WO2023157765A1 - 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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WO2023157765A1
WO2023157765A1 PCT/JP2023/004544 JP2023004544W WO2023157765A1 WO 2023157765 A1 WO2023157765 A1 WO 2023157765A1 JP 2023004544 W JP2023004544 W JP 2023004544W WO 2023157765 A1 WO2023157765 A1 WO 2023157765A1
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Prior art keywords
mass
less
annealing
temperature
rolling
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English (en)
French (fr)
Japanese (ja)
Inventor
雅紀 竹中
猛 今村
孝明 田中
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JFE Steel Corp
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JFE Steel Corp
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Priority to CN202380021559.XA priority Critical patent/CN118696135A/zh
Priority to EP23756291.3A priority patent/EP4474492A4/en
Priority to US18/837,692 priority patent/US20250163529A1/en
Priority to KR1020247026772A priority patent/KR20240134363A/ko
Priority to JP2023524309A priority patent/JP7338812B1/ja
Publication of WO2023157765A1 publication Critical patent/WO2023157765A1/ja
Anticipated expiration legal-status Critical
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    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C2202/00—Physical properties
    • C22C2202/02—Magnetic
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Definitions

  • the present invention relates to a method for producing a so-called grain-oriented electrical steel sheet in which crystal grains are highly concentrated in the miller index of ⁇ 110 ⁇ on the sheet surface and ⁇ 001> in the rolling direction.
  • a grain-oriented electrical steel sheet is a soft magnetic material, and is mainly used as iron cores of electrical equipment such as transformers.
  • This grain-oriented electrical steel sheet utilizes secondary recrystallization to highly accumulate crystal grains in the ⁇ 110 ⁇ 001> orientation (hereinafter referred to as "Goss orientation"), resulting in low iron loss and high magnetic flux density. It has excellent magnetic properties.
  • a magnetic flux density B 8 (T) at a magnetic field strength of 800 (A/m) and an alternating magnetic field with an excitation frequency of 50 (Hz) are 1.
  • Iron loss W 17/50 (W/kg) per 1 kg of steel sheet when magnetized to 7 (T) is generally used.
  • Patent Document 1 discloses a method using AlN and MnS as inhibitors
  • Patent Document 2 discloses a method using MnS and MnSe as inhibitors, both of which have been industrially put into practical use.
  • it is ideal to disperse the inhibitor uniformly and finely, and therefore, it is necessary to heat the raw material steel slab to a high temperature of 1300 ° C. or higher before hot rolling. ing.
  • Patent Document 7 discloses a method of regulating the final rolling reduction in hot rough rolling
  • Patent Document 8 discloses a method of controlling the casting structure of a slab
  • Patent Document 9 discloses a slab cross-sectional shape. is disclosed.
  • the techniques proposed in Patent Documents 7 to 9 are somewhat effective in preventing edge cracks, they cannot be said to be effective methods for completely preventing edge cracks.
  • Patent Documents 10 to 14 disclose hot rolling methods for grain-oriented silicon steel sheets in which edge cracks are prevented by arranging the side surface shape of the sheet bar during hot rolling.
  • these methods are more effective in preventing cracked edges than the above-described methods, they are still not completely capable of preventing cracked edges.
  • Patent Document 15 proposes a method of performing horizontal reduction in addition to width reduction after slab heating, followed by high-temperature slab heating.
  • Patent Document 15 the technique of performing width reduction processing on the slab before heating the slab at a high temperature disclosed in Patent Document 15 has the effect of significantly suppressing edge cracking of the hot-rolled sheet, but a new problem has arisen. That is, the temperature of the width edges of the slab decreases due to the width reduction, and the heating of the width edges becomes insufficient in the subsequent high-temperature slab heating, resulting in insufficient inhibitor solid solution and uniform finely dispersed precipitation during hot rolling. Become. As a result, there is a problem that a part where secondary recrystallization is incomplete occurs at the width end portion of the product sheet. The incompletely secondary recrystallized portion must be discarded, resulting in a significant decrease in yield.
  • the present invention has been made in view of the above-mentioned problems of the prior art, and an object of the present invention is to provide a method for producing a grain-oriented electrical steel sheet using AlN, MnS and/or MnSe as an inhibitor, during hot rolling.
  • the object of the present invention is to propose a technique for effectively preventing occurrence of secondary recrystallization defects at the width end portions of a product sheet while preventing edge cracks from occurring.
  • the inventors have diligently studied measures to solve the above problems.
