WO2011102456A1 - 方向性電磁鋼板の製造方法 - Google Patents

方向性電磁鋼板の製造方法 Download PDF

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WO2011102456A1
WO2011102456A1 PCT/JP2011/053491 JP2011053491W WO2011102456A1 WO 2011102456 A1 WO2011102456 A1 WO 2011102456A1 JP 2011053491 W JP2011053491 W JP 2011053491W WO 2011102456 A1 WO2011102456 A1 WO 2011102456A1
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mass
steel sheet
content
grain
oriented electrical
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PCT/JP2011/053491
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English (en)
French (fr)
Japanese (ja)
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村上　健一
義行 牛神
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新日本製鐵株式会社
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Priority to BR112012020741-5A priority Critical patent/BR112012020741B1/pt
Priority to US13/579,684 priority patent/US20120312423A1/en
Priority to PL11744742T priority patent/PL2537947T3/pl
Priority to JP2011523633A priority patent/JP4943559B2/ja
Priority to EP11744742.5A priority patent/EP2537947B1/en
Priority to KR1020137026864A priority patent/KR101389248B1/ko
Priority to CN201180009920.4A priority patent/CN102762752B/zh
Publication of WO2011102456A1 publication Critical patent/WO2011102456A1/ja

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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 for manufacturing a grain-oriented electrical steel sheet that suppresses variations in magnetic properties.
  • a grain-oriented electrical steel sheet is a steel sheet containing Si and having a crystal grain orientation highly accumulated in the ⁇ 110 ⁇ ⁇ 001> orientation, and is used as a material for a wound core of a stationary inductor such as a transformer. . Control of crystal grain orientation is performed by utilizing an abnormal grain growth phenomenon called secondary recrystallization.
  • An object of the present invention is to provide a method of manufacturing a grain-oriented electrical steel sheet that can suppress variations in magnetic properties.
  • the variation in magnetic properties after finish annealing as described above is particularly remarkable when the C content is 0.06% by mass or less, and further 0.048% by mass or less.
  • the cause of the variation in the magnetic properties after the finish annealing is not certain, but even if the crystal grains appear to be uniform before the finish annealing, the grains may not grow uniformly during the finish annealing. it is conceivable that.
  • the reason why the crystal grains do not grow uniformly is because the C content is low, the phase transformation during hot rolling is not sufficiently performed, the austenite transformation amount is small, and the hot rolling structure becomes unstable. It is possible that That is, it is considered that sufficient secondary recrystallization does not occur in the portion where the hot rolled structure becomes non-uniform, and sufficient magnetic properties are not obtained.
  • the present inventors are not able to sufficiently produce secondary recrystallization by forming effective precipitates in order to uniformize the grain growth during finish annealing. I thought. And the present inventors repeated the experiment which measures the magnetic characteristic of the grain-oriented electrical steel sheet obtained by adding various elements to a slab. As a result, the present inventors have found that the addition of Ti and Cu is effective for making the secondary recrystallization uniform.
  • the present invention has been made on the basis of the above findings, and the gist thereof is as follows.
  • Si 2.5% by mass to 4.0% by mass
  • C 0.01% by mass to 0.060% by mass
  • Mn 0.05% by mass to 0.20% by 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%
  • P 0.01 mass% to 0.00 mass%.
  • a step of hot-rolling steel comprising the balance of Fe and inevitable impurities to obtain a hot-rolled steel sheet; Performing annealing of the hot-rolled steel sheet to obtain an annealed steel sheet; Cold-rolling the annealed steel sheet to obtain a cold-rolled steel sheet; Performing decarburization annealing of the cold rolled steel sheet at a temperature of 800 ° C. to 950 ° C. to obtain a decarburized annealed steel sheet; Next, nitriding the decarburized annealed steel sheet at 700 ° C. to 850 ° C. to obtain a nitrided steel sheet, Performing a final annealing of the nitriding steel sheet; A method for producing a grain-oriented electrical steel sheet, comprising:
  • the steel further comprises Cr: 0.010 mass% to 0.20 mass%, Sn: 0.010 mass% to 0.20 mass%, 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 As: The method for producing a grain-oriented electrical steel sheet according to (1) or (2), comprising at least one selected from the group consisting of 0.005 mass% to 0.02 mass%.
