WO2013175733A1 - Procédé de fabrication d'une tôle d'acier électrique à grains orientés - Google Patents

Procédé de fabrication d'une tôle d'acier électrique à grains orientés Download PDF

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WO2013175733A1
WO2013175733A1 PCT/JP2013/003091 JP2013003091W WO2013175733A1 WO 2013175733 A1 WO2013175733 A1 WO 2013175733A1 JP 2013003091 W JP2013003091 W JP 2013003091W WO 2013175733 A1 WO2013175733 A1 WO 2013175733A1
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Prior art keywords
annealing
steel sheet
electrical steel
grain
tension
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PCT/JP2013/003091
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English (en)
Japanese (ja)
Inventor
木島　剛
稔 高島
智幸 大久保
龍一 末廣
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Ｊｆｅスチール株式会社
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Priority to JP2014516655A priority Critical patent/JP5907257B2/ja
Publication of WO2013175733A1 publication Critical patent/WO2013175733A1/fr

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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
    • 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
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • 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
    • C22C38/60—Ferrous alloys, e.g. steel alloys containing lead, selenium, tellurium, or antimony, or more than 0.04% by weight of sulfur
    • 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
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/24—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing hexavalent chromium compounds
    • C23C22/33—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing hexavalent chromium compounds containing also phosphates
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/16—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of sheets
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0278—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips involving a particular surface treatment
    • C21D8/0289—Application of a tension-inducing coating

Definitions

  • the present invention relates to a method for producing a grain-oriented electrical steel sheet capable of improving iron loss by improving the steel sheet tension applied by the insulating coating.
  • the grain-oriented electrical steel sheet is mainly used as a core material of a transformer, and is particularly required to have a low iron loss.
  • One method for reducing this iron loss is to apply tension to the steel sheet after secondary recrystallization. According to this technique, by applying tension in the rolling direction to the steel sheet after the secondary recrystallization, the magnetic domain width is narrowed and the abnormal eddy current loss is reduced, so that the iron loss can be reduced.
  • the steel sheet after the secondary recrystallization is made of a material having a thermal expansion coefficient smaller than that of the steel sheet, which is mainly composed of crystalline oxide (for example, forsterite), amorphous oxide, nitride, and carbide at a high temperature.
  • a method for forming a coating film and applying tension to the steel sheet by the difference in thermal expansion coefficient between the coating film and the steel sheet has been proposed and industrialized.
  • Patent Document 1 uses a phosphate glass film
  • Patent Document 2 uses a titanium carbide film as the film as described above.
  • Patent Document 1 discloses that if the flattening annealing at 800 to 900 ° C. is performed after the application of the phosphate processing solution, the phosphate film baking and the flattening annealing can be performed simultaneously. .
  • phosphate glass is further applied on a forsterite film formed by finish annealing.
  • Patent Document 3 discloses an aqueous solution containing metal phosphate and silica as main components as a tension-providing insulating coating treatment liquid with a plate thickness average S concentration of 25 ppm or less as a finish annealing plate containing a forsterite coating.
  • the molar ratio of phosphoric acid to silica (P 2 0 5 / SiO 2 ) is 0.15 to 4.0, and the baking temperature is 900 ° C. to 1100 ° C. for 5 seconds to 600 seconds.
  • a method for manufacturing a grain-oriented electrical steel sheet is disclosed.
  • Patent Document 3 S is added as an inhibitor in steel in the steelmaking stage, and even if it is not positively added, it exists as an impurity in steel or in an annealing separator to some extent.
  • the above-mentioned S at the interface between the forsterite film and the iron base remains after the finish annealing, and even if it is not actively added, it exists in excess of 25 ppm. It will remain.
  • S existing at this interface diffuses and dissolves in the steel, and finely precipitates in the steel at the time of cooling after baking, thereby deteriorating iron loss. Therefore, as in Patent Document 3, regulating the upper limit of the S amount has a certain effect.
  • An object of the present invention is to provide a method for producing a grain-oriented electrical steel sheet excellent in iron loss.
  • the inventors have provided tension-insulating insulation without taking measures such as increasing the temperature of flattening annealing, which simultaneously causes factors that adversely affect iron loss, such as S diffusion into steel and deterioration of forsterite film tension.
