EP0912768B1 - Procede de fabrication d'une tole d'acier electrique a grains orientes pour la fabrication notamment de circuits magnetiques de transformateurs - Google Patents

Procede de fabrication d'une tole d'acier electrique a grains orientes pour la fabrication notamment de circuits magnetiques de transformateurs Download PDF

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EP0912768B1
EP0912768B1 EP98914939A EP98914939A EP0912768B1 EP 0912768 B1 EP0912768 B1 EP 0912768B1 EP 98914939 A EP98914939 A EP 98914939A EP 98914939 A EP98914939 A EP 98914939A EP 0912768 B1 EP0912768 B1 EP 0912768B1
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Prior art keywords
annealing
hot
strip
sheet
precipitated
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German (de)
English (en)
French (fr)
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EP0912768A1 (fr
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Jean-Claude Bavay
Jacques Castel
Freddy Messeant
Philippe Martin
Frédéric Mazurier
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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
    • 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
    • C21D8/1216—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the working step(s) being of interest
    • C21D8/1222—Hot rolling
    • 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
    • C21D8/1261—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 following hot rolling
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1205—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties involving a particular fabrication or treatment of ingot or slab
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1277—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties involving a particular surface treatment
    • C21D8/1288—Application of a tension-inducing coating

Definitions

  • the texture ⁇ 110 ⁇ ⁇ 001> whereby the axes ⁇ 001>, which are axes of easy magnetization, are substantially parallel to the rolling direction and the ⁇ 110 ⁇ planes are substantially parallel to the surface of the sheet, giving the grain electrical steel sheets oriented with good magnetic properties in the rolling direction.
  • the fine precipitates MnS, AIN and CuS alone or in combination, of mean diameter less than 100 nm are growth inhibitors normal of primary grains not having the orientation ⁇ 110 ⁇ ⁇ 001>.
  • the redissolution of the AIN precipitates during reheating of the slab is incomplete, nitriding of the sheet decarburized being carried out to form the main inhibitor (Al, Si) N under forms fine particles before the start of secondary recrystallization.
  • the sulfur content is limited and less than 0.012%.
  • Aluminum nitrides AIN are only redissolved in one low proportion and also do not participate in inhibition since they are in the form of coarse particles in the hot-rolled sheet, in one amount equal to at least 60% of the total nitrogen content.
  • the inhibition is essentially carried out by the fine particles of copper sulfide which are formed during the annealing of the rolled sheet to hot.
  • the precipitates containing sulfur and / or nitrogen are redissolved during the reheating of the slab as a result of the adaptation of the chemical composition: sulfur ⁇ 0.020%, aluminum ⁇ 0.030%, [(% S) x (% Mn)] ⁇ 160.10 -5 and [(% Al) x (% N)] ⁇ 240.10 -6 .
  • the steel is hot rolled in order to precipitate the whole sulfur in the form of fine particles.
  • the steel is hot rolled so that do not precipitate nitrogen as fine AIN particles.
  • steel hot-rolled is annealed to precipitate nitrogen in the form of fine AIN particles which constitute the main inhibitor.
  • magnesia used as an annealing separator can be added to the magnesia used as an annealing separator at least one sulfur and / or nitrogen compound which allows additional inhibition.
  • the object of the present invention in accordance with claim 1 is to manufacture an electric steel sheet grain oriented ensuring improved magnetic quality sheet metal when the slab or strip is reheated at a temperature below 1350 ° C before hot rolling.
  • the invention also relates to an electric grain steel sheet oriented, obtained by the process.
  • FIG. 1 shows the mass percentage of non-precipitated sulfur, in the form of coarse particles with a diameter greater than or equal to 300 nm, hot rolled sheet before annealing, as shown on the curve A and hot-rolled sheet after annealing, as shown in the curve B, the mass percentage of non-precipitated sulfur being a function of the percentage by mass of the total sulfur contained in the reheated slab at 1300 ° C.