  • the Ti content of the steel is 0.0020 mass% to 0.0080 mass%
  • the Cu content of the steel is 0.01% by mass to 0.10% by mass
  • the Ti content (mass%) of the steel is expressed as [Ti] and the Cu content (mass%) as [Cu]
  • a relationship of “20 ⁇ [Ti] + [Cu] ⁇ 0.18” is established.
  • an appropriate amount of Ti and / or Cu is contained in the steel, and since decarburization annealing and nitriding are performed at an appropriate temperature, variation in magnetic properties can be suppressed.
  • FIG. 1 is a diagram showing the relationship between Ti content and Cu content, and evaluation of magnetic flux density and its variation.
  • FIG. 2 is a flowchart showing a method for manufacturing a grain-oriented electrical steel sheet according to an embodiment of the present invention.
  • the present inventors repeatedly conducted an experiment for measuring the magnetic properties of the grain-oriented electrical steel sheet obtained by adding various elements to the slab, and in order to make secondary recrystallization uniform, Ti And the addition of Cu was found to be effective.
  • silicon steel having a C content of 0.06% by mass or less with a composition used for manufacturing grain-oriented electrical steel sheets by a low-temperature slab heating method was used.
  • this carbon steel was made to contain Ti and Cu in various ratios, and the steel ingot of various compositions was produced.
  • the steel ingot was heated at a temperature of 1250 ° C. or less to perform hot rolling, and then cold rolling was performed.
  • decarburization annealing was performed after cold rolling, and then nitriding treatment and finish annealing were performed.
  • the magnetic flux density B8 of the obtained grain-oriented electrical steel sheet was measured, and the dispersion
  • the magnetic flux density B8 is a magnetic flux density generated in the grain-oriented electrical steel sheet when a magnetic field of 800 A / m is applied at 50 Hz.
  • FIG. 1 An example of the results obtained by the above experiment is shown in FIG. Although details of the experiment will be described later, the circles in FIG. 1 indicate that the average value of the magnetic flux density B8 of the five single plate samples is 1.90 T or more, and the difference between the maximum value and the minimum value of the magnetic flux density B8. Is 0.030T or less. In FIG. 1, at least, the average value of the magnetic flux density B8 of at least 5 single-plate samples was less than 1.90T, or the difference between the maximum value and the minimum value of the magnetic flux density B8 exceeded 0.030T. Indicates that it was. From FIG. 1, when 0.0020 mass% to 0.010 mass% Ti and / or 0.010 mass% to 0.50 mass% Cu is contained in the steel ingot, the average value of the magnetic flux density B8 It is clear that the variation of the magnetic flux density B8 is small.
  • FIG. 2 is a flowchart showing a method for manufacturing a grain-oriented electrical steel sheet according to an embodiment of the present invention.
  • molten steel for grain-oriented electrical steel sheets having a predetermined composition is cast to produce a slab (step S1).
  • the casting method is not particularly limited.
  • Molten steel is, 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%, P: 0.01 mass% to 0 0.08% by mass.
  • the molten steel further contains at least one selected from the group consisting of Ti: 0.0020 mass% to 0.010 mass% and Cu: 0.010 mass% to 0.50 mass%.
  • the molten steel contains at least one of both Ti and Cu within a range of Ti: 0.010% by mass or less and Cu: 0.50% by mass or less, or at least Ti: 0.0020% by mass or Cu: 0.010. It contains so that one of the mass% or more may be satisfy
  • the balance of the molten steel consists of the balance Fe and inevitable impurities. Inevitable impurities include elements that form inhibitors in the manufacturing process of grain-oriented electrical steel sheets and remain in the grain-oriented electrical steel sheets after purification by high-temperature annealing.
  • Si is an extremely effective element for increasing the electrical resistance of the grain-oriented electrical steel sheet and reducing eddy current loss that constitutes part of the iron loss. If the Si content is less than 2.5% by mass, eddy current loss cannot be sufficiently suppressed. On the other hand, if the Si content exceeds 4.0% by mass, the workability deteriorates. Accordingly, the Si content is set to 2.5% by mass to 4.0% by mass.
