WO2010047414A1 - Procédé de fabrication de tôles d’acier magnétiques à grains orientés - Google Patents

Procédé de fabrication de tôles d’acier magnétiques à grains orientés Download PDF

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WO2010047414A1
WO2010047414A1 PCT/JP2009/068444 JP2009068444W WO2010047414A1 WO 2010047414 A1 WO2010047414 A1 WO 2010047414A1 JP 2009068444 W JP2009068444 W JP 2009068444W WO 2010047414 A1 WO2010047414 A1 WO 2010047414A1
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annealing
slab
steel sheet
grain
ppm
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PCT/JP2009/068444
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English (en)
Japanese (ja)
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今村猛
村木峰男
早川康之
大村健
新垣之啓
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Ｊｆｅスチール株式会社
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Priority claimed from JP2008272261A external-priority patent/JP5338254B2/ja
Priority claimed from JP2009080090A external-priority patent/JP4962516B2/ja
Application filed by Ｊｆｅスチール株式会社 filed Critical Ｊｆｅスチール株式会社
Priority to KR1020147015188A priority Critical patent/KR20140077223A/ko
Priority to CN200980141876.5A priority patent/CN102197149B/zh
Publication of WO2010047414A1 publication Critical patent/WO2010047414A1/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
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1244—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest
    • C21D8/1272—Final recrystallisation annealing
    • C—CHEMISTRY; METALLURGY
    • 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
    • C21D6/00—Heat treatment of ferrous alloys
    • C21D6/008—Heat treatment of ferrous alloys containing Si
    • 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
    • C21D8/0221—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the working steps
    • C21D8/0236—Cold 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
    • C22C38/008—Ferrous alloys, e.g. steel alloys containing tin
    • 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
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/34—Ferrous alloys, e.g. steel alloys containing chromium with more than 1.5% by weight of silicon
    • C—CHEMISTRY; METALLURGY
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/16—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of sheets

Definitions

  • the present invention relates to a method for producing a grain oriented electrical steel sheet suitable for use in transformer core materials and the like.
  • Patent Document 1 discloses a method of containing specified amounts of Al and S, that is, a method of using AlN and MnS as inhibitors.
  • Patent Document 2 discloses a method of containing a specified amount of at least one of S and Se, that is, a method of using MnS or MnSe as an inhibitor.
  • Patent Document 3 discloses a method using Pb, Sb, Nb, Te
  • Patent Document 4 discloses Zr, Ti, B, Nb, Ta. , V, Cr, and Mo are disclosed.
  • the method using these inhibitors is an effective method for developing secondary recrystallized grains stably, it is necessary to finely disperse the inhibitors in steel. It was necessary to re-dissolve the inhibitor component (inhibitor-forming element) once by slab heating at a high temperature of 1300 ° C. or higher. Further, since the inhibitor component causes deterioration of magnetic properties after secondary recrystallization, a purification annealing step for removing the inhibitor is required, and the step is performed at 1100 ° C. or higher. It was necessary to control the atmosphere at a high temperature.
  • Patent Document 5 proposes a technique for developing Goss oriented crystal grains by secondary recrystallization in a material that does not contain an inhibitor component. This method reveals the grain boundary misorientation dependence of the grain boundary energy of the grain boundary during primary recrystallization by eliminating impurities such as inhibitor components as much as possible. This is a technique for performing secondary recrystallization of grains having Goth orientation without using an inhibitor. This effect is called a texture inhibition effect. Since the method of Patent Document 5 does not require a step of purifying the inhibitor, the final finish annealing does not need to be performed at a high temperature, and since the inhibitor does not need to be finely dispersed in the steel, high-temperature slab heating is also possible. Since this method is not necessary, it is a method having great merit in terms of manufacturing cost and equipment maintenance.
  • Japanese Patent Publication No. 40-15644 Japanese Patent Publication No. 51-13469 Japanese Patent Publication No. 38-8214 JP-A-52-24116 JP 2000-129356 A
  • the component system that does not contain an inhibitor has few precipitates that suppress grain growth, so that the grain size tends to increase due to grain growth during annealing, that is, the annealing temperature dependency is strong.
  • the grain size after hot band annealing and after recrystallization annealing also fluctuates due to slight variations in process conditions, specifically variations in each annealing temperature.
  • the magnetic characteristics at the full length and the full width fluctuate, and the problem that good magnetic characteristics cannot be obtained as a whole coil has become apparent.
  • the present invention advantageously solves the above-described problems, and an object of the present invention is to propose an advantageous method for producing a grain-oriented electrical steel sheet that can achieve high-level stabilization of product magnetic properties.
  • Magnetic flux density B 8 (magnetizing force 800 A / m) of the obtained sample was measured according to the method of JIS C2550. Although the obtained magnetic flux density seemed to fluctuate at first glance, a very good correlation was obtained when arranged by the ratio of Al and N of steel slab components.