  • a method for increasing the tension of the coating was explored. As a result, it was found that the tension of the tension-imparting insulating coating increases by rapidly cooling the average cooling rate from 800 ° C. to 500 ° C. to 20 ° C./s or more in the cooling after the flattening annealing. Further, it has been found that the effect of increasing the tension can be sufficiently obtained without performing the flattening annealing at a temperature as high as that of the conventional invention.
  • the present inventors performed a detailed study on the cause and estimated as follows. Due to the creep deformation of the steel plate during flattening annealing, the forsterite film is stretched and suffers slight damage. If the cooling rate after flattening annealing is increased in this state, thermal stress due to the difference in thermal expansion between steel and forsterite is suddenly applied, so that the forsterite film is destroyed. Therefore, in order to reduce the damage of the forsterite film due to creep deformation, it was newly found that the forsterite film can be prevented from being destroyed during the cooling process by reducing the flattening stress, that is, the stress in the furnace.
  • the present invention has been completed based on the above findings, and the gist of the present invention is as follows.
  • I. Directionality formed by applying flattening annealing to a directional electrical steel sheet having a forsterite film on the surface after finishing annealing by applying a treatment liquid of a tension-imparting type insulating film to the surface and baking it.
  • a method of manufacturing an electrical steel sheet (1) An aqueous solution containing a metal phosphate and silica and having a molar ratio of phosphoric acid to silica (P 2 O 5 / SiO 2 ) in the range of 0.15 to 4.0 as the treatment liquid for the tension applying insulating coating.
  • the average cooling rate from 800 ° C. to 500 ° C. in the cooling after the flattening annealing is 20 ° C./s or more
  • a method for producing a grain-oriented electrical steel sheet, wherein the stress in the furnace is in the range of 5 to 10 MPa.
  • the average cooling rate from 500 ° C. to 300 ° C. is set to 20 ° C./s or less.
  • the sheet thickness average S concentration of the grain-oriented electrical steel sheet having the forsterite film is 25 ppm or less, (5) The method for producing a grain-oriented electrical steel sheet according to the above I or II, wherein the flattening annealing temperature is 840 ° C. or higher.
  • a method for producing a grain-oriented electrical steel sheet according to any one of I to III Further, a steel slab containing Si: 2.0 to 5.0% by mass is hot-rolled and subjected to hot-rolled sheet annealing, and then cold-rolled once or twice with intermediate annealing, and then decarburized.
  • Annealing if necessary, performing a nitriding treatment, and after applying and drying an annealing separator mainly composed of magnesia, comprising a series of steps for performing the above-mentioned finish annealing and flattening annealing,
  • a method for producing a grain-oriented electrical steel sheet characterized in that when a strip rolled to a final thickness is subjected to decarburization annealing, a temperature rise from 500 ° C to 700 ° C is performed at a temperature rise rate of 50 to 300 ° C / sec.
  • the iron loss of the grain-oriented electrical steel sheet can be improved by increasing the tension of the tension-imparting insulating coating formed on the steel sheet surface.
  • the present invention applies a flattening annealing to a grain-oriented electrical steel sheet having a forsterite film on the surface after finish annealing, applying a treatment liquid of a tension-imparting type insulating film on the surface and performing baking together with the flattening. It is a manufacturing method of the grain-oriented electrical steel sheet.
  • the treatment liquid for the tension-imparting insulating coating is an aqueous solution containing a metal phosphate and silica, and the molar ratio of phosphoric acid to silica (P 2 0 5 / SiO 2 ) is in the range of 0.15 to 4.0. It needs to be adjusted. The reason is that, when (P 2 0 5 / SiO 2 ) is less than 0.15 or more than 4.0, the tension generated by the coating is reduced, and a desired iron loss cannot be obtained.
  • this film processing liquid is baked with planarization annealing.
  • the baking temperature it can be carried out in a temperature range of about 800 to 900 ° C., for example.
  • planarization annealing is performed at a temperature of 900 ° C. or higher, it becomes difficult to control the creep amount of the base iron, and it becomes difficult to stably obtain the effects of the invention.
