EP2537947A1 - Herstellungsverfahren für ein kornorientiertes elektromagnetisches stahlblech - Google Patents

Herstellungsverfahren für ein kornorientiertes elektromagnetisches stahlblech Download PDF

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EP2537947A1
EP2537947A1 EP11744742A EP11744742A EP2537947A1 EP 2537947 A1 EP2537947 A1 EP 2537947A1 EP 11744742 A EP11744742 A EP 11744742A EP 11744742 A EP11744742 A EP 11744742A EP 2537947 A1 EP2537947 A1 EP 2537947A1
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mass
steel sheet
content
grain
oriented electrical
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French (fr)
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EP2537947B1 (de
EP2537947A4 (de
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Kenichi Murakami
Yoshiyuki Ushigami
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Nippon Steel Corp
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Nippon Steel Corp
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    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • 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
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D3/00—Diffusion processes for extraction of non-metals; Furnaces therefor
    • C21D3/02—Extraction of non-metals
    • C21D3/04—Decarburising
    • 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
    • C21D8/1255—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest with diffusion of elements, e.g. decarburising, nitriding
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1244—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest
    • C21D8/1272—Final recrystallisation annealing
    • C—CHEMISTRY; METALLURGY
    • 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
    • C22C38/04—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
    • C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
    • C—CHEMISTRY; METALLURGY
    • 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
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/02—Pretreatment of the material to be coated
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/80—After-treatment
    • 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

Definitions

  • the present invention relates to a method of manufacturing a grain-oriented electrical steel sheet in which the variation in magnetic property is suppressed.
  • a grain-oriented electrical steel sheet is a steel sheet which contains Si and in which crystal grains are highly integrated in a ⁇ 110 ⁇ 001> orientation, and is used as a material of a wound core of a stationary induction apparatus such as a transformer.
  • the control of the orientation of the crystal grains is conducted with catastrophic grain growth phenomenon called secondary recrystallization.
  • heating is performed on a slab at a temperature of 1280°C or higher to almost completely solid-solve fine precipitates called inhibitors, and thereafter hot rolling, cold rolling, annealing and so on are performed to cause the fine precipitates to precipitate during the hot rolling and the annealing.
  • heating is performed on a slab at a temperature of lower than 1280°C, and thereafter hot rolling, cold rolling, decarburization annealing, nitridation, finish annealing and so on are performed to cause AlN (Al, Si)N and the like to precipitate as inhibitors during the nitridation.
  • An object of the present invention is to provide a method of manufacturing a grain-oriented electrical steel sheet, capable of suppressing the variation in magnetic property.
  • the above-described variation in magnetic properties after the finish annealing is remarkable when the C content is 0.06 mass% or less, and further, it is particularly noticeable when the C content is 0.048 mass% or less.
  • the cause of the variation in magnetic property after the finish annealing is not exactly known, the variation is considered to occur because the crystal grains sometimes do not uniformly grow during the finish annealing even if the crystal grains seem to be uniform before the finish annealing.
  • the reason why the crystal grains do not uniformly grow is because, due to the low C content, a phase transformation during the hot rolling is not sufficiently performed, so that an amount of austenite transformation is small, resulting in that a hot-rolled texture becomes unstable.
  • a sufficient secondary recrystallization does not occur in a portion in which the hot-rolled texture becomes nonuniform, resulting in that sufficient magnetic properties are not obtained.
  • the present inventors thought, based on such knowledge, that it is possible to sufficiently cause the secondary recrystallization throuth forming an effective precipitate in order to make the crystal grain growth uniform during the finish annealing. Then, the present inventors repeatedly carried out an experiment of measuring the magnetic properties of the grain-oriented electrical steel sheets obtained through adding various kinds of elements to slabs. As a result, the present inventors found that addition of Ti and Cu was effective to make the secondary recrystallization uniform.
  • the present invention has been made based on the above-described knowledge, and a summary thereof is as follows.