  • an annealing separator mainly composed of MgO is applied, and then 1200 Finish annealing was performed at 10 ° C. for 10 hours. Thereafter, planarization annealing was performed at 900 ° C. for 15 seconds under the condition of forming a tension-imparting coating mainly composed of magnesium phosphate and boric acid.
  • the magnetic flux density B 8 of the resulting samples was measured according to the method of JIS C2550. The result is shown in FIG. As shown in the figure, it can be seen that the magnetic flux density B 8 (vertical axis: unit T) obtained varies greatly depending on the types of added Zr, Ti, B, Nb and V. That is, the sample to which Zr (left end) and Ti (second from the left) were added had a low magnetic flux density and did not develop secondary recrystallization. On the other hand, when Nb (third from the same), B (third from the right), and V (second from the right) are added, the magnetic flux density is higher than when not added (right end). It became clear.
  • each steel slab was slab heated at 1250 ° C., it was hot-rolled to a hot-rolled sheet having a thickness of 2.8 mm, then annealed at 1100 ° C. for 60 seconds and then cold-rolled to a final thickness of 0.30 mm. Finished. Then, after recrystallization annealing in a soaking condition of 50% N 2 -50% H 2 at 840 ° C. for 80 seconds, after applying an annealing separator mainly composed of MgO, 1200 Finish annealing was performed at 10 ° C. for 10 hours. Thereafter, planarization annealing was performed at 900 ° C. for 15 seconds under the condition of forming a tension-imparting coating mainly composed of magnesium phosphate and boric acid.
  • the iron loss of the entire length of the coil is measured in advance with an in-line iron loss meter, a total of five samples are taken from the inside of the coil by the same method as in Experiment 1b, and the magnetic properties of the obtained sample are JIS C 2550 As a representative value of the coil, the value having the worst magnetic characteristics among the five locations was measured.
  • FIG. 4 shows that the magnetic flux density B 8 (vertical axis: unit T) varies greatly depending on the trace element added by about 50 ppm.
  • secondary recrystallization did not appear in the Zr additive (left end) and the Ti additive (second from the left) having a low magnetic flux density.
  • Nb third from the left
  • B third from the right
  • V second from the same
  • the reason why the magnetic characteristics change due to the addition of a trace element or the reason why the magnetic characteristics improve by adding at least one of B, Nb, and V is not necessarily clearly elucidated.
  • the elements having poor magnetic characteristics are Zr and Ti whose nitride is more stable than Al, and the elements having good magnetic characteristics are B and B whose nitride is unstable than Al. Nb and V. From this, when Zr and Ti are present, it is presumed that N in the steel is combined with these elements and the formation of ZrN and TiN deteriorates the magnetic properties. On the other hand, even if B, Nb, or V exists, N in the steel is considered to form a stable nitride with Al, and a nitride with B, Nb, or V is not formed.
  • the inventors conducted further experiments to investigate the effect of uniformizing the particle size.
  • a specific element is added in a small amount as described above, and the ratio of the impurities Al and N is specified, and further, the intended purpose is further controlled by controlling the rate of temperature increase during recrystallization annealing. The knowledge that it was achieved advantageously was obtained.
  • the final thickness was 0.23 mm by the second cold rolling.
  • recrystallization annealing was performed in a soaking condition of 50% N 2 -50% H 2 at 850 ° C. for 60 seconds. At this time, the average rate of temperature increase between 600 and 800 ° C. was variously changed.
  • the recrystallized particle size of the obtained sample was measured, and the average particle size and its standard deviation were determined from the particle size distribution.
  • the recrystallized grain size is measured by cutting a section perpendicular to the rolling direction of the sample, etching with a nital liquid (nitral) and observing it with an optical microscope, and using an image processing device to check the grains in the field of view by an elliptical approximation method (fitting an approximate to an ellipse, and the average of the major axis and minor axis dimensions was taken as the grain size of the grains.
  • the above samples were collected from both ends and the center in the width direction of the produced recrystallized plate, and the observation location was set to the full thickness. Samples were collected so that the number of observed grains was at least 2000 in total in both ends and the center.
  • the standard deviation (vertical axis) when the average grain size is normalized to 1.0 is the temperature increase rate of recrystallization annealing (horizontal axis (average temperature increase rate between 600 to 800 ° C.): unit ° C. / S).
  • horizontal axis average temperature increase rate between 600 to 800 ° C.
  • S unit ° C. / S
  • the inventors define the ratio of Al and N, and control the rate of temperature rise during recrystallization annealing in a system in which at least one of B, Nb and V is added in a trace amount. This led to the conclusion that a grain-oriented electrical steel sheet having even better magnetic properties (including uniformity of magnetic properties) can be obtained.
  • the present invention is based on the above findings.