  • tension-imparting insulating coating conventionally known ones can be applied, but metal phosphates such as aluminum phosphate, magnesium phosphate, barium phosphate, strontium phosphate, iron phosphate or zinc phosphate, and silica
  • metal phosphates such as aluminum phosphate, magnesium phosphate, barium phosphate, strontium phosphate, iron phosphate or zinc phosphate
  • silica A vitreous tension insulating film mainly composed of In addition to the metal phosphate and silica, chromic acid, chromic anhydride, chromate, and other additives can be added to the tension-imparting insulating coating in addition to metal phosphate and silica.
  • the film thickness of the tension applying insulating film is preferably about 1 to 5 ⁇ m.
  • the grain-oriented electrical steel sheet in the present invention is not particularly limited in its components, and all conventionally known ones are suitable.
  • the manufacturing method according to the present invention it is desirable to use a slab containing Si: 2.0 to 5.0% by mass as the material of the grain-oriented electrical steel sheet from the viewpoint of iron loss improvement.
  • Si is less than 2.0% by mass, the effect of improving iron loss is small, and when Si exceeds 5.0% by mass, rolling may be difficult.
  • the inhibitor component is not particularly limited, and known inhibitors such as AlN, BN, TiN, MnS, MnSe, Sn, Sb, and Bi can be used. These may be added at the steel making stage, or may be added by performing nitriding treatment or the like in a subsequent process.
  • the slab obtained by casting is hot-rolled, subjected to hot-rolled sheet annealing, and then cold-rolled twice or once with intermediate annealing, and then decarburized annealing.
  • a series of steps of performing the above-described finish annealing and flattening annealing after performing nitriding treatment as necessary, applying and drying an annealing separator mainly composed of magnesia, can be further provided.
  • conventionally known conditions can be used, but when decarburizing and annealing a strip that has been rolled to the final plate thickness, the heating rate from 500 ° C. to 700 ° C. is set to 50 to 300 ° C./sec. This is particularly effective from the viewpoint of iron loss improvement.
  • the heating rate of decarburization annealing is 50 to 300 ° C / sec
  • the Goss orientation of the primary recrystallization texture increases and the grain size after secondary recrystallization decreases.
  • the secondary recrystallized grain size is reduced, the demagnetizing effect at the grain boundaries is increased and the magnetic domain width is narrowed. Therefore, when the coating tension is increased, a more excellent iron loss can be obtained. If it is less than 50 ° C./sec, the effect is small, and if it exceeds 300 ° C./sec, the iron loss deteriorates, so 50 to 300 ° C./sec is preferable.
  • magnesia (MgO) and principal can be as, advantageously adapt those including TiO 2, MgSO 4, SrSO 4 .
  • S may be added as an inhibitor in steel at the steel making stage, or may be added as a sulfide to the annealing separator.
  • it exists to some extent as an impurity in steel and magnesia.
  • Such S concentrates at the forsterite film / steel interface after finish annealing and may exist in excess of 25 ppm even if it is not actively added, and if it is actively added, it will remain in a larger amount. . And, when the temperature in flattening annealing becomes high, S existing at this interface diffuses and dissolves in the steel, and finely precipitates in the steel at the time of cooling after baking, thereby deteriorating iron loss. it is conceivable that.
  • the plate thickness average S concentration of the finish annealed plate including the forsterite coating is 25 ppm or less.
  • the plate thickness average S concentration is an average value of S concentration at each position of the plate thickness, and a plate before coating application is used, or a plate obtained by removing the coating of the product plate with boiling alkali or the like. And can be calculated by performing a wet analysis.
  • the present invention applies a treatment liquid of a tension-imparting type insulating coating to a grain-oriented electrical steel sheet having a forsterite coating on the surface after finish annealing and performs baking together with flattening. It is important to increase the average cooling rate from °C to 500 °C to 20 °C / s or more.
  • the temperature from 800 ° C. to 500 ° C. in the cooling is a temperature region where the glass transition point of the tension-imparting insulating coating exists, and it is estimated that the tension of the insulating coating increases by rapidly cooling this temperature region. In the cooling, the average cooling rate from 800 ° C. to 500 ° C.