  • a method of manufacturing a grain-oriented electrical steel sheet comprising:
  • the present inventors repeatedly conducted the experiments of measuring the magnetic properties of the grain-oriented electrical steel sheets obtained through adding various kinds of elements to slabs and found out that addition of Ti and Cu is effective to make the secondary recrystallization uniform.
  • silicon steel with a composition used for manufacturing a grain-oriented electrical steel sheet based on a low-temperature slab heating method in which a C content was 0.06 mass% or less was used, for example.
  • Ti and Cu were contained at various ratios into the carbon steel to produce steel ingots with various compositions.
  • the steel ingots were heated at a temperature of 1250°C or lower and subjected to hot rolling, and then subjected to cold rolling. Further, decarburization annealing was performed after the cold rolling, and thereafter, nitridation treatment and finish annealing were performed.
  • the magnetic flux density B8 is the magnetic flux density occurring in the grain-oriented electrical steel sheet when a magnetic field of 800 A/m at 50 Hz is applied thereto.
  • Fig. 1 An example of the results obtained through the above-described experiments is illustrated in Fig. 1 .
  • an open circle mark in Fig. 1 indicates that the average value of the magnetic flux densities B8 of five single-plate samples was 1.90 T or more and the difference between the maximum value and the minimum value of the magnetic flux density B8 was 0.030 T or less.
  • a filled circle mark in Fig. 1 indicates that at least the average value of the magnetic flux densities B8 of the five single-plate samples was less than 1.90 T or the difference between the maximum value and the minimum value of the magnetic flux densities B8 was more than 0.030 T. It is apparent from Fig.
  • FIG. 2 is a flowchart illustrating the method of manufacturing a grain-oriented electrical steel sheet according to the embodiment of the present invention.
  • a slab is produced through casting of molten steel for a grain-oriented electrical steel sheet with a predetermined composition (Step 1).
  • the casting method therefor is not particularly limited.
  • the molten steel contains, for example, Si: 2.5 mass% to 4.0 mass%, C: 0.01 mass% to 0.060 mass%, Mn: 0.05 mass% to 0.20 mass%, acid-soluble Al: 0.020 mass% to 0.040 mass%, N: 0.002 mass% to 0.012 mass%, S: 0.001 mass% to 0.010 mass%, and P: 0.01 mass% to 0.08 mass%.
  • the molten steel further contains at least one kind selected from a group consisting of Ti: 0.0020 mass% to 0.010 mass% and Cu: 0.010 mass% to 0.50 mass%.
  • the molten steel contains one or both of Ti and Cu in ranges of Ti: 0.010 mass% or less and Cu: 0.50 mass% or less to satisfy at least one of Ti: 0.0020 mass% or more or Cu: 0.010 mass% or more.
  • the balance of the molten steel may be composed of Fe and inevitable impurities. Note that the inevitable impurities may include an element(s) forming an inhibitor in the manufacturing process of the grain-oriented electrical steel sheet and remaining in the grain-oriented electrical steel sheet after purification is performed through a high-temperature annealing.
  • Si is an element that is extremely effective to enhance the electrical resistance of the grain-oriented electrical steel sheet to reduce the eddy current loss constituting a part of the core loss.
  • the Si content is less than 2.5 mass%, the eddy current loss cannot be sufficiently suppressed.
  • the Si content is more than 4.0 mass%, the processability is lowered. Accordingly, the Si content is set to 2.5 mass% to 4.0 mass%.
  • C is an element that is effective to control the structure (primary recrystallization structure) obtained through primary recrystallization.
  • the C content is less than 0.01 mass%, the effect cannot be sufficiently obtained.
  • the C content is more than 0.06 mass, the time required for decarburization annealing increases, resulting in a larger exhaust amount of CO 2 .
  • the C content is set to 0.01 mass% to 0.06 mass%.
  • the embodiment is particularly effective in the case where the C content is 0.048 mass% or less.