  • Figures 2a, 2b, 2c show the magnetic characteristics of sheet metal, sheet metal to the final thickness 0.285mm after cold rolling, coated an insulating coating inducing a tensile stress, the slab having been heated to 1300 ° C, depending on the mass percentage of sulfur not precipitated as coarse particles of equal diameter or greater than 300 nm from the hot-rolled sheet before annealing.
  • Figure 3 shows the B800 induction of the final product at thickness 0.285 mm after cold rolling as a function of the annealing temperature the hot rolled sheet, the slab having been reheated to 1300 ° C.
  • Figure 4 shows the average diameter, in microns, of the grain after the primary recrystallization and decarburization annealing depending on the mass percentage of the sulfur of the slab reheated to 1300 ° C, the thickness of the hot rolled strip being 2.3 mm and 2 mm.
  • FIG. 5 presents the magnetic characteristics of the final product, to the thickness 0.285 mm, depending on the percentage of grains having a diameter greater than 15 ⁇ m, after primary recrystallization annealing and decarburization, the heating of the slab being carried out at 1300 ° C.
  • Figures 6a, 6b, 6c show the magnetic characteristics of the final product, thickness 0.285 mm, depending on the percentage of grains having a diameter less than 5 ⁇ m, after primary recrystallization annealing and decarburization, the heating of the slab being carried out at 1300 ° C.
  • Figure 7 shows the losses at 1.7 T and 50 Hz of the final product, at the thickness 0.285 mm, depending on the percentage by weight of aluminum soluble in the slab reheated to 1300 ° C.
  • Figures 8a, 8b, 8c show the magnetic characteristics of the final product at the thickness 0.285 mm as a function of the mass percentage in tin of the slab reheated to 1300 ° C and the mass percentage l of the non-precipitated sulfur in the form of coarse particles of equal diameter or greater than 300 nm, hot-rolled sheet before annealing.
  • fine particles particles the average diameter of which is less than 300 nm, most of these particles with an average diameter less than 100 nm, per particle coarse, particles whose average diameter is equal to or greater than 300 nm, and in particular by non-precipitated sulfur in the form of particles coarse, sulfur precipitated mainly as fine particles the majority of which have an average diameter of less than 100 nm and sulfur in solid solution.
  • the mass percentage l of non-precipitated sulfur in the form of coarse particles from hot rolled sheet is equal to the difference between the mass percentage of total sulfur in the steel slab, determined by chemical analysis, and the mass percentage of sulfur precipitated under coarse particle form of hot-rolled sheet, determined at Electronique scanning microscope. In order to eliminate artifacts from detection, only precipitates containing sulfur of equal average diameter or greater than 300 nm have been taken into account. Crossings in the fields contiguous were made on a micrographic section, from the upper side on the underside of the sheet, with a magnification of 1000 and with a electron acceleration voltage of 15 kV. The area fraction of sulfur-containing precipitates is equal to the total area of the precipitates containing sulfur over the total area examined.
  • the fraction surface area of the precipitates is equal to the volume fraction of the precipitates.
  • Hot roughing and finishing laminates are made in continuous, by successive passage in, for example, the twelve cages of a rolling mill, the successive reduction rates being 21, 39, 20 25 and 25% for roughing rolling and 53, 38, 43, 38, 26, 18 and 4% for the finish rolling.
  • 2.3mm thick hot rolled sheet is wound at a temperature between 510 ° C and 540 ° C.
  • Hot rolled sheet metal annealing is carried out with a temperature rise of 1100 ° C in 100 seconds, maintaining 1100 ° C for 160 seconds, cooling to 800 ° C in 30 seconds and quenching at 65 ° C in 10 seconds.
  • the hot rolled and annealed sheet is then subjected to rolling cold to the thickness of 0.285 mm in a step comprising six passes corresponding to successive reduction rates of approximately 30% and at an overall reduction rate of 87.6%, the rolling temperature exceeding 150 ° C for at least one pass.