  • the average temperature increase rate in the width direction between 700 and 900 ° C. in the first annealing applied to the steel plate after hot rolling
  • the present invention based on the above knowledge is a method for producing a grain-oriented electrical steel sheet, wherein the above-mentioned production method includes C: 0.02 to 0.10 mass%, Si: 2.5 to 5.5 mass%, Mn: 0.01 to 0.30 mass%, sol.
  • a steel slab having a chemical composition with the balance being Fe and unavoidable impurities is heated, then hot rolled, and then cold rolled once or cold rolled twice or more with intermediate annealing in between to obtain the final thickness
  • the cold-rolled sheet is subjected to primary recrystallization annealing that also serves as decarburization annealing, an annealing separator is applied to the surface of the steel sheet, and then finish annealing is performed.
  • the temperature rise rate at the center of the width between 700 and 900 ° C. in the temperature rise process of the first annealing after hot rolling is Rc (° C./s)
  • the temperature rise rate of the width end is Re (° C./s)
  • the above Rc and Re are expressed by the following formula (2); Re ⁇ Rc (2) is characterized by satisfying
  • the Tc and Te are expressed by the following formula (3); 10 ⁇ (Tc ⁇ Te) ⁇ 100 (3) and the above Rc and Re are the following formula (4); (Re ⁇ Rc) ⁇ (Tc ⁇ Te)/50 (4) is characterized by satisfying
  • the method for manufacturing the grain-oriented electrical steel sheet according to the present invention is characterized by including any one of the following steps. Note ⁇ After heating the steel slab, after rough rolling in a temperature range of 1100 ° C to 1400 ° C for one pass or more, finish rolling in a temperature range of 800 to 1300 ° C for two passes or more to make a hot rolled sheet, After that, a hot rolling process of winding into a coil at a coiling temperature of 400 to 750 ° C.
  • the intermediate annealing process is cooled from 800 ° C to 350 ° C at 5 to 100 ° C / s ⁇ H2 and N2 included,
  • a primary recrystallization annealing process that also serves as decarburization annealing, in which the temperature range of 750 to 950°C is maintained for 10 seconds or more in a moist atmosphere with a dew point of 20 to 80°C or less.
  • the steel slab used in the method for producing the grain-oriented electrical steel sheet of the present invention further includes Ni: more than 0 mass% and 1.00 mass% or less, Sb: more than 0 mass% and 0.50 mass% or less, Sn: more than 0 mass% and 0.50 mass% or less, Cu: more than 0 mass% and 0.50 mass% or less, Cr: more than 0 mass% and 0.50 mass% or less, P: more than 0 mass% and 0.50 mass% or less, Mo: more than 0 mass% and 0 .50 mass% or less, Nb: 0 mass% to 0.020 mass%, V: 0 mass% to 0.010 mass%, B: 0 mass% to 0.0025 mass%, Bi: 0 mass% to 0.50 mass%, and Zr : characterized by containing at least one selected from more than 0 mass% and 0.10 mass% or less.
  • the steel slab used in the method for producing the grain-oriented electrical steel sheet of the present invention is characterized by further containing Co: more than 0 mass% and 0.0200 mass% or less in addition to the above chemical composition.
  • the steel slab used in the method for producing the grain-oriented electrical steel sheet of the present invention further includes, in addition to the above chemical composition, Ti: more than 0 mass% and 0.0200 mass% or less and W: 0.001 to 0.050 mass% or less characterized by containing at least one selected from
  • the steel slab used in the method for producing the grain-oriented electrical steel sheet of the present invention further includes, in addition to the above chemical composition, Zn: more than 0 mass% and 0.0200 mass% or less, Pb: more than 0 mass% and 0.0100 mass% or less, As: more than 0 mass% and 0.020 mass% or less, Ag: more than 0 mass% and 0.200 mass% or less, Au: more than 0 mass% and 0.200 mass% or less, Ga: more than 0 mass% and 0.0200 mass% or less, Ge: more than 0 mass% and 0 .0200 mass% or less, Ca: more than 0 mass% and 0.0200 mass% or less, Mg: more than 0 mass% and 0.0200 mass% or less, REM: more than 0 mass% and 0.0200 mass% or less, and Hf: more than 0 mass% and 0.020 mass% or less characterized by containing at least one selected from
  • grain-oriented electrical steel sheets can be manufactured at high yield and at low cost.
  • 4 is a graph showing the effects of (Tc-Te) and R on the maximum width of secondary recrystallization defects. 4 is a graph showing the effects of (Tc-Te) and (Re-Rc) on the maximum width of secondary recrystallization defects.