  • the tension of the tension-imparting film cannot be sufficiently improved, so that a desired iron loss cannot be obtained.
  • the upper limit is 120 ° C. / S or less is preferable.
  • a more preferable cooling rate range is 40 to 120 ° C./s, and a further preferable range is 60 to 120 ° C./s.
  • the cooling rate at 500 ° C. or less for the cooling is not particularly limited, but the temperature region from 500 ° C. to 300 ° C. is a region where the yield stress of steel changes rapidly, and this temperature region is gradually cooled. By doing so, it is considered that the residual distortion due to the cooling unevenness is effectively reduced and the deterioration of the iron loss can be suppressed.
  • the average cooling rate in the temperature range from 500 ° C. to 300 ° C. is preferably 20 ° C./s or less, and more preferably 10 ° C./s or less. When the cooling rate is less than 0.1 ° C./s, it takes too much time for cooling, which is not preferable from the viewpoint of manufacturing cost.
  • the stress in the furnace is in the range of 5 to 10 MPa. This is because it is possible to suppress the deterioration of the forsterite film due to the creep deformation of the base iron while performing the flattening treatment of the grain-oriented electrical steel sheet after the finish annealing, and it is preferable that the range be 6 to 8 MPa. .
  • the in-furnace stress is less than 5 MPa, the grain-oriented electrical steel sheet cannot be sufficiently flattened, and when the in-furnace stress exceeds 10 MPa, the stress is too large and the forsterite is deteriorated.
  • the prepared coating chemical was applied to a finish annealing plate with a bar coater, pre-baked at 300 ° C., and then flattened. About the fabric weight, it adjusted so that the coating film thickness after planarization annealing might be set to 2 micrometers. Unless otherwise specified, the soaking temperature of flattening annealing was 820 ° C., and the soaking time was constant for 15 seconds.
  • FIG. 1 is a graph showing the tension of a phosphate glass film when the average cooling rate in the temperature range from 800 ° C. to 500 ° C. after baking of the phosphate glass coating is changed.
  • the cooling rate from 500 ° C to 300 ° C was constant at 20 ° C / sec. It can be seen from FIG. 1 that the tension of the phosphate glass coating film can be increased by quenching the cooling rate regardless of the furnace stress. In particular, it can be seen that a high film tension is obtained at a cooling rate of 20 ° C./s or more.
  • FIG. 2 shows the forsterite film tension when the average cooling rate in the temperature region from 800 ° C. to 500 ° C. after baking the phosphate glass coating is changed.
  • the cooling rate from 500 ° C to 300 ° C was constant at 20 ° C / sec.
  • FIG. 2 shows that the forsterite film tension deteriorates by rapidly cooling the cooling rate and increasing the stress in the furnace.
  • FIG. 3 shows the total film tension when the average cooling rate in the temperature range from 800 ° C. to 500 ° C. after baking the phosphate glass coating is changed.
  • the cooling rate from 500 to 300 ° C was constant at 20 ° C / sec.
  • the total film tension is the sum of the phosphate glass film tension and the forsterite film tension.
  • FIG. 3 shows that the total film tension tends to increase by rapidly cooling the average cooling rate in the temperature range from 800 ° C. to 500 ° C. Furthermore, it can be seen that the film tension is more effectively increased by reducing the stress in the furnace.
  • the film tension in FIGS. 1, 2 and 3 is a value calculated from the amount of warpage of the steel sheet when one side of the film is completely removed.
  • Figure 4 shows a test in which the cooling rate from 800 ° C to 500 ° C after baking the phosphate glass coating was set to two levels of 10 ° C / sec and 80 ° C / sec, and the cooling rate from 500 ° C to 300 ° C was changed. It shows about the result of measuring the iron loss (W 17/50 ) of a piece.
  • the stress in the furnace was 6 MPa.
  • the iron loss was improved by rapidly cooling the temperature range from 800 ° C. to 500 ° C.
  • the iron loss was further improved by reducing the cooling rate from 500 ° C to 300 ° C under conditions of rapid cooling from 800 ° C to 500 ° C.
  • the cooling rate from 500 ° C. to 300 ° C. had little effect on the film tension.
