.
  • the inventors further performed studies and have found that precipitation of at least 10% of the total Nb content is necessary to provide advantages of the present invention.
  • the amount of a precipitate-forming element such as Nb remaining in steel the better the ⁇ W characteristic seems to become.
  • precipitates also degrade the iron loss characteristic of a material itself to be processed. Accordingly, the amount of precipitates is preferably small within a range in which degradation of iron loss due to shearing is small.
  • the iron loss of the materials themselves degraded and hence the content needs to be suppressed to 50 ppm or less.
  • Steel slabs containing, by mass%, 0.035% of C, 3.31% of Si, 0.13% of Mn, 0.039% of Sb, 0.05% of Cr, and 0.012% of P; 42 ppm of N and 31 ppm of S; and the balance being Fe and unavoidable impurities were produced by continuous casting, subjected to slab reheating at 1,250°C, then hot-rolled to provide hot-rolled sheets having a thickness of 2.7 mm. The hot-rolled sheets were subsequently annealed at 1,000°C for 15 seconds and then cold-rolled to provide sheets having a thickness of 0.30 mm.
  • the sheets were subjected to recrystallization annealing in a 50%N 2 -50%H 2 wet atmosphere (decarburization atmosphere) under soaking conditions in a temperature range of 800°C to 880°C for 60 seconds.
  • the sheets were then coated with an annealing separator mainly containing MgO and subsequently subjected to purification annealing by being retained in a temperature range of 1,050°C to 1,230°C for 10 hours.
  • the temperatures in the recrystallization annealing and the purification annealing were varied to vary crystal grain size provided by secondary recrystallization caused in the purification annealing.
  • the steel substrates were exposed by pickling and the crystal grain size of secondary recrystallized grains was measured.
  • the crystal grain size was determined by measuring the grain sizes of four Epstein specimens and averaging the measured grain sizes. Analysis of the components of the steel substrates revealed 0.0018% of C, 3.30% of Si, 0.13% of Mn, 0.039% of Sb, 0.05% of Cr, and 0.011% of P, and the contents of the other elements were less than the detection limits.
  • ⁇ W ordinate axis: W/kg
  • crystal grain size abcissa axis: mm
  • features of the present invention are as follows.
  • C is an element that unavoidably enters steel. Since C causes degradation of magnetic characteristics by magnetic aging, the C content is desirably minimized. However, it is difficult to completely remove C and a C content of 0.005% or less is allowable in view of production cost, preferably 0.002% or less. There is no reason for particularly defining the lower limit of the C content.
  • the C content is industrially more than zero.
  • Si is an element necessary for increasing the resistivity of steel and achieving improvement in terms of iron loss in final product sheets.
  • the Si content is less than 1.0%, such an advantage is not sufficiently provided.
  • the Si content is more than 8.0%, the saturation flux density of a steel sheet considerably decreases. Accordingly, the Si content is limited to a range of 1.0% to 8.0%.
  • the lower limit of the Si content is preferably 3.0%.
  • the upper limit of the Si content is preferably 3.5%.
  • Mn is an element necessary for enhancing formability in hot rolling.
  • the Mn content is less than 0.005%, the effect of enhancing workability is not sufficiently provided.
  • the Mn content is more than 1.0%, secondary recrystallization becomes unstable and magnetic characteristics are degraded. Accordingly, the Mn content is limited to a range of 0.005% to 1.0%.
  • the lower limit of the Mn content is preferably 0.02%.
  • the upper limit of the Mn content is preferably 0.20%.
  • Nb or the like Nb, Ta, V, and Zr
  • the total content thereof is 10 to 50 ppm.
  • the total content of Nb or the like is less than 10 ppm, precipitates for improvement in terms of iron loss, which are the main feature of the present invention, are not sufficiently generated.
  • the upper limit of the total content is defined as 50 ppm.
  • the total content is preferably in the range of 10 to 30 ppm.
  • the precipitates of Nb or the like are present in a percentage of 10% or more and the precipitates have an average diameter (equivalent circle diameter) of 0.02 to 3 ⁇ m.
  • the average diameter is less than 0.02 ⁇ m, the precipitates are too small and stress is less likely to be concentrated.
  • the average diameter is more than 3 ⁇ m, the frequency of the presence (number) of the precipitates becomes small and the number of portions where stress is concentrated becomes small.
  • the precipitates preferably have an average diameter of 0.05 to 3 ⁇ m.
  • the lower limit is more preferably 0.12 ⁇ m, still more preferably 0.33 ⁇ m.
  • the upper limit is more preferably 1.2 ⁇ m, still more preferably 0.78 ⁇ m.