  • Table 1 shows the surface temperature Tc (° C.) at the center of the width of the slab after width reduction and horizontal rolling, the surface temperature Te (° C.) at the edge of the width, and the temperature difference between Tc and Te (Tc ⁇ Te). Indicated.
  • the surface temperature at the center of the slab width means the surface temperature at the center of the width of the upper surface (long side) of the slab, and the surface temperature at the width end means the temperature at the center of the thickness of the side face (short side) of the slab.
  • edge cracks are reduced by width reduction processing.
  • Working strain is introduced into the slab width end by performing a width reduction of 50 mm per side of the steel slab.
  • processing distortion is also introduced by horizontal reduction for correcting the dog-bone shape generated at the slab width end portion by the width reduction processing. As a result, a large working strain was applied to the width end portions of the slab, and the crystal grain size at the width end portions of the slab was reduced.
  • the hot-rolled sheet was soaked at 1150°C for 120 seconds, it was subjected to hot-rolled sheet annealing by water cooling from 800°C to 350°C at 50°C/s.
  • the average temperature increase rate R (° C./s) in the width direction between 700 and 900 ° C. in the temperature increase process of hot-rolled steel annealing, the temperature increase rate Rc (° C./ s) and the temperature rise rate Re (°C/s) at the edge of the sheet width were variously changed as shown in Table 1.
  • the rate of temperature rise in the width direction is the average rate of temperature rise over the entire width of the strip, and the rate of temperature rise at the edge of the width of the strip is the rate of temperature rise at the portion 30 mm inward from both width edges. It is the lower heating rate of the rates.
  • the steel sheet after the hot-rolled sheet annealing was pickled to remove surface scales, and then cold-rolled to obtain a cold-rolled sheet having a final sheet thickness of 0.27 mm.
  • the cold-rolled sheet was subjected to primary recrystallization annealing, which also serves as decarburization annealing, at 800° C. for 60 s in a moist atmosphere containing H 2 and N 2 and having a dew point of 50° C.
  • primary recrystallization annealing which also serves as decarburization annealing, at 800° C. for 60 s in a moist atmosphere containing H 2 and N 2 and having a dew point of 50° C.
  • an annealing separator containing MgO as a main component was applied to the surface of the steel sheet at 5 g/m 2 per side, dried, and wound into a coil.
  • final annealing was performed by holding at a temperature of 1240° C. for 5 hours for purification.
  • the temperature range of 1050° C. or higher was an atmosphere containing H 2 as a main component.
  • a phosphate-based tension imparting insulation coating is applied, and flattened annealing is performed to bake the coating and correct the shape of the steel sheet. was applied to make a product board.
  • FIG. 1 shows the relationship between (Tc ⁇ Te) and R in a coil with a width reduction of 50 mm per side and the maximum width of secondary recrystallization defects.
  • the depth (distance from the width edge) of the secondary recrystallization defect generated at the width edge of the product sheet is the tip (coil outermost winding) and the tail end of each product sheet coil.
  • a sample of 30 mm width was taken from both ends of the sheet (the innermost winding of the coil). It is obtained by measuring the crystal orientation by the SEM-EBSD method after mirror finishing by diamond polishing, alumina polishing, colloidal silica polishing, or the like.
  • an area of 2 mm in the rolling direction ⁇ 30 mm in the sheet width direction is measured in steps of 1 ⁇ m for samples taken using an EBSD measurement system manufactured by EDAX, and an area of 95% or more of the entire measurement area
  • the surface state of the sample, the SEM conditions, and the EBSD conditions were adjusted so as to obtain a Confidence Index>0.1.
  • the obtained data was analyzed by OIM Analysis manufactured by EDAX, and secondary recrystallized grains with a misorientation angle of 20° or less from ⁇ 110 ⁇ 001> and a recrystallized grain size of 1 mm or more were selected.
  • the other regions were determined to be secondary recrystallization defects, and the distance from the edge of the width of the region where the secondary recrystallization defects occurred was defined as the depth of the secondary recrystallization defects.
  • the maximum depth of the secondary recrystallization defect at both the leading edge and the trailing edge of the product sheet was taken as the maximum width of the secondary defective recrystallization area of the coil.
  • the width end portion of the slab whose temperature has decreased during the slab heating process, remains lower in temperature than the width center portion even if the slab is subsequently heated to a high temperature. Moreover, even if the predetermined soaking temperature is reached, the soaking time is shorter than that at the center of the width, so the inhibitor is not completely solid-dissolved. As a result, the amount of precipitates (inhibitors) that precipitate uniformly and finely during the hot rolling process is reduced, making it difficult to create a difference in grain boundary mobility between Goss-oriented grains and other oriented grains. is considered to be in a state where secondary recrystallization is difficult.