  • C is an element effective in controlling the structure (primary recrystallization structure) obtained by the primary recrystallization. If the C content is less than 0.01% by mass, this effect cannot be sufficiently obtained. On the other hand, when the C content exceeds 0.06 mass%, the time required for decarburization annealing is increased, the discharge amount of CO 2 is increased. If the decarburization annealing is insufficient, it is difficult to obtain a grain-oriented electrical steel sheet with good magnetic properties. Therefore, the C content is set to 0.01 mass% to 0.06 mass%. In addition, as described above, in the conventional technique, when the C content is 0.048% by mass or less, the variation in magnetic properties after finish annealing is particularly remarkable. This is particularly effective when the content is 0.048% by mass or less.
  • Mn increases the specific resistance of grain-oriented electrical steel sheets and reduces iron loss. Mn also exhibits the effect of preventing cracking during hot rolling. When the Mn content is less than 0.05% by mass, these effects cannot be obtained sufficiently. On the other hand, when Mn content exceeds 0.20 mass%, the magnetic flux density of a grain-oriented electrical steel sheet will fall. Accordingly, the Mn content is set to 0.05 mass% to 0.20 mass%.
  • Acid-soluble Al is an important element that forms AlN that acts as an inhibitor. If the content of acid-soluble Al is less than 0.020% by mass, a sufficient amount of AlN cannot be formed, and the inhibitor strength is insufficient. On the other hand, if the content of acid-soluble Al exceeds 0.040% by mass, AlN becomes coarse and the inhibitor strength decreases. Therefore, the content of acid-soluble Al is 0.020 mass% to 0.040 mass%.
  • N is an important element that reacts with acid-soluble Al to form AlN.
  • nitriding since nitriding is performed after cold rolling, it is not necessary that the steel for grain-oriented electrical steel sheet contains a large amount of N.
  • the N content is set to 0.002 mass% to 0.012 mass%.
  • the N content is preferably 0.010% by mass or less.
  • MnS precipitate mainly affects the primary recrystallization, and exhibits the effect of suppressing the local fluctuation of the primary recrystallization grain growth caused by hot rolling. If the Mn content is less than 0.001% by mass, this effect cannot be sufficiently obtained. On the other hand, if the Mn content exceeds 0.010% by mass, the magnetic properties are likely to deteriorate. Accordingly, the Mn content is set to 0.001% by mass to 0.010% by mass. In order to further improve the magnetic properties, the Mn content is preferably 0.009% by mass or less.
  • P increases the specific resistance of the grain-oriented electrical steel sheet and reduces iron loss.
  • the P content is set to 0.01% by mass to 0.08% by mass.
  • Ti reacts with N to form TiN precipitates.
  • Cu reacts with S to form CuS precipitates. And these precipitates have the effect
  • TiN precipitates suppress variation in grain growth in the high temperature region of finish annealing and reduce deviation of magnetic properties of grain-oriented electrical steel sheets.
  • CuS precipitate suppresses the dispersion
  • the molten steel contains one or both of Ti and Cu in a range of Ti: 0.010 mass% or less and Cu: 0.50 mass% or less, at least Ti: 0.0020 mass% or more, or Cu: 0.010. It contains so that one of the mass% or more may be satisfy
  • the lower limit of the Ti content is preferably 0.0020% by mass, and the upper limit of the Ti content is preferably 0.0080% by mass. Moreover, it is preferable that the minimum of Cu content is 0.01 mass%, and it is preferable that the upper limit of Cu content is 0.10 mass%. Further, when the Ti content (mass%) is expressed as [Ti] and the Cu content (mass%) is expressed as [Cu], the relationship of “20 ⁇ [Ti] + [Cu] ⁇ 0.18” is established. Is more preferable, and the relationship of “10 ⁇ [Ti] + [Cu] ⁇ 0.07” is preferably satisfied.
  • Cr and Sn make the properties of the oxide layer formed during decarburization annealing good, and the properties of the glass film formed using this oxide layer during finish annealing also good. That is, Cr and Sn improve the magnetic characteristics through stabilization of the formation of the oxide layer and the glass film, and suppress variations in the magnetic characteristics.
  • Cr content exceeds 0.20% by mass
  • Sn content exceeds 0.20 mass%
  • coat may become inadequate. Therefore, it is preferable that both Cr content and Sn content are 0.20 mass% or less. Moreover, in order to fully obtain said effect, it is preferable that both Cr content and Sn content are 0.01 mass% or more.