  • the precipitation percentage of the precipitates of Nb or the like is preferably 20% or more, more preferably 31% or more, still more preferably 48% or more. It is not necessary to define the upper limit and a precipitation percentage of 100% does not cause problems.
  • the average diameter of the precipitates of Nb or the like is preferably determined in the following manner: a section of an obtained sample is observed with a scanning electron microscope; micrographs of about 10 fields of view are taken at a magnification of about 10,000; the micrographs are subjected to image analysis and the average of equivalent circle diameters is determined.
  • the percentage of precipitates is preferably measured in accordance with the method described in Experiment 1.
  • the total content (mass%) of Nb or the like in precipitates should be divided by the total content (mass%) of Nb or the like in the steel sheet.
  • a precipitate-forming element one or more selected from Nb, V, and Zr are preferred because they are less likely to form defects in steel sheets during hot rolling.
  • Nb is preferred because defects during hot rolling can be reduced.
  • the essential range is also 10 to 50 ppm and the preferred range is also 10 to 30 ppm; and a preferred diameter of precipitates and a preferred precipitation percentage are the same as those described above.
  • the average grain size of secondary recrystallized grains of a material is made 5 mm or more.
  • a grain size is a general grain size in electrical steel sheets for large transformers having a size of several meters described in the Technical Problem in the present invention, regardless of such a sheet size, by controlling a temperature increase rate and an atmosphere in secondary recrystallization, the average grain size can be controlled to be 5 mm or more.
  • the average grain size of secondary recrystallized grains is preferably determined by the method described in Experiment 2. Note that a method of decreasing ⁇ W by making the average grain size of secondary recrystallized grains be less than 5 mm is not preferred because the absolute values of iron loss and magnetic flux density become poor.
  • Ni 0.010% to 1.50%
  • Ni may be added. In such a case, when the amount of Ni added is less than 0.010%, magnetic characteristics are not sufficiently enhanced. When the amount of Ni added is more than 1.50%, secondary recrystallization becomes unstable and magnetic characteristics may be degraded. Accordingly, the Ni content is preferably made in the range of 0.010% to 1.50%.
  • At least one of Cr, Cu, and P may be added.
  • the amounts of the elements added are less than the lower limits, the effect of decreasing iron loss is not sufficiently provided.
  • the amounts of the elements added are more than the upper limits, development of secondary recrystallized grains is suppressed, resulting in an unintended increase in iron loss. Accordingly, the contents of the elements are preferably in the ranges described above, respectively.
  • At least one of Sn, Sb, Bi, and Mo may be added.
  • the amounts of the elements added are less than the lower limits, the effect of enhancing the magnetic characteristic is not sufficiently provided.
  • the amounts of the elements added are more than the upper limits, development of secondary recrystallized grains is suppressed, resulting in degradation of the magnetic characteristic. Accordingly, the contents of the elements are preferably in the ranges described above, respectively.
  • an electrical steel sheet according to the present invention may further contain at least one selected from 0.010% to 1.50% of Ni, 0.01% to 0.50% of Cr, 0.01% to 0.50% of Cu, 0.005% to 0.50% of P, 0.005% to 0.50% of Sn, 0.005% to 0.50% of Sb, 0.005% to 0.50% of Bi, and 0.005% to 0.100% of Mo. Further, as for a subset constituted by elements freely selected from the group of these elements, at least one selected from elements (group) constituting the subset may be made to be contained.
  • inhibitor-forming elements for example, AIN-forming elements: Al and N, MnS-forming elements: Mn and S, MnSe-forming elements: Mn and Se, and TiN-forming elements: Ti and N
  • AIN-forming elements Al and N
  • MnS-forming elements Mn and S
  • MnSe-forming elements Mn and Se
  • TiN-forming elements Ti and N
  • the balance is Fe and normal unavoidable impurities.
  • unavoidable impurities include P, S, O, Al, N, Ti, Ca, and B (when Al and the like are not added as inhibitor-forming elements, they are impurities).
  • grooves are preferably formed in a surface of a steel sheet, the grooves having the shape of a solid line or a broken line, a width of 50 to 1,000 ⁇ m, and a depth of 10 to 50 ⁇ m, and extending in a direction so as to intersect at an angle of 15° or less a direction perpendicular to a rolling direction.
  • the formation of such grooves provides the magnetic domain refining effect, resulting in a further decrease in iron loss.
  • the space between the grooves (pitch) is preferably about 2 to 7 mm.