  • the cold-rolled sheet is subjected to a primary recrystallization and to a decarburization comprising in particular a rise to the temperature of 700 ° C in approximately 15 seconds, a rise from 700 ° C to 820 ° C in approximately 100 seconds, a holding at 820 ° C for 40 seconds in a humid N 2 / H 2 atmosphere.
  • the decarburized sheet is coated with a milk of magnesia containing 150 g of MgO magnesia per liter of water, 6 g of TiO 2 per 100 g of MgO, 0.04% of antimony chloride per 100 g of MgO, and dried .
  • the decarburized sheet coated with magnesia is then subjected to a secondary recrystallization annealing with a temperature rise of 15 ° C / h, under an atmosphere 25% N 2 - 75% H 2 , between 650 ° C and 1200 ° C and a maintenance at 12.00 ° C under hydrogen until complete purification of the metal in S and N.
  • Curve A in Figure 1 shows, unpredictably, that under the heating conditions at 1300 ° C of the pouring slab continuous and hot rolling according to the invention, the mass percentage non-precipitated sulfur in the form of coarse sheet metal particles hot rolled not annealed increases when the mass percentage of the total sulfur in the slab increases.
  • the No. 1 steel slab with the lowest percentage of total sulfur. 0.011%, and which does not contain a voluntary addition of tin leads to a end product characterized by poor magnetic quality, the mass percentage of non-precipitated sulfur in the form of particles coarse with an average diameter equal to or greater than 300 nm being of 0.0055% in hot rolled sheet.
  • Steel No. 2 the slab of which contains 0.015% total sulfur and of which the hot-rolled sheet has a mass percentage of sulfur not precipitated as coarse particles greater than 0.006%, has a slightly lower magnetic quality than that of steels 3, 4 and 5, of which hot rolled sheets are characterized by a mass percentage higher non-precipitated sulfur as coarse particles.
  • the Figure 3 shows, the slab having been heated to 1300 ° C, as soon as we strongly deviates from the optimal annealing temperature, close to 1100 ° C., hot-rolled sheet corresponding to steel No. 2, the quality magnetic representation by the B800 induction is strongly degraded, in particular when the annealing temperature is equal to 1050 and 1150 ° C., the thickness of the final product being 0.285 mm after cold rolling.
  • a steel slab n ° 3 was reheated in another example, at core, at 1250 ° C, the core of the slab 210 mm thick being maintained 45 minutes above 1200 ° C, including 32 minutes above at 1230 ° C.
  • the end temperature of hot rolling of roughing is 1075 ° C
  • the temperature at which hot rolling begins finish temperature is 1030 ° C
  • the end temperature of the hot rolling of finish is 950 ° C
  • the winding temperature is 525 ° C.
  • Annealing hot rolled sheet was made at 1100 ° C for 160 seconds, with the temperature rise and cooling conditions already described.
  • l mass percentage of sulfur not precipitated as coarse particles with a diameter equal to or greater than 300 nm, in hot rolled sheet.
  • a reheat time of the slab or strip longer allows to increase, in hot rolled sheet or in band, the mass percentage of non-precipitated sulfur as coarse particles with a diameter of 300 nm or more. So the the core of a steel slab n ° 3 was heated to 1300 ° C in the following conditions: maintenance of 65 minutes above 1250 ° C, of which 45 minutes above 1280 ° C. Under these conditions, the percentage mass l of the non-precipitated sulfur in the form of coarse particles is 0.013% in hot-rolled sheet, instead of 0.008% (Table 2).
  • Annealing of the hot-rolled sheet according to the invention must be carried out under conditions such that there is no increase in the percentage of the sulfur precipitated as coarse particles of equal mean diameter or greater than 300 nm.
  • the annealing conditions according to the invention must favor the partial dissolution of precipitates of equal average diameter or greater than 300 nm and precipitation of sulfur in solid solution, at cooling, in the form of fine particles of smaller average diameter at 100 nm.