  • the heating rate in the heating process of the first annealing after hot rolling is increased, the additionally precipitated precipitates are refined, so that the mobility difference at the grain boundary is reduced. It is thought that it can be imparted and the secondary recrystallization failure is suppressed.
  • the temperature Tc (° C.) at the center of the width of the slab and the temperature Te (° C.) at the edge of the width of the slab after width reduction and horizontal rolling were measured.
  • the slab is put into the heating furnace again, heated to a temperature of 1300° C., held at the temperature for 120 minutes, extracted from the heating furnace, and subjected to rough hot rolling to obtain a sheet bar having a thickness of 30 mm, Furthermore, after finishing hot rolling to obtain a hot-rolled sheet having a sheet thickness of 3.0 mm, the sheet was water-cooled and wound into a coil at a temperature of 700°C.
  • the hot-rolled sheet was pickled without performing hot-rolled sheet annealing to remove scales on the surface, and then cold-rolled for the first time to an intermediate sheet thickness of 0.7 mm.
  • intermediate annealing is performed by water cooling from 800°C to 350°C at 30°C/s
  • pickling is performed to remove scales on the surface
  • cold rolling is performed for the second time to achieve a final thickness of 0.23 mm. cold-rolled sheet.
  • the heating rate Re (°C/s) of the part was changed as shown in Table 2.
  • the cold-rolled sheet is subjected to primary recrystallization annealing, which also serves as decarburization annealing, at 900°C for 120 seconds in a moist atmosphere containing H 2 and N 2 at a dew point of 60°C, and then separated by annealing containing MgO as the main component.
  • the agent was applied to the surface of the steel sheet at 3 g/m 2 per side, dried, and wound into a coil.
  • the steel sheet was held at a temperature of 1150°C for 20 hours to undergo final annealing for purification. did.
  • the atmosphere in the temperature range of 900° C. or higher was an atmosphere containing H 2 as a main component.
  • a phosphate-based tension imparting insulation coating is applied, and flattened annealing is performed to bake the coating and correct the shape of the steel sheet. was applied to make a product board.
  • FIG. 2 shows the relationship between (Re--Rc), (Tc--Te) and the maximum width of secondary recrystallization defects.
  • the secondary recrystallization defect that occurs at the width edge of the product sheet can be reduced by increasing the temperature increase rate in the heating process of the first annealing after hot rolling.
  • the reason why it can be suppressed is as described in ⁇ Experiment 1>.
  • the temperature rising rate at the edge of the width is actively increased more than the temperature rising rate at the center of the width, and the above equations (2) to (4)
  • the inventors believe that the reason why the effect of the present invention becomes more remarkable by heating while satisfying is as follows.
  • the temperature increase rate in the temperature increase process of the first annealing after hot rolling is such that the temperature increase rate at the edge of the width is higher than the temperature increase rate at the center of the width as shown in equation (2),
  • the temperature within the range of the formula (4) it is possible to refine the precipitates that are additionally precipitated during the temperature rising process. As a result, the effect of suppressing secondary recrystallization defects in the final annealing step becomes remarkable.
  • C 0.02 to 0.10 mass%
  • C is an element necessary for improving the hot-rolled sheet structure by utilizing the austenite-ferrite transformation that occurs during hot rolling and soaking in hot-rolled sheet annealing. If the C content is less than 0.02 mass%, the grain boundary strengthening effect of C is lost, causing defects such as cracks in the slab that hinder production. On the other hand, if the C content exceeds 0.10 mass%, not only will the decarburization load increase, but the decarburization itself will be incomplete, which may cause magnetic aging in the product sheet. Therefore, the C content should be in the range of 0.02 to 0.10 mass%. It is preferably in the range of 0.03 to 0.08 mass%.
  • Si 2.5 to 5.5 mass%
  • Si is an element that is extremely effective in increasing the resistivity of steel and reducing eddy current loss that constitutes a part of core loss. If the Si content is less than 2.5 mass%, the reduction effect is small, and good iron loss characteristics cannot be obtained. On the other hand, the specific resistance of steel increases monotonously up to a Si content of 11 mass%, but when the Si content exceeds 5.5 mass%, the workability drops significantly, making it difficult to manufacture by rolling. Therefore, the Si content should be in the range of 2.5 to 5.5 mass%. It is preferably in the range of 3.0 to 4.0 mass%.