  • grooves When grooves extend at an angle of 0° with respect to a direction perpendicular to a rolling direction, in a strict sense, the grooves do not intersect the direction perpendicular to the rolling direction; however, such a case is also referred to as intersection. In summary, grooves should be formed at an angle of 15° or less with respect to a direction perpendicular to a rolling direction. As a result of the formation of such grooves, the iron loss of an electrical steel sheet according to the present invention decreases by about 0.17 W/kg. Such an advantage was found to be achieved regardless of selection of an element from Nb, Ta, V, and Zr.
  • production steps for a standard grain oriented electrical steel sheet can be used. Specifically, a series of steps can be used in which slabs produced from a molten steel adjusted to have a predetermined component composition are hot-rolled; the resultant hot-rolled sheets are optionally subjected to hot-rolled sheet annealing and then subjected to a single cold-rolling step or two or more cold-rolling steps that include an intermediate annealing therebetween so as to have a final sheet thickness; the steel sheets are subsequently subjected to recrystallization annealing, then to purification annealing, and optionally to flattening annealing; and the steel sheets are then coated.
  • the amount of C added in molten steel is preferably made 0.10% or less.
  • the Si content may be adjusted to be 1.0% to 8.0%, which is the finally required content, in the adjustment of the component composition of molten steel.
  • the amount of Si added to molten steel may be less than the finally required content.
  • Nb, Ta, V, and Zr which are essential components in the present invention, during steps after the molten steel state. Accordingly, it is most desirable that a required amount of such a component be added in the adjustment of the component composition of molten steel.
  • slabs may be produced by a standard ingot making process or a standard continuous casting process, or otherwise thin cast slabs having a thickness of 100 mm or less may be produced by direct casting process.
  • slabs are heated and hot-rolled in a standard manner, slabs after being cast may be instead directly hot-rolled without being heated. In the case of thin cast slabs, it may be hot-rolled or jumped straight to next steps without being hot-rolled.
  • the heating temperature of slabs to be hot-rolled in a component system containing an inhibitor-forming element is normally a high temperature of about 1,400C. In contrast, the heating temperature in a component system without inhibitor-forming elements is normally a low temperature of 1,250°C or less, which is advantageous in terms of cost.
  • the temperature of the hot-rolled sheet annealing is preferably 800°C or more and 1,150°C or less. This is because, when the temperature of the hot-rolled sheet annealing is less than 800°C, a band texture due to hot rolling remains and it becomes difficult to achieve a primary recrystallization texture having uniformly-sized grains; accordingly, the hot-rolled sheet annealing provides a relatively limited effect of promoting development of secondary recrystallized grains.
  • the temperature of the hot-rolled sheet annealing is more than 1,150°C, crystal grains after the hot-rolled sheet annealing become coarse. Accordingly, also in this case, it becomes difficult to achieve a primary recrystallization texture having uniformly-sized grains.
  • one or more cold-rolling steps optionally including a process an intermediate annealing therebetween are performed and recrystallization annealing is then performed.
  • it is effective to perform cold rolling in a temperature range of 100°C to 300°C and/or to perform one or more aging treatments in a range of 100°C to 300°C during the cold rolling process.
  • recrystallization annealing when decaburization is necessary, a wet atmosphere is employed in the recrystallization annealing; however, when decaburization is not necessary, the recrystallization annealing may be performed in a dry atmosphere. After the recrystallization annealing, a technique of increasing Si content by siliconization may be further employed.
  • the sheets are coated with an annealing separator mainly containing MgO and then subjected to final annealing (purification annealing) to develop a secondary recrystallization texture and to form a forsterite coating.
  • an annealing separator is not applied; or, even when an annealing separator is applied, silica, alumina, or the like should be used instead of MgO forming a forsterite coating.
  • an annealing separator is applied, for example, electrostatic coating without involving water content is effectively performed.
  • a heat-resistant inorganic material sheet (silica, alumina, or mica) may be used.
  • the final annealing is sufficiently performed at a temperature allowing for secondary recrystallization, and desirably at 800°C or more.
  • An annealing condition under which secondary recrystallization is completed is desirable and it is generally desirable that the sheets be held at a temperature of 800°C or more for 20 or more hours.
  • the holding temperature is desirably about 850°C to 950°C and the final annealing may be finished with this holding treatment.
  • the temperature is advantageously increased to about 1,200°C.
  • the cooling is desirably performed at a rate of 5°C/hr to 100°C/hr at least in a temperature range of 900°C to 500°C.
  • the cooling is desirably performed at a rate of 5°C/hr to 100°C/hr in a temperature range of the holding temperature to 500°C. This is because, when the cooling rate is more than 100°C/hr in such a temperature range, there may be cases where precipitates become excessively fine or precipitation from a solid solution does not occur.