  • Curve B in Figure 1 shows examples, according to the invention, the percentage by mass of sulfur not precipitated in the form of coarse particles with an average diameter equal to or greater than 300 nm, i.e. in solid solution and precipitated essentially in the form of fine particles with an average diameter of less than 100 nm, after annealing the hot rolled sheet.
  • the mass percentage of sulfur in solid solution and precipitated in the form of fine particles, after annealing the rolled sheet to hot is greater than 0.010% for steels 3, 4 and 5.
  • the method according to the invention allows the precipitation of sulfur in solid solution in the form of fine particles of average diameter less than 100 nm during the annealing carried out before or / and after the first cold rolling, during decarburization annealing, during secondary recrystallization annealing and in particular before the start of the secondary recrystallization.
  • the annealing of the hot-rolled sheet or strip, according to the invention, must also be carried out under conditions such that there is significant precipitation of nitrogen, with more than 60% of the mass percentage of nitrogen. total, in the form of fine particles with an average diameter less than or equal to 100 nm.
  • Mass percentage of nitrogen precipitated in the AIN state in the hot-rolled strip Reheating temperature N of AIN (10 -4 %) Steel 1 1250 ° C 6 Steel 1 1300 ° C 2 Steel 2 1250 ° C 8 Steel 2 1300 ° C 4 Steel 3 1250 ° C 14 Steel 3 1300 ° C 4 Steel 4 1300 ° C 9 Steel 5 1300 ° C 8
  • the principle of the method for measuring the percentage by mass of precipitated nitrogen is as follows: dissolving the matrix using a bromine-methanol mixture, separation of the precipitated aluminum by filtration through a membrane, dissolution of aluminum nitride by dilute sodium hydroxide, determination of aluminum by ICP emission spectrometry and calculation of the corresponding nitrogen.
  • Mass percentage of nitrogen precipitated in the AIN state after annealing of the hot-rolled strip Reheating temperature N of AIN (10 -4 %) Steel 1 1250 ° C 50 Steel 1 1300 ° C 55 Steel 2 1250 ° C - Steel 2 1300 ° C 58 Steel 3 1250 ° C 50 Steel 3 1300 ° C 53 Steel 4 1300 ° C 57 Steel 5 1300 ° C 56
  • Tables 3 and 4 show typical percentage values mass of nitrogen precipitated before and after annealing the hot rolled sheet. It has been verified by transmission electron microscopy that the diameter mean nitrogen-containing particles is less than 100 nm, before and after annealing the hot rolled sheet.
  • annealing the rolled sheet hot or tape simultaneously promoting the decrease in mass percentage of sulfur precipitated as coarse particles of average diameter equal to or greater than 300 nm and the precipitation of nitrogen in the form of fine AIN particles, alone or combined with sulfur, average diameter less than 100 nm.
  • the above examples correspond to an annealing cycle, according to the invention, comprising the rise in temperature, maintaining at a given temperature and cooling rapid, and in particular comprising maintaining between 900 ° C and 1150 ° C of minus 50 seconds.
  • More complex cycles can be used, for example a temperature rise to 800 ° C in 50 seconds, from 800 ° C to 1100 ° C in 40 seconds, a 50 second hold between 1100 ° C and 1125 ° C, cooling from 1125 ° C to 900 ° C in 30 seconds, holding at 900 ° C for 160 seconds, cooling from 900 ° C to 100 ° C in less than 40 seconds.
  • losses at 1.7 Tesla and 50 Hz of 1.01 W / kg, losses at 1.5 Tesla and 50 Hz of 0.75 W / kg and a B800 induction of 1.94 Tesla were obtained from a No. 3 steel slab reheated to 1300 ° C for a final thickness of 0.285 mm after cold rolling in a step, the final product being coated with an inducing insulating coating tensile stress.