  • Sn is a grain boundary segregation element and has the effect of stabilizing secondary recrystallization.
  • Sb 0.010% by mass to 0.20% by mass
  • Ni 0.010% by mass to 0.20% by mass
  • Se 0.005% by mass to 0.02% by mass
  • Bi 0.005% by 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% may be contained in the molten steel. All of these elements are inhibitor strengthening elements.
  • the slab is heated (step S2).
  • the heating temperature is preferably 1250 ° C. or less from the viewpoint of energy saving.
  • a hot rolled steel sheet is obtained by performing hot rolling of the slab (step S3).
  • the thickness of the hot-rolled steel sheet is not particularly limited and is, for example, 1.8 mm to 3.5 mm.
  • an annealed steel sheet is obtained by annealing the hot-rolled steel sheet (step S4).
  • the annealing conditions are not particularly limited, and for example, the annealing is performed at a temperature of 750 ° C. to 1200 ° C. for 30 seconds to 10 minutes. This annealing improves the magnetic properties.
  • a cold rolled steel sheet is obtained by performing cold rolling of the annealed steel sheet (step S5).
  • Cold rolling may be performed only once, or multiple times of cold rolling may be performed while 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, for example.
  • the reduction ratio of the final cold rolling is preferably 80% to 95%.
  • the cold rolled steel sheet is decarburized and annealed in a wet atmosphere containing hydrogen and nitrogen at 800 ° C. to 950 ° C. to obtain a decarburized annealed steel sheet (step S6).
  • Carbon in the steel sheet is removed by decarburization annealing, and primary recrystallization occurs.
  • the temperature of decarburization annealing is less than 800 ° C., crystal grains (primary recrystallized grains) obtained by primary recrystallization are too small, and subsequent secondary recrystallization is not sufficiently exhibited.
  • the temperature of decarburization annealing exceeds 950 ° C., the primary recrystallized grains are too large and the subsequent secondary recrystallization is not sufficiently developed.
  • the decarburized and annealed steel sheet is subjected to nitriding treatment in an atmosphere containing a gas having nitriding ability such as hydrogen, nitrogen and ammonia at 700 ° C. to 850 ° C. to obtain a nitrided steel sheet (step S7).
  • a gas having nitriding ability such as hydrogen, nitrogen and ammonia at 700 ° C. to 850 ° C.
  • the nitrogen content in the steel sheet increases. If the temperature of the nitriding treatment is less than 700 ° C. or exceeds 850 ° C., nitrogen hardly diffuses to the inside of the steel sheet, and the subsequent secondary recrystallization is not sufficiently developed.
  • an annealing separator mainly composed of MgO is applied to the surface of the nitrided steel sheet with a water slurry, and the nitrided steel sheet is wound into a coil shape. Then, by performing batch-type finish annealing on the coiled nitriding steel plate, a coiled finish annealed steel plate is obtained (step S8). Secondary recrystallization occurs by finish annealing.
  • step S9 After that, the coiled finish annealed steel sheet is unwound and the annealing separator is removed. Subsequently, a coating liquid mainly composed of aluminum phosphate and colloidal silica is applied to the surface of the finish-annealed steel sheet, and this baking is performed to form an insulating film (step S9).
  • the steel to be subjected to hot rolling is not limited to a slab obtained by casting molten steel, and a so-called thin slab may be used. Moreover, when using a thin slab, it is not necessary to perform slab heating below 1250 degreeC.
  • the hot-rolled steel sheet was annealed at 1100 ° C. for 120 seconds to obtain an annealed steel sheet.
  • pickling of the annealed steel sheet was performed, and then the annealed steel sheet was cold-rolled to obtain a cold-rolled steel sheet having a thickness of 0.23 mm.
  • decarburization annealing of the cold-rolled steel plate was performed for 100 seconds in the gas atmosphere containing water vapor
  • nitriding treatment of the decarburized and annealed steel sheet was performed for 20 seconds at 770 ° C. in a gas atmosphere containing hydrogen, nitrogen, and ammonia to obtain a nitrided steel sheet.