  • Mn increases the specific resistance of the grain-oriented electrical steel sheet to reduce the core loss. Mn also functions to prevent occurrence of cracks in the hot rolling. When the Mn content is less than 0.05 mass%, the effects cannot be sufficiently obtained. On the other hand, when the Mn content is more than 0.20 mass%, the magnetic flux density of the grain-oriented electrical steel sheet is lowered. Accordingly, the Mn content is set to 0.05 mass% to 0.20 mass%.
  • Acid-soluble Al is an important element forming AlN serving as an inhibitor.
  • the acid-soluble Al content is less than 0.020 mass%, a sufficient amount of AlN cannot be formed, resulting in insufficient inhibitor strength.
  • the acid-soluble Al content is more than 0.040 mass%, AlN becomes coarse, resulting in a decrease in inhibitor strength. Accordingly, the acid-soluble Al content is set to 0.020 mass% to 0.040 mass%.
  • N is an important element forming AlN through reacting with the acid-soluble Al. Though a large amount of N does not need to be contained in the grain-oriented electrical steel sheet because nitridation treatment is performed after the cold rolling as will be described later, a great load may be required in steelmaking in order to make the N content less than 0.002 mass%. On the other hand, when the N content is more than 0.012 mass%, a hole called blister is generated in the steel sheet in the cold rolling. Accordingly, the N content is set to 0.002 mass% to 0.012 mass%. The N content is preferably 0.010% mass% or less in order to further reduce the blister.
  • MnS precipitate is an important element forming a MnS precipitate through reacting with Mn.
  • the MnS precipitate mainly affects the primary recrystallization and functions to suppress the variation depending on site in grain growth in the primary recrystallization due to the hot rolling.
  • the Mn content is set to 0.001 mass% to 0.010 mass%.
  • the Mn content is preferably 0.009 mass% or less in order to further improve the magnetic property.
  • P increases the specific resistance of the grain-oriented electrical steel sheet to reduce the core loss.
  • the P content is less than 0.01 mass%, the effect cannot be sufficiently obtained.
  • the P content is more than 0.08 mass%, the cold rolling may become difficult to perform. Accordingly, the P content is set to 0.01 mass% to 0.08 mass%.
  • Ti forms a TiN precipitate through reacting with N.
  • Cu forms a CuS precipitate through reacting with S.
  • These precipitates function to make the growth of the crystal grains in the finish annealing uniform irrespective of the site of the coil and suppress the variation in magnetic property of the grain-oriented electrical steel sheet.
  • the TiN precipitate is considered to suppress the variation in grain growth in a high temperature region in the finish annealing to decrease the deviation of the magnetic property of the grain-oriented electrical steel sheet.
  • the CuS precipitate is considered to suppress the variation in grain growth in a low temperature region in the decarburization annealing and the finish annealing to decrease the deviation of the magnetic property of the grain-oriented electrical steel sheet.
  • the Ti content is less than 0.0020 mass% and the Cu content is less than 0.010 mass%, the effects cannot be sufficiently obtained.
  • the Ti content is more than 0.010 mass%, the TiN precipitate is excessively formed and remains even after the finish annealing.
  • the Cu content is more than 0.50 mass%, the CuS precipitate is excessively formed and remains even after the finish annealing. If these precipitates remain in the grain-oriented electrical steel sheet, it is difficult to obtain a high magnetic property.
  • the molten steel contains one or both of Ti and Cu in ranges of Ti: 0.010 mass% or less and Cu: 0.50 mass% or less to satisfy at least one of Ti: 0.0020 mass% or more or Cu: 0.010 mass% or more.
  • the molten steel contains at least one kind selected from a group consisting of Ti: 0.0020 mass% to 0.010 mass% and Cu: 0.010 mass% to 0.50 mass%.
  • the lower limit of the Ti content is preferably 0.0020 mass%, and the upper limit of the Ti content is preferably 0.0080 mass%.
  • the lower limit of the Cu content is preferably 0.01 mass%, and the upper limit of the Cu content is preferably 0.10 mass%.