  • Figures 2a, 2b, 2c show an example of characteristics magnetic of the final product to the thickness 0.285 mm after cold rolling in one step, coated with an insulating coating inducing a stress traction: energy losses W (1.5 / 50), W (1.7 / 50) in Watt / kg at one frequency of 50 Hz and for a work induction of 1.5 respectively Tesla and 1.7 Tesla and B800 induction acquired under a magnetic field of 800 A / m depending on the percentage by mass of sulfur not precipitated under form of coarse particles of the hot-rolled sheet (before annealing), the slab having been reheated to 1300 ° C.
  • a reduction rate at cold above 70%, before the primary recrystallization annealing and decarburization provides a B800 induction greater than 1.84 Tesia and may exceed 1.90 Tesla if the mass percentage of sulfur not precipitated as coarse particles of equal average diameter or greater than 300 nm is greater than 0.006% before annealing primary recrystallization and decarburization.
  • cold rolling will preferably be carried out in two stages, with a intermediate annealing.
  • a reduction rate in the second rolling step at cold, after intermediate annealing, greater than 70% provides a B800 induction greater than 1.84 Tesla and possibly exceeding 1.90 Tesla if, in hot-rolled sheet, the mass percentage l of sulfur not precipitate in the form of coarse particles is greater than 0.006%, the slab containing less than 0.08% tin.
  • Annealing hot rolled sheet or strip before rolling cold in one step and intermediate annealing before the second rolling to cold in a two-stage cold rolling include a hold at least 50 seconds between 900 ° C and 1150 ° C, followed by a rapid cooling.
  • the rolled sheet hot or the strip may be annealed before the first rolling at cold.
  • Such annealing promotes obtaining a good magnetic quality.
  • This annealing includes maintaining at least 50 seconds between 900 ° C and 11 50 ° C, followed by rapid cooling. It contributes to the solution partial coarse particles containing sulfur and precipitation fine particles containing sulfur or (and) nitrogen. In no case does it must lead to the formation of coarse particles containing sulfur and or nitrogen.
  • the sheet is maintained at a temperature above 150 ° C for at least one passes from the cold rolling stage preceding the recrystallization annealing primary and decarburization, cold rolling taking place in one or two steps. Raising the temperature of the sheet above 150 ° C during several passes promotes good quality magnetic, especially if the cold reduction rate is greater than 70%.
  • the non-precipitated sulfur in the form of coarse particles influences the grain size formed by primary recrystallization, the mean grain diameter after primary recrystallization and decarburization being according to the invention less than 15 microns.
  • the conditions according to the invention are not met, and especially when the mass percentage of sulfur not precipitated under coarse particle form is less than 0.006% before annealing primary recrystallization and decarburization, some primary grains have a diameter greater than 15 microns due to a quantity insufficient sulfur in solid solution and precipitated as fines particles with an average diameter of less than 100 nm. It follows a bad secondary recrystallization and degradation of the magnetic quality.
  • the Figure 4 shows the influence of the mass percentage of sulfur in the slab on the average diameter expressed in ⁇ m of the grain after annealing primary recrystallization and decarburization.
  • the average grain diameter primary decreases when the mass percentage of total sulfur in the slab increases.
  • the average grain diameter primary changes little as a function of the mass percentage of the total sulfur of the slab which is linked to the mass percentage of sulfur not precipitated under form of coarse particles with an average diameter of 300 or more nm of the hot rolled sheet by the relation of figure 1.
  • the use of a thickness of the laminated strip 2 mm hot appears preferable to improve the magnetic quality.
  • the improvement is 6%, 5% and 1% respectively for the losses and the B800 when the thickness of the hot rolled strip is 2 mm rather than 2.3 mm, cold rolling being carried out in one step.
  • Figures 5 and 6 show that, in the case of the example above, for thicknesses of hot and cold rolled strips 2.00 mm and 0.285 mm respectively, the best quality magnetic, losses at 1.5 T and 1.7 T the lowest and B800 the highest, is obtained when the percentage of primary grains in diameter greater than 15 ⁇ m is less than 25%, and preferably less than 20%, and when the percentage of primary grains with a diameter of less than 5 ⁇ m is greater than 10%, the average grain diameter after annealing primary recrystallization and decarburization being close to 10 ⁇ m.