  • an annealing separator mainly composed of MgO was applied to the surface of the nitrided steel sheet with a water slurry. And the finish annealing for 20 hours was performed at 1200 degreeC, and the finish annealing steel plate was obtained. Subsequently, the finish-annealed steel sheet was washed with water and then sheared to a single-plate magnetic measurement size having a width of 60 mm and a length of 300 mm. Next, a coating liquid mainly composed of aluminum phosphate and colloidal silica was applied to the surface of the finish annealed steel sheet, and this baking was performed to form an insulating film. In this way, a sample of grain-oriented electrical steel sheet was obtained.
  • the magnetic flux density B8 of each grain-oriented electrical steel sheet was measured.
  • the magnetic flux density B8 is a magnetic flux density generated in the grain-oriented electrical steel sheet when a magnetic field of 800 A / m is applied at 50 Hz.
  • the magnetic flux density B8 of 5 single plate samples for measurement was measured.
  • an average value “average B8”, a maximum value “B8max”, and a 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 characteristics.
  • the evaluation results based on the average value “average B8” and the difference “ ⁇ B8” are shown in FIG. As described above, the circles in FIG. 1 indicate that the average value “average B8” is 1.90 T or more and the difference “ ⁇ B8” is 0.030 T or less. Further, in FIG. 1, ⁇ indicates that the average value “average B8” was less than 1.90T or the difference “ ⁇ B8” exceeded 0.030T.
  • Sample No. with a Ti content of less than 0.0020 mass% and a Cu content of less than 0.010 mass% In 1, the difference “ ⁇ B8” was as large as over 0.030T. That is, there was a large variation in magnetic characteristics. In addition, Sample No. with Ti content exceeding 0.010 mass%. 5 and Sample No. with a Cu content exceeding 0.50 mass%. No. 10 contained a large amount of precipitates, and as a result of affecting the finish annealing, the average value “average B8” was as small as less than 1.90T. That is, sufficiently high magnetic properties could not be obtained.
  • the hot-rolled steel sheet was annealed at 1090 ° C. for 120 seconds to obtain an annealed steel sheet.
  • pickling of the annealed steel sheet was performed, and then the annealed steel sheet was cold-rolled to obtain a cold-rolled steel sheet having a thickness of 0.23 mm.
  • eight steel plates for annealing were cut out from the cold-rolled steel plates, and the steel plates were decarburized and annealed at a temperature T1 of 790 ° C. to 960 ° C. shown in Table 2 in a gas atmosphere containing steam, hydrogen, and nitrogen. A decarburized and annealed steel sheet was obtained after 80 seconds.
  • nitriding treatment of the decarburized annealing steel sheet was performed for 20 seconds in a gas atmosphere containing water vapor, hydrogen, nitrogen, and ammonia at a temperature T2 of 680 ° C. to 880 ° C. shown in Table 2 to obtain a nitriding steel sheet.
  • an annealing separator mainly composed of MgO was applied to the surface of the nitrided steel sheet with a water slurry. And the finish annealing for 20 hours was performed at 1200 degreeC, and the finish annealing steel plate was obtained. Subsequently, in the same manner as in the first experiment, treatments from washing to formation of the insulating coating were performed, and a sample of grain-oriented electrical steel sheet was obtained.
  • the sample No. 2 has a decarburization annealing temperature T1 and a nitriding temperature T2 within the scope of the present invention. 22-No. 24, and no. 27, the average value “average B8” was as large as 1.90 T or more, and the difference “ ⁇ B8” was as small as 0.030 T or less. That is, high magnetic characteristics were obtained, and variations in magnetic characteristics were small.
  • Sample No. with a decarburization annealing temperature T1 of more than 950 ° C. 25 the difference “ ⁇ B8” was as large as over 0.030T, and the average value “average B8” was as small as less than 1.90T.
  • the sample No. nitriding temperature T2 is less than 700 ° C. 26
  • the average value “average B8” was as small as less than 1.90T.
  • Sample No. with nitriding temperature T2 exceeding 850 ° C. 28 the difference “ ⁇ B8” was as large as more than 0.030T, and the average value “average B8” was as small as less than 1.90T.
  • the hot-rolled steel sheet was annealed at 1090 ° C. for 120 seconds to obtain an annealed steel sheet.
  • pickling of the annealed steel sheet was performed, and then the annealed steel sheet was cold-rolled to obtain a cold-rolled steel sheet having a thickness of 0.23 mm.