  • the Ti content (mass%) is expressed as [Ti] and the Cu content (mass%) is expressed as [Cu]
  • it is more preferable that the relation of "20 ⁇ [Ti]+[Cu] ⁇ 0.18" is established and, preferably, the relation of "10 ⁇ [Ti]+[Cu] ⁇ 0.07" is established.
  • each of the Cr content and the Sn content is preferably 0.20 mass% or less. Further, in order to sufficiently obtain the above effects, each of the Cr content and the Sn content is preferably 0.01 mass% or more. Note that Sn is a grain boundary segregation element and thus also has an effect to stabilize secondary recrystallization.
  • the molten steel may contain Sb: 0.010 mass% to 0.20 mass%, Ni: 0.010 mass% to 0.20 mass%, Se: 0.005 mass% to 0.02 mass%, Bi: 0.005 mass% to 0.02 mass%, Pb: 0.005 mass% to 0.02 mass%, B: 0.005 mass% to 0.02 mass%, V: 0.005 mass% to 0.02 mass%, Mo: 0.005 mass% to 0.02 mass%, and/or As : 0.005 mass% to 0.02 mass%.
  • These elements may be inhibitor strengthening elements.
  • the slab is heated (Step S2).
  • the temperature of the heating is preferably set to 1250°C or lower from the viewpoint of energy saving.
  • the thickness of the hot-rolled steel sheet is not particularly limited, and may be set to 1.8 mm to 3.5 mm.
  • annealing is performed on the hot-rolled steel sheet to obtain an annealed steel sheet (Step S4).
  • the condition of the annealing is not particularly limited, and the annealing may be performed, for example, at a temperature of 750°C to 1200°C for 30 seconds to 10 minutes. The annealing improves the magnetic property.
  • Step S5 cold rolling is performed on the annealed steel sheet to obtain a cold-rolled steel sheet.
  • the cold rolling may be performed only once or a plurality of times while an intermediate annealing is performed therebetween.
  • the intermediate annealing is preferably performed at a temperature of 750°C to 1200°C for 30 seconds to 10 minutes.
  • the cold rolling is performed without performing the above-described intermediate annealing, it may be difficult to obtain uniform properties.
  • the cold rolling is performed a plurality of times while the intermediate annealing is performed therebetween, the uniform properties are easily obtained but the magnetic flux density may decrease. Accordingly, it is preferable to determine the number of times of the cold rolling and the presence or absence of the intermediate annealing according to the property required for and the cost of the finally obtained grain-oriented electrical steel sheet.
  • the rolling reduction at the final cold rolling it is preferable to set the rolling reduction at the final cold rolling to 80% to 95%.
  • the decarburization annealing is performed on the cold-rolled steel sheet in a wet atmosphere containing hydrogen and nitrogen at 800°C to 950°C after the cold rolling to obtain a decarburization annealed steel sheet (step S6).
  • the decarburization annealing removes carbon in the steel sheet and causes primary recrystallization.
  • the temperature of the decarburization annealing is lower than 800°C, the crystal grain obtained through the primary recrystallization (primary recrystallization grain) is small so that the subsequent secondary recrystallization does not sufficiently appear.
  • the temperature of the decarburization annealing is higher than 950°C, the primary recrystallization grain is large so that the subsequent secondary recrystallization does not sufficiently appear.
  • nitridation treatment is performed on the decarburization annealed steel sheet in an atmosphere containing hydrogen, nitrogen and a gas having a nitriding capability such as ammonia at 700°C to 850°C to obtain a nitrided steel sheet (step S7).
  • the nitridation treatment increases the nitrogen content in the steel sheet.
  • the temperature of the nitridation treatment is lower than 700°C or high than 850°C, nitrogen is difficult to be diffused to the inner part of the steel sheet so that the subsequent secondary recrystallization does not sufficiently appear.
  • an annealing separating agent containing MgO as a main component is applied, in a water slurry, to the surface of the nitrided steel sheet, and the nitrided steel sheet is coiled.
  • batch-type finish annealing is performed on the coiled nitrided steel sheet to obtain a coiled finish-annealed steel sheet (Step S8).