  • Mn 0.01-0.30 mass%
  • Mn forms MnS and MnSe and functions as an inhibitor that suppresses normal grain growth during the temperature rising process of final annealing, so it is an important element in the production of grain-oriented electrical steel sheets.
  • the Mn content is less than 0.01 mass%, the absolute amount of the inhibitor becomes insufficient, and the ability to suppress normal grain growth becomes insufficient.
  • the Mn content exceeds 0.30 mass%, it becomes difficult to sufficiently dissolve the Mn by heating the slab, and the magnetic properties deteriorate. Therefore, the content of Mn should be in the range of 0.01 to 0.30 mass%. It is preferably in the range of 0.05 to 0.20 mass%.
  • At least one of S and Se 0.001 to 0.040 mass% in total S and Se combine with Mn to form MnS and MnSe, which act as inhibitors.
  • the total content of S and Se is less than 0.001 mass %, the amount of inhibitor will be insufficient and the effect of improving magnetic properties will not be sufficiently obtained.
  • the total content exceeds 0.040 mass %, it becomes difficult to achieve a sufficient solid solution by heating the slab, and the magnetic properties are greatly deteriorated.
  • S exceeds 0.040 mass% edge cracking occurs during hot rolling. Therefore, in order to achieve both magnetic properties and manufacturability, the total content of S and Se should be in the range of 0.001 to 0.040 mass%. It is preferably in the range of 0.002 to 0.015 mass%.
  • sol. Al 0.010 to 0.040 mass%
  • Al is an element that forms and precipitates AlN, functions as an inhibitor that suppresses normal grain growth in secondary recrystallization annealing, and is an important element in grain-oriented electrical steel sheets.
  • the Al content is less than 0.010 mass% in terms of acid-soluble Al (sol. Al)
  • the absolute amount of the inhibitor is insufficient, and the ability to suppress normal grain growth is insufficient.
  • sol. If Al exceeds 0.040 mass%, it cannot be dissolved sufficiently by heating the slab, and fine dispersion in the steel cannot be achieved, resulting in significant deterioration in magnetic properties. Therefore, the Al content is sol.
  • Al should be in the range of 0.010 to 0.040 mass%. It is preferably in the range of 0.015 to 0.030 mass%.
  • N 0.004 to 0.020 mass% N binds and precipitates with Al to form AlN, which acts as an inhibitor. However, if the content is less than 0.004 mass%, the absolute amount of the inhibitor is insufficient, and the ability to suppress normal grain growth is insufficient. On the other hand, if it exceeds 0.020 mass%, the slab may swell during hot rolling. Therefore, the content of N should be in the range of 0.004 to 0.020 mass%. It is preferably in the range of 0.006 to 0.010 mass%.
  • the steel material used in the present invention may contain the following components in addition to the essential components described above. Ni: more than 0 mass% and 1.00 mass% or less, Sb: more than 0 mass% and 0.50 mass% or less, Sn: more than 0 mass% and 0.50 mass% or less, Cu: more than 0 mass% and 0.50 mass% or less, Cr: more than 0 mass% and 0 .50 mass% or less, P: 0 mass% to 0.50 mass%, Mo: 0 mass% to 0.50 mass%, Nb: 0 mass% to 0.020 mass%, V: 0 mass% to 0.010 mass%, B : more than 0 mass% and 0.0025 mass% or less, Bi: more than 0 mass% and 0.50 mass% or less, and Zr: more than 0 mass% and 0.10 mass% or less. can be contained as appropriate. However, if the amount of each element added exceeds the above upper limit, the growth of secondary recrystallized grains is suppressed and the magnetic properties are rather deteriorat
  • Co More than 0 mass% and 0.0200 mass% or less Co is an element effective in improving the primary recrystallization texture and improving the magnetic properties of the product sheet, so it can be contained as appropriate. However, when the above upper limit is exceeded, the effect of improving the magnetic properties is saturated, leading to an increase in raw material costs.
  • Ti more than 0 mass% and 0.0200 mass% or less and W: at least one selected from 0.001 to 0.050 mass% or less Ti and W form fine carbides and nitrides, and crystals after annealing Since it refines the grain size, it has the effect of improving brittleness and suppressing problems in sheet threading, so it can be contained as appropriate. However, when the above upper limit is exceeded, the above effect is saturated, and the raw material cost is increased.