  • FIG. 5 shows the relationship between the flattening annealing temperature and the iron loss (W 17/50 ) in test pieces having various sheet thickness average S concentrations.
  • 0.23 mm thick directional electrical steel sheet coils with a forsterite coating that has been subjected to finish re-annealing and secondary recrystallization containing 3.3% Si was manufactured by adjusting the amount of magnesium sulfate added to the annealing separator and adjusting the sheet thickness average S concentration of the grain-oriented electrical steel sheet having a forsterite coating.
  • the cooling rate from 800 ° C. to 500 ° C. was 80 ° C./sec
  • the iron loss improvement allowance when the flattening annealing temperature is 840 ° C. or higher is larger as the S concentration is lower.
  • the iron loss improvement allowance is greater when the S concentration is 25 ppm or less. It was. That is, it is understood that particularly excellent iron loss can be obtained by setting the plate thickness average S concentration to 25 ppm or less and the planarization annealing temperature to 840 ° C. or more. That is, in the present invention, the iron loss improvement effect can be obtained without performing high-temperature annealing at 900 ° C. or higher.
  • the plate thickness average S concentration of the finish annealed plate including the forsterite film of the finish annealed plate was 25 ppm or less.
  • Apply a tension-providing insulating coating treatment solution containing metal phosphate and colloidal silica and bake at 840 ° C to form a tension-providing insulating coating.
  • planarization annealing was performed. Table 1 shows the molar ratio of phosphoric acid and silica (P 2 0 5 / SiO 2 ) in the treatment liquid and the stress in the furnace during flattening annealing.
  • cooling was performed at a cooling rate from 800 ° C. to 500 ° C. at the cooling rate shown in Table 1 to obtain grain-oriented electrical steel sheets for each sample.
  • the cooling rate from 500 ° C. to 300 ° C. was constant at 20 ° C./sec.
  • each sample according to the inventive example has a lower iron loss than the sample according to the comparative example and shows a good result. This is because the tension of the forsterite coating and the tension-imparting insulating coating is improved by optimizing the cooling rate and the furnace tension.
  • Table 2 shows the thickness average S concentration of the finish annealed plate including the forsterite coating.
  • the plate thickness average S concentration is changed by adjusting the amount of magnesium sulfate added to the annealing separator and changing the S concentration.
  • the temperature increase rate from 500 ° C. to 700 ° C. in the temperature increase process of decarburization annealing was set to 100 ° C./sec.
  • a magnesium phosphate aqueous solution and colloidal silica were mixed at a molar ratio of phosphoric acid to silica (P 2 0 5 / SiO 2 ) of 0.5, and chromic acid and phosphoric acid.
  • a chemical solution prepared by adding chromic anhydride so that the molar ratio (Cr 2 O 3 / P 2 0 5 ) was 0.3 was applied, and flattening annealing was performed at a soaking temperature and a cooling rate shown in Table 2.
  • the in-furnace stress of the flattening annealing was 8 MPa.
  • each sample according to the inventive example has a lower iron loss than the sample according to the comparative example.
  • the plate thickness average S concentration is low and the flattening annealing temperature is high.
  • a directional electrical steel sheet with a forsterite film was prepared by subjecting to finish annealing at 1200 ° C. for 5 hours.
  • the plate thickness average S concentration of the finish annealed plate including the forsterite film of the finish annealed plate was 25 ppm or less.
  • the rate of temperature increase from 500 ° C. to 700 ° C. in the temperature increase process of decarburization annealing was set to the values shown in Table 3.
  • a magnesium phosphate aqueous solution and colloidal silica were added in a molar ratio of phosphoric acid to silica (P 2 0 5 / SiO 2 ) of 0.45, and chromic acid and phosphoric acid.
  • the stress in the furnace for flattening annealing was 7 MPa
  • the cooling rate from 500 ° C. to 300 ° C. was 20 ° C./s.
  • each sample according to the inventive example has a lower iron loss than the sample according to the comparative example and shows a good result.
  • the present invention it is possible to provide a method for producing a grain-oriented electrical steel sheet that can improve the iron loss by improving the tension of the tension-imparting type insulation coating, and has a remarkable industrial effect.