  • the finish annealing causes secondary recrystallization.
  • step S9 a coating solution containing aluminum phosphate and colloidal silica as main components is applied to the surface of the finish-annealed steel sheet, and baking is performed thereon to form an insulating film.
  • the grain-oriented electrical steel sheet can be manufactured.
  • the steel being an object for the hot rolling is not limited to the slab obtained through casting of the molten steel, but a so-called thin slab may be used. Further, when using the thin slab, it is not always necessary to perform the slab heating at 1250°C or lower.
  • annealing was performed on the hot-rolled steel sheets at 1100°C for 120 seconds to obtain annealed steel sheets.
  • acid pickling was performed on the annealed steel sheets, and then cold rolling was performed on the annealed steel sheets to obtain cold-rolled steel sheets with a thickness of 0.23 mm.
  • decarburization annealing was performed on the cold-rolled steel sheets in an atmosphere containing water vapor, hydrogen, and nitrogen at 860°C for 100 seconds to obtain decarburization annealed steel sheets.
  • nitridation treatment was performed on the decarburization annealed steel sheets in an atmosphere containing hydrogen, nitrogen, and ammonia at 770°C for 20 seconds to obtain nitrided steel sheets.
  • an annealing separating agent containing MgO as a main component was applied, in a water slurry, to the surfaces of the decarburized nitrided steel sheets. Then, finish annealing was performed on them at 1200°C for 20 hours to obtain finish-annealed steel sheets. Subsequently, the finish-annealed steel sheets were washed with water, and then cutout into a single-plate magnetic measurement size with a width of 60 mm and a length of 300 mm. Subsequently, a coating solution containing aluminum phosphate and colloidal silica as main components was applied to the surfaces of the finish-annealed steel sheets, and baking was performed thereon to form an insulating film. In this manner, samples of the grain-oriented electrical steel sheets were obtained.
  • the magnetic flux density B8 of each of the grain-oriented electrical steel sheets was measured.
  • the magnetic flux density B8 is the magnetic flux density occurring in the grain-oriented electrical steel sheet when a magnetic field of 800 A/m at 50 Hz is applied thereto as described above.
  • the magnetic flux densities B8 of five single-plate samples for measurement were measured for each of the samples.
  • the average value "average B8,” the maximum value “B8max,” and the minimum value “B8min” were obtained.
  • the difference “ ⁇ B8” between the maximum value "B8max” and the minimum value “B8min” was also obtained.
  • the difference " ⁇ B8” is an index indicating the fluctuation range of the magnetic property.
  • Fig. 1 the evaluation results based on the average value "average B8" and the difference " ⁇ B8” are indicated in Fig. 1 .
  • an open circle mark in Fig. 1 indicates that the average value "average B8” was 1.90 T or more and the difference " ⁇ B8" was 0.030 T or less.
  • a filled circle mark in Fig. 1 indicates that the average value "average B8" was less than 1.90 T or the difference " ⁇ B8" was more than 0.030 T.
  • the balance between the average value "average B8" and the difference " ⁇ B8” was excellent in the samples No. 11, No. 13, and No. 15, in which the relation of "20 ⁇ [Ti]+[Cu] ⁇ 0.18" was established where the Ti content (mass%) was expressed as [Ti] and the Cu content (mass%) was expressed as [Cu].
  • the balance between the average value "average B8" and the difference " ⁇ B8” was extremely excellent in the sample No. 15, in which the relation of "10 ⁇ [Ti]+[Cu] ⁇ 0.07" was established.
  • the difference " ⁇ B8" was large to be more than 0.030 T.
  • the variation in magnetic property was large.
  • the sample No. 5 in which the Ti content was more than 0.010 mass% and the sample No. 10, in which the Cu content was more than 0.50 mass%, a large amount of precipitate was contained to affect the finish annealing, with the result that the average value "average B8" was small to be less than 1.90 T. In short, a sufficiently high magnetic property could not be obtained.