  • Zn more than 0 mass% and 0.0200 mass% or less
  • Pb more than 0 mass% and 0.0100 mass% or less
  • Ca more than 0 mass% and 0.0200 mass% or less
  • Mg more than 0 mass% and 0.0200 mass% or less
  • REM more than 0 mass% and 0.0200 mass% or less
  • Hf more than 0 mass% and 0.020 mass% or less Since it has the effect of strengthening boundaries and suppressing defects caused by intergranular fracture, it can be contained as appropriate. However, when the above upper limit is exceeded, the above effect is saturated, and the raw material cost is increased.
  • the balance other than the above components is Fe and unavoidable impurities.
  • the above-mentioned unavoidable impurities mean elements that are unavoidably mixed from raw materials, scraps, smelting pots, etc. when steel is smelted.
  • the steel material (slab) used for manufacturing the grain-oriented electrical steel sheet of the present invention is produced by melting steel having the above-described chemical composition by a commonly known refining process and then by a commonly known ingot casting method or continuous casting method.
  • a thin slab having a thickness of 100 mm or less may be produced by a direct casting method.
  • the above slabs and thin cast pieces are subjected to hot rolling after being heated by a normal method, but it is desirable that the slab heating temperature before hot rolling is 1300°C or higher so that the inhibitor-forming components are completely dissolved.
  • the slab may be heated to 1300° C. or higher in one heating furnace, or may be heated using two or more heating furnaces.
  • a heating method a known method such as a combustion gas heating method, an electric heating method, or an induction heating method can be adopted.
  • the slab heating step the slab is heated to a temperature range of 900 to 1300° C., and then width reduction is performed within a range of 50 to 200 mm per side.
  • Horizontal rolling horizontal reduction
  • the crystal grain size at the width end portion of the slab is refined, and edge cracking in subsequent hot rolling can be remarkably suppressed.
  • a width reduction of 50 mm or more per side is required.
  • the upper limit is set to about 200 mm.
  • a preferable width reduction amount is in the range of 100 to 150 mm.
  • the processing method for width reduction is not particularly limited as long as it is suitable for this purpose, and known processing techniques such as press, vertical roll, and edger can be used.
  • the horizontal rolling that follows the width reduction process is performed for the purpose of correcting and flattening the dog-bone shape caused by the width reduction process, but the pressure reduction may be performed within a range that does not hinder productivity.
  • the slabs and thin cast pieces subjected to width reduction and horizontal rolling are heated at a high temperature of 1300 to 1450°C for 0 to 120 minutes, and then subjected to hot rolling consisting of rough rolling and finish rolling.
  • Rough rolling is preferably carried out in the range of 1100 to 1400° C. with one pass or more.
  • the finish rolling subsequent to the rough rolling is preferably carried out in the range of 800 to 1300° C. under conditions of two or more passes.
  • the coiling temperature after finish rolling is preferably in the range of 400 to 750° C. from the viewpoint of controlling the form of precipitated carbides and preventing cracks in the steel sheet. More preferably, it is in the range of 500 to 700°C.
  • the steel sheet (hot-rolled sheet) after the hot rolling is subjected to hot-rolled sheet annealing at a temperature of 900 to 1250° C. for 5 seconds or more from the viewpoint of homogenizing the steel sheet structure and reducing the variation in magnetic properties. preferably applied.
  • a more preferable soaking condition is a condition in which a temperature of 950 to 1150° C. is maintained for 10 to 180 seconds. After the soaking, it is preferable to cool the temperature range from 800° C. to 350° C. at a cooling rate of 5 to 100° C./s from the viewpoint of optimizing the morphology of the second phase and precipitates. More preferably, it is in the range of 15 to 80°C/s.
  • the steel sheet (hot-rolled sheet) after hot rolling or after hot-rolled sheet annealing is preferably descaled in order to remove the oxide film formed on the surface of the steel sheet during hot rolling.
  • known methods such as a pickling method using a heated acid, a mechanical descaling method for mechanically removing scale, and a combination of these methods can be used.
  • the hot-rolled sheet from which the scale has been removed is cold-rolled once or cold-rolled twice or more with intermediate annealing to obtain a cold-rolled sheet having a final thickness.
  • the soaking conditions for the intermediate annealing are preferably such that the temperature is kept at 900 to 1250° C. for 5 seconds or longer. If the soaking temperature is less than 900° C., the recrystallized grains become too fine, the number of Goss nuclei in the primary recrystallized structure decreases, and the magnetic properties may deteriorate. On the other hand, if the temperature exceeds 1250° C., rapid growth and decomposition of the inhibitor occur, which may also lead to deterioration of the magnetic properties. More preferably, the temperature is maintained at 900 to 1150° C. for 10 to 180 seconds.