  • the lower limit of the cooling rate is more preferably 7.8°C/hr.
  • the upper limit of the cooling rate is more preferably 30°C/hr. In view of achieving results with stability, the upper limit of the cooling rate is still more preferably 14°C/hr.
  • a magnetic domain refining treatment is desirably performed.
  • An example of this treatment is, as generally performed, a method of forming grooves in final product sheets or linearly introducing thermal strain or impact strain with laser or plasma into final product sheets, or a method of forming grooves in intermediate products having a final sheet thickness such as cold-rolled sheets.
  • a preferred method for producing an iron core using steel sheets according to the present invention for example, there is provided the method including shearing steel sheets according to the present invention and laminating the sheets without subjecting them to stress relief annealing.
  • a steel sheet according to the present invention degradation of iron loss of the steel sheet due to the shearing can be suppressed to 0.1 W/kg or less (preferably, 0.041 W/kg or less).
  • the production method is particularly advantageous for producing large iron cores, for example, in the cases where a steel sheet is sheared into sheets having a longest side more than 500 mm. Matters including the number of steel sheets stacked, the size and shape of steel sheets obtained by the shearing, the presence or absence of the grooves, the size of the grooves, the presence or absence of coating, and the type of coating may be appropriately determined on the basis of ordinary knowledge.
  • the steel slabs were subjected to slab reheating at 1,400°C and then hot-rolled to sheets so as to have a thickness of 2.4 mm.
  • the sheets were then subjected to hot-rolled sheet annealing at 1,000°C for 40 seconds, subsequently to cold rolling so as to have a thickness of 1.6 mm, to intermediate annealing at 900°C, and then to cold rolling to sheets so as to have a thickness of 0.23 mm.
  • the resultant sheets were then subjected to recrystallization annealing in a 60%N 2 -40%H 2 wet atmosphere under soaking conditions at 850°C for 90 seconds, subsequently coated with an annealing separator mainly containing MgO, and subjected to purification annealing at 1,220°C for 6 hours.
  • the cooling rate for a range of 900°C to 500°C was controlled as described in Table 1 to thereby vary the diameter of Nb precipitates and Nb precipitation percentage.
  • the sheets were subjected to flattening annealing at 850°C for 20 seconds.
  • the obtained samples were cut so as to have a size of 30 mm x 280 mm. At this time, the cutting was performed under two conditions: cutting with a wire cutter and cutting with a shearing machine. Magnetic characteristics of obtained samples were measured by the method described in JIS C 2550 and the magnetic characteristics of the samples obtained by the cutting with the wire cutter are described in Table 1.
  • ⁇ W determined by subtracting the iron loss of a sample obtained by cutting with the wire cutter from the iron loss of a sample obtained by cutting with the shearing machine is also described in Table 1.
  • the samples having been subjected to the magnetic were then subjected to pickling to remove coatings and the crystal grain size of secondary recrystallized grains was measured. The results are also described in Table 1 together with the measurement results of the diameter and precipitation percentage of Nb precipitates.
  • the component composition of steel sheets of the coating-removed samples was measured. As a result, the component composition confirmed was 0.0016% of C, 3.24% of Si, 0.13% of Mn, and 18 ppm of Nb (for No. 7 steel only, 15 ppm of Nb), which satisfied requirements of the present invention.
  • Product sheets (sheet thickness: 0.23 mm) of grain oriented electrical steel sheets were provided that contained components described in Table 2 and that were produced by a standard production method in which recrystallization annealing was performed, followed by purification annealing at 1,150°C, and cooling at a cooling rate in the range of 900°C to 500°C of 25°C/hr.
  • the grain oriented electrical steel sheets were cut so as to have a size of 30 mm x 280 mm. At this time, the cutting was performed under two conditions: cutting with a wire cutter and cutting with a shearing machine.
  • the magnetic characteristics of the obtained samples were measured by the method described in JIS C 2550 and the magnetic characteristics of the samples obtained by the cutting with the wire cutter are described in Table 2.
  • ⁇ W determined as in EXAMPLE 1 is also described in Table 2.
  • the samples having been subjected to the magnetic measurement were subjected to pickling to remove coatings and the crystal grain size of secondary recrystallized grains was measured.
  • the results are also described in Table 2 together with the measurement results of the diameter and precipitation percentage of precipitates of Nb or the like.
  • the component compositions of steel sheets in Table 2 are results obtained by measuring the component compositions of coating-removed samples after the pickling.
  • the precipitates were measured. As a result, the precipitates had an average diameter of 0.05 to 3.34 ⁇ m and a precipitation percentage of 0% to 79%.