  • annealing was performed on the hot-rolled steel sheet at 1090°C for 120 seconds to obtain an annealed steel sheet. Then, acid pickling was performed on the annealed steel sheet, and then cold rolling was performed on the annealed steel sheet to obtain a cold-rolled steel sheet with a thickness of 0.23 mm. Subsequently, eight pieces of steel sheets for annealing were cutout from the cold-rolled steel sheet, and decarburization annealing was performed on each of the steel sheets in an atmosphere containing water vapor, hydrogen, and nitrogen at a temperature T1 ranging from 790°C to 960°C listed in Table 2 for 80 seconds to obtain decarburization annealed steel sheets.
  • nitridation treatment was performed on each of the decarburization annealed steel sheets in an atmosphere containing water vapor, hydrogen, nitrogen, and ammonia at a temperature T2 ranging from 680°C to 880°C listed in Table 2 for 20 seconds to obtain nitrided steel sheets.
  • an annealing separating agent containing MgO as a main component was applied, in a water slurry, to the surfaces of the nitrided steel sheets. Then, finish annealing was performed on them at 1200°C for 20 hours to obtain finish annealed steel sheets. Subsequently, treatments from the water washing to the formation of the insulating film were performed similarly to the first experiment to obtain samples of the grain-oriented electrical steel sheets.
  • the average value "average B8" was large to be 1.90 T or more, and the difference " ⁇ B8" was small to be 0.030 T or less. In short, a high magnetic property was obtained and the variation in the magnetic property was small.
  • annealing was performed on the hot-rolled steel sheets at 1090°C for 120 seconds to obtain annealed steel sheets. Then, acid pickling was performed on the annealed steel sheets, and then, cold rolling was performed on the annealed steel sheets to obtain cold-rolled steel sheets with a thickness of 0.23 mm. Subsequently, steel sheets for annealing were cutout from the cold-rolled steel sheets, and decarburization annealing was performed on the steel sheets in an atmosphere containing water vapor, hydrogen, and nitrogen at 860°C for 80 seconds to obtain decarburization annealed steel sheets. Next, nitridation treatment was performed on the decarburization annealed steel sheets in an atmosphere containing water vapor, hydrogen, nitrogen, and ammonia at 760°C for 20 seconds to obtain nitrided steel sheets.
  • an annealing separating agent containing MgO as a main component was applied, in a water slurry, to the surfaces of the nitrided steel sheets. Then, finish annealing was performed on them at 1200°C for 20 hours to obtain finish annealed steel sheets. Subsequently, treatments from the water washing to the formation of insulating film were performed similarly to the first experiment to obtain samples of the grain-oriented electrical steel sheets.
  • the average value "average B8" was large to be 1.90 T or more, and the difference " ⁇ B8" was small to be 0.025 T or less. In short, a high magnetic property was obtained and the variation in magnetic property was small. Particularly, when the C content was small, a good result was obtained.
  • the balance between the average value "average B8" and the difference " ⁇ B8” was excellent in the samples No. 32, No. 33, No. 37, No. 38, No. 42, No. 43, No. 47, and No. 48, in each of which the Ti content was 0.0020 mass to 0.080 mass%, the Cu content was 0.010 mass to 0.10 mass%, and the relation of "20 ⁇ [Ti]+[Cu] ⁇ 0.18" was established.
  • the balance between the average value "average B8" and the difference " ⁇ B8” was extremely excellent in the samples No. 32, No. 37, No. 42, and No. 47, in each of which the relation of "10 ⁇ [Ti]+[Cu] ⁇ 0.07" was established.
  • annealing was performed on the hot-rolled steel sheets at 1080°C for 120 seconds to obtain annealed steel sheets. Then, acid pickling was performed on the annealed steel sheets, and then cold rolling was performed on the annealed steel sheets to obtain cold-rolled steel sheets with a thickness of 0.23 mm. Subsequently, decarburization annealing was performed on the cold-rolled steel sheets in an atmosphere containing water vapor, hydrogen, and nitrogen at 870°C for 90 seconds to obtain decarburization annealed steel sheets. Next, nitridation treatment was performed on the decarburization annealed steel sheets in an atmosphere containing hydrogen, nitrogen, and ammonia at 760°C for 20 seconds to obtain nitrided steel sheets.