  • the cooling after the soaking is preferably from 800°C to 350°C at a rate of 5 to 100°C/s from the viewpoint of controlling the morphology of the second phase and precipitates. More preferably, it is 15 to 80°C/s.
  • it is preferable to remove the rolling oil before the intermediate annealing.
  • it is desirable to remove the scale on the surface of the steel sheet caused by the annealing.
  • a descaling method a known method such as a pickling method using a heated acid, a mechanical descaling method for mechanically removing scale, or a combination thereof can be used.
  • the average temperature increase rate R (° C./s) in the plate width direction between ° C. is the following (1) formula; R ⁇ 5+(Tc ⁇ Te)/20 (1) It means that it is necessary to control so as to satisfy
  • Tc and Te are expressed by the following formula (3); 10 ⁇ (Tc ⁇ Te) ⁇ 100 (3) and the above Rc and Re are the following formula (4); (Re ⁇ Rc) ⁇ (Tc ⁇ Te)/50 (4) It is preferable to satisfy
  • the first annealing performed on the steel sheet after hot rolling means hot-rolled sheet annealing when hot-rolled sheet annealing is performed, and intermediate annealing is performed between cold rolling without hot-rolled sheet annealing. If it is performed, it refers to intermediate annealing, and if neither hot-rolled sheet annealing nor intermediate annealing is performed, it refers to primary recrystallization annealing that also serves as decarburization annealing after cold rolling.
  • the method for making the temperature rise rate Re at the strip width edge faster than the temperature rise rate Rc at the strip width center is not particularly limited as long as it is suitable for this purpose.
  • the edge of the width of the strip is locally heated, the surface condition is devised to increase the heat absorption of the edge of the width of the strip, and heat retention measures are taken to suppress heat extraction from the edge of the width of the strip. etc., a known method can be used.
  • the total rolling reduction of the cold rolling is preferably in the range of 50 to 92%.
  • the total rolling reduction of each cold rolling is in the range of 50 to 92%.
  • the steel sheet (cold-rolled sheet) cold-rolled to the final thickness is then subjected to primary recrystallization annealing that also serves as decarburization annealing, but before that, degreasing and pickling are performed to clean the surface of the steel sheet.
  • Decarburization annealing in the primary recrystallization annealing is preferably carried out at a temperature of 750 to 950° C. for 10 seconds or longer. More preferable conditions are 800-900° C. ⁇ 30-180 s.
  • the atmosphere during the decarburization annealing is preferably a moist atmosphere containing H 2 and N 2 and having a dew point of 20 to 80°C. A more preferred dew point is in the range of 40-70°C.
  • the steel sheet is preferably coated with an annealing separator containing MgO as a main component on the surface of the steel sheet in a basis weight of 3 g/m 2 or more per side.
  • the upper limit of the basis weight is not particularly limited, it is preferably about 10 g/m 2 from the viewpoint of manufacturing cost.
  • MgO may be applied to the surface of the steel sheet in the form of a slurry, or may be dry-applied by electrostatic coating. When the slurry is applied, it is preferable to keep the slurry solution at a constant temperature of 15° C. or less in order to suppress the viscosity increase of the slurry.
  • MgO as a main component means that the content of MgO is 60 mass % or more with respect to the entire annealing separator.
  • the steel sheet coated with the annealing separator is wound into a coil, placed in an up-ended state, subjected to final annealing, secondary recrystallization, and a forsterite coating formed on the surface of the steel sheet. At this time, in order to prevent the outer winding of the coil from unwinding, it is desirable to wind a band or the like around the outer circumference of the coil.
  • the atmosphere in a part of the temperature range of 800° C. or higher including the purification treatment in which the temperature is kept at 1050 to 1300° C. for 3 hours or more is an atmosphere containing H 2 .
  • the steel sheet subjected to the above finish annealing is then washed with water, brushed, or pickled in order to remove the unreacted annealing separator. It is preferable to perform flattening annealing in order to reduce the
  • grain-oriented electrical steel sheets are often used by laminating steel sheets, and in order to ensure insulation in that case, it is preferable to coat the surface of the steel sheet with an insulating coating. It is preferable to employ a tension applying type for the insulating coating, which has an effect of reducing iron loss.
  • the insulating coating may be formed on the surface of the steel sheet by applying a coating liquid before flattening annealing and baking the steel sheet by flattening annealing, or by performing the above treatment on a separate line.
  • a tension-imparting insulation coating is formed via a binder, and inorganic substances are deposited on the surface of the steel sheet using physical vapor deposition or chemical vapor deposition.