  • Steel slabs containing 0.065% of C, 3.25% of Si, 0.13% of Mn, 0.05% of Cr, 240 ppm of Al, 70 ppm of N, 36 ppm of S, 0.013% of P, 0.075% of Sn, 0.036% of Sb, 0.011% of Mo, and 25 ppm of Nb, and the balance being Fe and unavoidable impurities, were produced by continuous casting.
  • the steel slabs were subjected to slab reheating at 1,400°C and then hot--rolled to sheets so as to have a thickness of 2.4 mm.
  • the sheets were then subjected to hot-rolled sheet annealing at 1,000°C for 40 seconds, subsequently to cold rolling so as to have a thickness of 1.6 mm, to intermediate annealing in a temperature range of 700°C to 1,020°C, and then to cold rolling to provide steel sheets having a thickness of 0.23 mm.
  • Linear grooves having a width of 100 ⁇ m and a depth of 25 ⁇ m were then formed by local electrolytic etching in the surfaces of the steel sheets so as to extend at an angle of 10° with respect to a direction perpendicular to the rolling direction at a pitch of 8 mm.
  • the sheets were then subjected to recrystallization annealing in a 60%N 2 -40%H 2 wet atmosphere under soaking conditions at 800°C to 900°C for 90 seconds.
  • the sheets were then coated with an annealing separator mainly containing MgO and subsequently subjected to purification annealing at 1,220°C for 6 hours. After that, the sheets were cooled such that they were cooled from 900°C to 500°C at a cooling rate of 10°C/hr.
  • the sheets were then subjected to flattening annealing at 850°C for 20 seconds.
  • the temperatures of the intermediate annealing and the temperatures of the recrystallization annealing were varied to vary the grain size after secondary recrystallization.
  • the obtained samples were cut into Epstein specimens having a size of 30 mm x 280 mm. At this time, the cutting was performed under two conditions: cutting with a wire cutter and cutting with a shearing machine.
  • the samples having been subjected to the magnetic measurement were subjected to pickling to remove coatings and the crystal grain size of secondary recrystallized grains was measured.
  • the results are also described in Table 3 together with the measurement results of the diameter and precipitation percentage of Nb precipitates.
  • the component composition of steel sheets of the coating-removed samples was measured.
  • the component composition confirmed was 0.0016% of C, 3.24% of Si, 0.13% of Mn, 0.05% of Cr, 0.011% of P, 0.074% of Sn, 0.036% of Sb, 0.011% of Mo, and 18 ppm of Nb, which satisfied requirements of the present invention.
  • the diameter (average diameter) of the precipitates is 0.12 ⁇ m or more and 1.2 ⁇ m or less (preferably 0.78 ⁇ m or less; the precipitation percentage is preferably 48% or more) and ⁇ W is 0.038 W/kg or less.
  • the cooling rate after final annealing is preferably made 7.8°C/hr to 30°C/hr, more preferably 7.8°C/hr to 14°C/hr.

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EP3309271A4 (de) * 2015-06-09 2018-07-04 JFE Steel Corporation Orientiertes elektromagnetisches stahlblech und verfahren zur herstellung davon

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WO2014132354A1 (ja) * 2013-02-27 2014-09-04 Ｊｆｅスチール株式会社 方向性電磁鋼板の製造方法
CN105008557B (zh) * 2013-02-28 2017-10-24 杰富意钢铁株式会社 取向性电磁钢板的制造方法
CN107109552B (zh) * 2014-10-06 2018-12-28 杰富意钢铁株式会社 低铁损取向性电磁钢板及其制造方法
KR101719231B1 (ko) 2014-12-24 2017-04-04 주식회사 포스코 방향성 전기강판 및 그 제조방법
KR102062182B1 (ko) 2015-02-13 2020-01-03 제이에프이 스틸 가부시키가이샤 방향성 전자 강판 및 그의 제조 방법
JP6424875B2 (ja) * 2015-12-14 2018-11-21 Ｊｆｅスチール株式会社 方向性電磁鋼板およびその製造方法
CN111566232B (zh) 2018-01-31 2022-03-08 日本制铁株式会社 方向性电磁钢板
KR102249920B1 (ko) * 2018-09-27 2021-05-07 주식회사 포스코 방향성 전기강판 및 그의 제조방법

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RU2496905C1 (ru) 2013-10-27
US20120131982A1 (en) 2012-05-31
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RU2012107393A (ru) 2013-09-10
EP2460902B1 (de) 2016-05-04
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JP4735766B2 (ja) 2011-07-27
KR20130126751A (ko) 2013-11-20

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