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Abstract

La présente invention aborde le problème consistant à fournir une tôle d'acier électrique à grains orientés qui possède un film isolant du type communiquant une tension ayant une tension renforcée sur sa surface et qui affiche une perte de fer améliorée. Afin de résoudre le problème, la présente invention propose un procédé de fabrication d'une tôle d'acier électrique à grains orientés, ledit procédé comprenant : l'application d'un fluide de traitement pour former un film isolant du type communiquant une tension à la surface d'une tôle d'acier électrique à grains orientés qui possède un film de forstérite sur sa surface et qui a subi un recuit final ; et la soumission de la tôle d'acier résultante à un processus de recuit d'aplanissement, la cuisson du fluide de traitement et l'aplatissement de la tôle étant conduits simultanément. En outre, le procédé est caractérisé par l'ajustement correct (1) du fluide de traitement pour former un film isolant du type communiquant une tension, (2) la vitesse moyenne de refroidissement de 800 °C à 500 °C lors du refroidissement réalisé après le processus de recuit d'aplanissement, et (3) la contrainte dans un four.
PCT/JP2013/003091 2012-05-24 2013-05-15 Procédé de fabrication d'une tôle d'acier électrique à grains orientés WO2013175733A1 (fr)

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Cited By (9)

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JP2021075769A (ja) * 2019-11-12 2021-05-20 日本製鉄株式会社 方向性電磁鋼板及び方向性電磁鋼板の製造方法
CN113073177A (zh) * 2021-03-17 2021-07-06 武汉钢铁有限公司 改善取向钢氧化层组分的控制方法
CN113302337A (zh) * 2019-01-16 2021-08-24 日本制铁株式会社 方向性电磁钢板及其制造方法
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JP6323625B1 (ja) * 2016-08-30 2018-05-16 Ｊｆｅスチール株式会社 被膜付金属、被膜形成用処理液及び被膜付金属の製造方法
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JP2019019358A (ja) * 2017-07-13 2019-02-07 新日鐵住金株式会社 皮膜密着性に優れる一方向性電磁鋼板及びその製造方法
WO2019181952A1 (fr) 2018-03-20 2019-09-26 日本製鉄株式会社 Procédé de production d'une tôle d'acier magnétique à grains orientés, et tôle d'acier magnétique à grains orientés
KR20200123471A (ko) 2018-03-20 2020-10-29 닛폰세이테츠 가부시키가이샤 방향성 전자 강판의 제조 방법 및 방향성 전자 강판
US11661636B2 (en) 2018-03-20 2023-05-30 Nippon Steel Corporation Method for manufacturing grain-oriented electrical steel sheet and grain-oriented electrical steel sheet
JP7265186B2 (ja) 2018-12-28 2023-04-26 日本製鉄株式会社 方向性電磁鋼板及びその製造方法
JPWO2020138069A1 (ja) * 2018-12-28 2021-11-11 日本製鉄株式会社 方向性電磁鋼板及びその製造方法
EP3904557A4 (fr) * 2018-12-28 2022-09-14 Nippon Steel Corporation Tôle magnétique en acier à grains orientés et son procédé de fabrication
RU2779985C1 (ru) * 2018-12-28 2022-09-16 Ниппон Стил Корпорейшн Лист анизотропной электротехнической стали и способ его производства
WO2020138069A1 (fr) * 2018-12-28 2020-07-02 日本製鉄株式会社 Tôle magnétique en acier à grains orientés et son procédé de fabrication
US12031191B2 (en) 2018-12-28 2024-07-09 Nippon Steel Corporation Grain-oriented electrical steel sheet and method for manufacturing same
CN113302337A (zh) * 2019-01-16 2021-08-24 日本制铁株式会社 方向性电磁钢板及其制造方法
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JP2021075769A (ja) * 2019-11-12 2021-05-20 日本製鉄株式会社 方向性電磁鋼板及び方向性電磁鋼板の製造方法
JP7356017B2 (ja) 2019-11-12 2023-10-04 日本製鉄株式会社 方向性電磁鋼板及び方向性電磁鋼板の製造方法
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