  • magnesia In addition to the optional addition of titanium dioxide the addition to magnesia, alone or in combination, of boron or a boron compound, sulfur or one or more sulfur compounds, one or more sulfur and nitrogen compounds, antimony chloride, a compound of tin improves the magnetic quality.
  • magnesia additives enhance the inhibition of normal growth of primary grains during secondary recrystallization annealing.
  • magnesium, manganese sulfate, sodium thiosulfate, sulfate ammonium, ammonium thiosulfate, amidosulfuric acid (or acid sulfamic), urea, thiourea, tin sulfate can improve the quality magnetic.
  • nitriding at a temperature above 500 ° C, with ammonia (NH 3 ) diluted in an N 2 / H 2 mixture is another means of reinforcing the inhibition and improving the magnetic quality .
  • the increase in the manganese content can exceed 0.20% provided that the mass percentage of sulfur not precipitated as coarse particles of equal average diameter or greater than 300 nm remains greater than 0.006% before the annealing of primary recrystallization and decarburization.
  • This increase in manganese content, a gammagenic element that promotes formation austenite may be accompanied by a decrease in the sulfur content and a decrease in the carbon content, gamma element, and or a increase in the content of silicon, an alpha-element which promotes ferrite formation. It is essential to maintain a certain fraction austenite to dissolve AIN during reheating of the slab or bandaged.
  • the method according to the present invention is described for slabs continuous casting thickness between 150 and 300 mm. More the greater the slab thickness, the longer the time required for reach the target temperature at the heart of the slab. In the case of a reheating at parade, for example, it is best to slow down the speed passage of the slab in the oven when the thickness of the slab passes from 210 mm to 240 mm. It is possible to accelerate the speed of passage of the slab in the reheating furnace when the slab is thin, i.e. of thickness between approximately 15 and 100 mm.
  • the temperature of hot winding must be such that the mass percentage of sulfur not precipitated as coarse particles is equal to or greater than 0.004% and preferably 0.006% and such as the mass percentage nitrogen precipitated only as fine particles is less than 40% of the total mass percentage of nitrogen in the hot-rolled sheet. This temperature is generally less than 700 ° C.
  • the method according to the present invention can also be applied to thin strips of thickness between 1 and 10 mm obtained by pouring of liquid steel between two cooled rollers, the strips being quickly reheated to the core, given the small thickness, to a temperature below 1350 ° C before hot rolling.
  • the number of hot rolling passes is a function of the initial thickness of the slab or strip and the thickness of the sheet hot rolled. If the thickness of the slab or strip cast in continuous is sufficiently low, hot rolling roughing can be deleted.
  • Reheating and hot rolling of the thin strip cast in continuous can be suppressed if the mass percentage of sulfur not precipitated as coarse particles with a diameter equal to or greater than 300 nm, is greater than 0.006% and if the mass percentage of nitrogen precipitated only as fine particles is less than 40% of the total mass percentage of nitrogen in the raw sheet metal between two rolls.
  • the thin strip is then subjected to at least one annealing according to the invention.