  • a method of forming a coating may be employed.
  • grooves are formed on the surface of the steel sheet by etching or the like, or after forming an insulating coating, in one of the processes after cold rolling, heat such as laser or plasma is applied to the surface of the steel sheet.
  • the magnetic domain refining treatment may be performed by irradiating an energy beam to form a thermally strained region, or by pressing a roll having projections or the like against the steel sheet surface to form a work strained region.
  • a steel slab with a thickness of 220 mm was produced containing the various components shown in Table 3, with the balance being Fe and unavoidable impurities. It was extracted from the heating furnace, subjected to a width reduction process of 100 mm per side, and then subjected to horizontal rolling for flattening by correcting the dog-bone shape produced by the width reduction process. At this time, the amount of temperature drop at the width edge of the slab was varied by changing the contact time between the slab and the width reduction equipment. Table 4 shows the temperature Tc (° C.) at the center of the width of the slab after the width reduction and the horizontal rolling, the temperature Te (° C.) at the edge of the width, and the difference between Tc and Te (Tc ⁇ Te).
  • the steel slab was put into the heating furnace again, heated at 1400° C. for 20 minutes, subjected to rough hot rolling to obtain a sheet bar having a thickness of 50 mm, and further subjected to hot finish rolling to have a thickness of 2.8 mm.
  • After making a hot-rolled sheet it was water-cooled and wound into a coil at a temperature of 500°C.
  • both width edges of the hot-rolled sheet are continuously photographed inline, and from the images, the maximum width of edge cracks occurring at the width edges is measured. The results are shown in Table 4.
  • the hot-rolled sheet was soaked at 1000°C for 10 seconds, it was subjected to hot-rolled sheet annealing by water cooling from 800°C to 350°C at 20°C/s.
  • the first cold rolling was performed to make the intermediate sheet thickness 2.0 mm, and after soaking at 1100 ° C.
  • the intermediate thickness steel plate was pickled to remove surface scales, and then subjected to second cold rolling to obtain a cold-rolled steel plate having a final thickness of 0.23 mm.
  • the cold-rolled sheet is subjected to primary recrystallization annealing that also serves as decarburization annealing at 850° C. for 120 s in a moist atmosphere containing H 2 and N 2 with a dew point of 55° C., and then an annealing separator containing MgO as a main component. was applied to the surface of a steel plate at 8 g/m 2 per side, dried, and wound into a coil. After that, the steel sheet wound around the coil was subjected to secondary recrystallization, and then subjected to final annealing in which the steel sheet was held at a temperature of 1200° C. for 10 hours for purification.
  • primary recrystallization annealing that also serves as decarburization annealing at 850° C. for 120 s in a moist atmosphere containing H 2 and N 2 with a dew point of 55° C.
  • an annealing separator containing MgO as a main component was applied to the surface of
  • the atmosphere in the temperature range of 950° C. or higher was an atmosphere containing H 2 as the main component.
  • a phosphate-based tension imparting insulation coating is applied, and flattened annealing is performed to bake the coating and correct the shape of the steel sheet. was applied to make a product board.
  • the crystal orientation was measured by the SEM-EBSD method at both the front end and the tail end of the product coil thus obtained, and the maximum width of the secondary recrystallization defect part of each coil was obtained.
  • a test piece for measuring magnetic properties was taken from the entire width of the innermost and outermost windings of the product sheet coil with the rolling direction as the measurement direction, and the magnetic flux density B 8 at a magnetizing force of 800 A / m was measured according to JIS C2550- 1 (2011), and the value with the lowest magnetic flux density was taken as the in-coil guaranteed value.
  • the grain-oriented electrical steel sheets manufactured under the conditions suitable for the present invention using steel slabs having chemical compositions suitable for the present invention all have edge cracks suppressed to less than 10 mm.
  • the maximum width of the secondary recrystallization defect part at the sheet width end is suppressed to 5 mm or less, and the magnetic flux density B8 at the sheet end is also 1.93 T or more, which is good magnetic properties. Recognize.

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WO2025239047A1 (ja) * 2024-05-14 2025-11-20 Ｊｆｅスチール株式会社 方向性電磁鋼板の製造方法

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CN119640013B (zh) * 2024-12-18 2026-02-13 湖南华菱涟源钢铁有限公司 一种减少高磁感取向硅钢边裂的生产方法

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WO2025239047A1 (ja) * 2024-05-14 2025-11-20 Ｊｆｅスチール株式会社 方向性電磁鋼板の製造方法

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