  • an annealing separating agent containing MgO as a main component was applied, in a water slurry, to the surfaces of the nitrided steel sheets. Then, finish annealing was performed on them at 1200°C for 20 hours to obtain finish annealed steel sheets. Subsequently, treatments from the water washing to the formation of the insulating film were performed similarly to the first experiment to obtain samples of the grain-oriented electrical steel sheets.
  • the average value *average B8* was large ot be 1.90 T or more and the difference " ⁇ B8" was small to be 0.030 T or less.
  • a high magnetic property was obtained and the variation in the magnetic property was small.
  • the average value "average B8" was particularly large to be 1.91 T or more, and the difference " ⁇ B8" was particularly small to be 0.025 T or less.
  • the present invention is applicable, for example, in electrical steel sheet manufacturing industries and electrical steel sheet using industries.

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Families Citing this family (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103741031B (zh) * 2013-12-27 2016-01-20 钢铁研究总院 薄板坯连铸连轧含钒普通取向硅钢及其制造方法
EP3196320B1 (de) 2014-09-04 2019-08-21 JFE Steel Corporation Verfahren zur herstellung eines direktionalen magnetischen stahlblechs und anlage zur nitrierbehandlung
BR112018005469B1 (pt) * 2015-09-28 2021-08-31 Nippon Steel Corporation Chapa de aço elétrico com grão orientado, chapa de aço laminada a quente para chapa de aço elétrico com grão orientado e seus métodos de produção
KR101676630B1 (ko) * 2015-11-10 2016-11-16 주식회사 포스코 방향성 전기강판 및 그 제조방법
BR112020000223A2 (pt) * 2017-07-13 2020-07-07 Nippon Steel Corporation folha de aço eletromagnética orientada
US20200123632A1 (en) * 2017-07-13 2020-04-23 Nippon Steel Corporation Grain-oriented electrical steel sheet
JP6946847B2 (ja) * 2017-08-17 2021-10-13 日本製鉄株式会社 方向性電磁鋼板の製造方法
JP6946846B2 (ja) * 2017-08-17 2021-10-13 日本製鉄株式会社 方向性電磁鋼板の製造方法
KR102099866B1 (ko) * 2017-12-26 2020-04-10 주식회사 포스코 방향성 전기강판 및 그의 제조방법

Family Cites Families (29)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3276923A (en) * 1961-04-17 1966-10-04 Gen Electric Reduction in magnetic losses in electrical induction apparatus
GB1261945A (en) * 1968-04-24 1972-01-26 Kobe Steel Ltd A method for producing a mono-directional silicon steel sheet
US4202711A (en) * 1978-10-18 1980-05-13 Armco, Incl. Process for producing oriented silicon iron from strand cast slabs
JPS5956522A (ja) * 1982-09-24 1984-04-02 Nippon Steel Corp 鉄損の良い一方向性電磁鋼板の製造方法
JPS6240315A (ja) * 1985-08-15 1987-02-21 Nippon Steel Corp 磁束密度の高い一方向性珪素鋼板の製造方法
EP0326912B1 (de) * 1988-02-03 1994-07-27 Nippon Steel Corporation Verfahren zum Herstellen kornorientierter Elektrostahlbleche mit hoher Flussdichte