  • the steel plate for annealing was cut out from the cold rolled steel plate, and the decarburization annealing of the steel plate was performed for 80 seconds in the gas atmosphere containing water vapor
  • nitriding treatment of the decarburized and annealed steel sheet was performed for 20 seconds in a gas atmosphere containing water vapor, hydrogen, nitrogen, and ammonia at 760 ° C. to obtain a nitrided steel sheet.
  • an annealing separator mainly composed of MgO was applied to the surface of the nitrided steel sheet with a water slurry. And the finish annealing for 20 hours was performed at 1200 degreeC, and the finish annealing steel plate was obtained. Subsequently, in the same manner as in the first experiment, treatments from washing to formation of the insulating coating were performed, and a sample of grain-oriented electrical steel sheet was obtained.
  • sample Nos. C, C, Ti and Cu are within the scope of the present invention.
  • 32-No. 34, no. 37-No. 39, no. 42-No. 44, and no. 47-No. 49 the average value “average B8” was as large as 1.90 T or more, and the difference “ ⁇ B8” was as small as 0.025 T or less. That is, high magnetic characteristics were obtained, and variations in magnetic characteristics were small. In particular, good results were obtained when the C content was low.
  • the Ti content is 0.0020 to 0.080 mass%
  • the Cu content is 0.010 to 0.10 mass%
  • “20 ⁇ [Ti] + [Cu] ⁇ 0.18” Sample no. 32, no. 33, no. 37, no. 38, no. 42, no. 43, no. 47, and no. 48, the balance of the average value “average B8” and the difference “ ⁇ B8” was good. Among them, sample No. 1 in which the relationship of “10 ⁇ [Ti] + [Cu] ⁇ 0.07” is satisfied. 32, no. 37, no. 42, and no. 47, the balance between the average value “average B8” and the difference “ ⁇ B8” was very good.
  • the hot-rolled steel sheet was annealed at 1080 ° C. for 120 seconds to obtain an annealed steel sheet.
  • pickling of the annealed steel sheet was performed, and then the annealed steel sheet was cold-rolled to obtain a cold-rolled steel sheet having a thickness of 0.23 mm.
  • decarburization annealing of the cold-rolled steel sheet was performed for 90 seconds in a gas atmosphere containing water vapor, hydrogen, and nitrogen at 870 ° C. to obtain a decarburized annealed steel sheet.
  • nitriding treatment of the decarburized and annealed steel sheet was performed for 20 seconds in a gas atmosphere containing hydrogen, nitrogen, and ammonia at 760 ° C. to obtain a nitrided steel sheet.
  • an annealing separator mainly composed of MgO was applied to the surface of the nitrided steel sheet with a water slurry. And the finish annealing for 20 hours was performed at 1200 degreeC, and the finish annealing steel plate was obtained. Subsequently, in the same manner as in the first experiment, treatments from washing to formation of the insulating coating were performed, and a sample of grain-oriented electrical steel sheet was obtained.
  • sample no. In any of 51 to 60 the average value “average B8” was as large as 1.90 T or more, and the difference “ ⁇ B8” was as small as 0.030 T or less. That is, high magnetic characteristics were obtained, and variations in magnetic characteristics were small.
  • sample No. 1 containing 0.010% by mass to 0.20% by mass of Cr and / or 0.010% by mass to 0.20% by mass of Sn. 52, no. 53, no. 55, no. 56, no. 58-No.
  • the average value “average B8” was particularly large at 1.91 T or more, and the difference “ ⁇ B8” was particularly small at 0.025 T or less.
  • the present invention can be used, for example, in the electrical steel sheet manufacturing industry and the electrical steel sheet utilizing industry.

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JP2019035120A (ja) * 2017-08-17 2019-03-07 新日鐵住金株式会社 方向性電磁鋼板の製造方法
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BR112020000223A2 (pt) 2017-07-13 2020-07-07 Nippon Steel Corporation folha de aço eletromagnética orientada
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KR20170041233A (ko) 2014-09-04 2017-04-14 제이에프이 스틸 가부시키가이샤 방향성 전기 강판의 제조 방법 및 질화 처리 설비
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JP2019035120A (ja) * 2017-08-17 2019-03-07 新日鐵住金株式会社 方向性電磁鋼板の製造方法

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