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  • Physics & Mathematics (AREA)
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EP98914939A 1997-03-21 1998-03-18 Procede de fabrication d'une tole d'acier electrique a grains orientes pour la fabrication notamment de circuits magnetiques de transformateurs Expired - Lifetime EP0912768B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
FR9703451A FR2761081B1 (fr) 1997-03-21 1997-03-21 Procede de fabrication d'une tole d'acier electrique a grains orientes pour la fabrication notamment de circuits magnetiques de transformateurs
FR9703451 1997-03-21
PCT/FR1998/000540 WO1998042882A1 (fr) 1997-03-21 1998-03-18 Procede de fabrication d'une tole d'acier electrique a grains orientes pour la fabrication notamment de circuits magnetiques de transformateurs

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EP0912768A1 EP0912768A1 (fr) 1999-05-06
EP0912768B1 true EP0912768B1 (fr) 2004-05-12

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EP (1) EP0912768B1 (cs)
JP (1) JP2001506704A (cs)
KR (1) KR20000011149A (cs)
CN (1) CN1220704A (cs)
AT (1) ATE266742T1 (cs)
CZ (1) CZ375398A3 (cs)
DE (1) DE69823771T2 (cs)
FR (1) FR2761081B1 (cs)
PL (1) PL330039A1 (cs)
WO (1) WO1998042882A1 (cs)

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EP1162280B1 (en) * 2000-06-05 2013-08-07 Nippon Steel & Sumitomo Metal Corporation Method for producing a grain-oriented electrical steel sheet excellent in magnetic properties
JP4272557B2 (ja) * 2004-02-12 2009-06-03 新日本製鐵株式会社 磁気特性に優れた一方向性電磁鋼板の製造方法
JP4954876B2 (ja) * 2005-06-10 2012-06-20 新日本製鐵株式会社 磁気特性が極めて優れた方向性電磁鋼板及びその製造方法
JP4823719B2 (ja) * 2006-03-07 2011-11-24 新日本製鐵株式会社 磁気特性が極めて優れた方向性電磁鋼板の製造方法
CN103878175A (zh) * 2012-12-21 2014-06-25 鞍钢股份有限公司 一种低牌号冷轧硅钢热轧工序中的热轧方法
DE102014112286A1 (de) * 2014-08-27 2016-03-03 Thyssenkrupp Ag Verfahren zur Herstellung eines aufgestickten Verpackungsstahls
KR101696627B1 (ko) * 2014-11-26 2017-01-16 주식회사 포스코 방향성 전기강판용 소둔 분리제 조성물, 및 이를 이용한 방향성 전기강판의 제조방법
MX2018006621A (es) * 2015-12-04 2018-08-01 Jfe Steel Corp Metodo para producir lamina de acero electrico de grano orientado.
CN106319174B (zh) * 2016-09-23 2018-10-16 武汉钢铁有限公司 提高低温铸坯加热高磁感取向硅钢底层质量的退火隔离剂
CN111020140A (zh) * 2019-12-17 2020-04-17 无锡晶龙华特电工有限公司 一种磁性优良取向硅钢氧化镁退火隔离剂及其涂覆工艺
CN111996354B (zh) * 2020-08-27 2022-04-19 上海实业振泰化工有限公司 一种取向硅钢用液体添加剂的制备方法
WO2025187773A1 (ja) * 2024-03-06 2025-09-12 日本製鉄株式会社 方向性電磁鋼板の製造方法

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5948934B2 (ja) * 1981-05-30 1984-11-29 新日本製鐵株式会社 高磁束密度一方向性電磁鋼板の製造方法
DE4311151C1 (de) * 1993-04-05 1994-07-28 Thyssen Stahl Ag Verfahren zur Herstellung von kornorientierten Elektroblechen mit verbesserten Ummagnetisierungsverlusten
FR2731713B1 (fr) * 1995-03-14 1997-04-11 Ugine Sa Procede de fabrication d'une tole d'acier electrique a grains orientes pour la realisation notamment de circuits magnetiques de transformateurs

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WO1998042882A1 (fr) 1998-10-01
FR2761081A1 (fr) 1998-09-25
CN1220704A (zh) 1999-06-23
DE69823771T2 (de) 2005-05-12
EP0912768A1 (fr) 1999-05-06
DE69823771D1 (de) 2004-06-17
KR20000011149A (ko) 2000-02-25
ATE266742T1 (de) 2004-05-15
PL330039A1 (en) 1999-04-26
JP2001506704A (ja) 2001-05-22
FR2761081B1 (fr) 1999-04-30

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