JPH0686632B2 (ja) * 1988-02-03 1994-11-02 新日本製鐵株式会社 磁束密度の高い一方向性珪素鋼板の製造方法
US5759293A (en) * 1989-01-07 1998-06-02 Nippon Steel Corporation Decarburization-annealed steel strip as an intermediate material for grain-oriented electrical steel strip
JPH02200733A (ja) * 1989-01-31 1990-08-09 Nippon Steel Corp 高磁束密度方向性電磁鋼板の製造方法
US5186762A (en) * 1989-03-30 1993-02-16 Nippon Steel Corporation Process for producing grain-oriented electrical steel sheet having high magnetic flux density
JPH0774388B2 (ja) * 1989-09-28 1995-08-09 新日本製鐵株式会社 磁束密度の高い一方向性珪素鋼板の製造方法
JPH03122227A (ja) 1989-10-05 1991-05-24 Nippon Steel Corp 方向性電磁鋼板の脱炭連続焼鈍炉
JPH07122096B2 (ja) * 1990-11-07 1995-12-25 新日本製鐵株式会社 磁気特性、皮膜特性ともに優れた一方向性電磁鋼板の製造方法
JP2620438B2 (ja) * 1991-10-28 1997-06-11 新日本製鐵株式会社 磁束密度の高い一方向性電磁鋼板の製造方法
US5288736A (en) * 1992-11-12 1994-02-22 Armco Inc. Method for producing regular grain oriented electrical steel using a single stage cold reduction
JP3065853B2 (ja) * 1992-12-08 2000-07-17 新日本製鐵株式会社 磁気特性の優れた一方向性電磁鋼板の安定製造方法
JPH06256847A (ja) 1993-03-03 1994-09-13 Nippon Steel Corp 磁気特性の優れた一方向性電磁鋼板の製造方法
JP2951852B2 (ja) * 1994-09-30 1999-09-20 川崎製鉄株式会社 磁気特性に優れる一方向性珪素鋼板の製造方法
JP3056970B2 (ja) * 1995-04-07 2000-06-26 新日本製鐵株式会社 磁気特性が優れた一方向性電磁鋼板の製造方法
IT1290977B1 (it) 1997-03-14 1998-12-14 Acciai Speciali Terni Spa Procedimento per il controllo dell'inibizione nella produzione di lamierino magnetico a grano orientato
JP3481491B2 (ja) 1998-03-30 2003-12-22 新日本製鐵株式会社 磁気特性に優れた一方向性電磁鋼板の製造方法
JP4261633B2 (ja) 1998-05-11 2009-04-30 新日本製鐵株式会社 一方向性電磁鋼板の製造方法
EP1162280B1 (de) * 2000-06-05 2013-08-07 Nippon Steel & Sumitomo Metal Corporation Verfahren zur Herstellung eines kornorientierten Elektrobleches mit ausgezeichneten magnetischen Eigenschaften
JP4272557B2 (ja) * 2004-02-12 2009-06-03 新日本製鐵株式会社 磁気特性に優れた一方向性電磁鋼板の製造方法
WO2006132095A1 (ja) * 2005-06-10 2006-12-14 Nippon Steel Corporation 磁気特性が極めて優れた方向性電磁鋼板及びその製造方法
JP4598702B2 (ja) 2006-03-23 2010-12-15 新日本製鐵株式会社 磁気特性が優れた高Ｓｉ含有方向性電磁鋼板の製造方法
JP4916847B2 (ja) * 2006-11-21 2012-04-18 新日本製鐵株式会社 一方向性電磁鋼板の製造方法
JP5428188B2 (ja) * 2008-04-15 2014-02-26 新日鐵住金株式会社 方向性電磁鋼板の製造方法
CN101775547B (zh) * 2009-12-31 2012-11-21 武汉钢铁(集团)公司 高磁感取向硅钢带的生产方法

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO2011102456A1 *

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BR112012020741A2 (pt) 2016-08-23
US20120312423A1 (en) 2012-12-13
KR20120118504A (ko) 2012-10-26
CN102762752B (zh) 2016-04-13
KR101389248B1 (ko) 2014-04-24
WO2011102456A1 (ja) 2011-08-25
KR20130119516A (ko) 2013-10-31
EP2537947B1 (de) 2018-12-19
JPWO2011102456A1 (ja) 2013-06-17
BR112012020741B1 (pt) 2022-07-19
EP2537947A4 (de) 2017-07-26
JP4943559B2 (ja) 2012-05-30
CN102762752A (zh) 2012-10-31

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