  • the gist configuration of the present invention is as follows. (1) By mass%, C: 0.10% or less, Si: 2.0 to 8.0% and Mn: 0.005 to 1.0%, Al 100 ppm or less, N, S and A grain-oriented electrical steel sheet comprising a series of steps in which Se is set to 50 ppm or less, and the balance is finished by rolling a slab composed of Fe and inevitable impurities to finish the final plate thickness, and then performing recrystallization annealing and then finishing annealing. In the manufacturing method, The ratio of the amount of Al and the amount of N contained in the slab is set to 1.4 or more in terms of mass ratio, and one or more selected from B, Nb and V are further added to the slab. A method for producing a grain-oriented electrical steel sheet, characterized by containing 10 to 150 ppm in total.
  • C 0.10% or less
  • Si 2.0 to 8.0%
  • Mn 0.005 to 1.0%
  • N, S And Se are each reduced to 50 ppm or less
  • the balance is composed of a series of steps in which a final slab is rolled by rolling a slab composed of Fe and inevitable impurities, and then subjected to recrystallization annealing and then finish annealing.
  • the slab further contains one or more selected from B, Nb and V in a total range of 10 to 150 ppm, and the ratio of Al to N contained as impurities is expressed as Al by mass ratio. /N ⁇ 1.4, and the average heating rate between 600 and 800 ° C. in recrystallization annealing is set to 15 ° C./s or more.
  • the present invention in a component system that does not substantially contain an inhibitor, it is possible to reduce variations in magnetic characteristics in the longitudinal direction and width direction of the coil, and as a result, excellent magnetic characteristics (that is, high-level stability) as a whole product coil. Can be obtained.
  • FIG. 1 is a graph showing the relationship between the Al / N ratio Al / N (horizontal axis: mass ratio) in steel and the magnetic flux density B 8 (vertical axis: unit T).
  • FIG. 2 is a graph showing the relationship between the ratio Al / N (horizontal axis: mass ratio) between impurities Al and N in steel and the magnetic flux density B 8 (vertical axis: unit T).
  • FIG. 3 is a diagram showing a comparison of the relationship between the type of trace elements added to steel (horizontal axis) and the magnetic flux density B 8 (vertical axis: unit T).
  • FIG. 1 is a graph showing the relationship between the Al / N ratio Al / N (horizontal axis: mass ratio) in steel and the magnetic flux density B 8 (vertical axis: unit T).
  • FIG. 2 is a graph showing the relationship between the ratio Al / N (horizontal axis: mass ratio) between impurities Al and N in steel and the magnetic flux density B 8 (vertical
  • FIG. 4 is a diagram showing the relationship between the type of trace elements added to the steel (horizontal axis) and the magnetic flux density B 8 (vertical axis: unit T).
  • FIG. 5 is a diagram showing the standard deviation (vertical axis) when the average grain size is normalized to 1.0 in relation to the rate of temperature increase of recrystallization annealing (horizontal axis: ° C./s).
  • the present invention will be specifically described below. First, the reason why the component composition of the slab is limited to the above range in the present invention will be described. In principle, the reason for limitation will be described for each element, but this does not mean that each element affects each other independently, and it is effective on the assumption that other elements are within the scope of the present specification. . In other words, the range limitation of each element achieves the target effect or a more preferable effect by the range limitation of other elements or the combination effect with manufacturing conditions. As described above,% and ppm in the composition are based on mass unless otherwise specified.
  • C 0.10% or less
  • the amount of C exceeds 0.10%, it is difficult to reduce to 50 ppm or less where magnetic aging does not occur even when decarburization treatment is performed. Therefore, the C content is limited to 0.10% or less.
  • a particularly preferable range is 0.04% or less.
  • a smaller amount of C is desirable, but industrially, it is generally contained at 30 ppm or more.
  • Si 2.0 to 8.0% Si is an element necessary for increasing the specific resistance of steel and improving iron loss, but its effect is poor at less than 2.0%. On the other hand, if it exceeds 8.0%, workability deteriorates and rolling becomes difficult. Therefore, the Si content is limited to the range of 2.0 to 8.0%. A particularly preferred lower limit is 2.8%. A particularly preferred upper limit is 3.5%.
  • Mn 0.005 to 1.0%
  • Mn is an element necessary for improving the hot workability, but its effect is poor when it is less than 0.005%.
  • Mn if it exceeds 1.0%, the magnetic flux density of the product plate decreases. For this reason, the amount of Mn was limited to the range of 0.005 to 1.0%.
  • a particularly preferred lower limit is 0.02%.
  • a particularly preferred upper limit is 0.20%.
  • Al 100 ppm or less
  • N, S, Se 50 ppm or less
  • the amount of Al is 100 ppm or less
  • the amount of N, S, and Se is 50 ppm or less.
  • Al and Se are elements that are difficult to remove (purify) from the steel by finish annealing or the like, and therefore, it is more preferable that Al is 80 ppm and Se is 20 ppm or less. In general, it is generally contained 20 ppm or more and 6 ppm or more, respectively.
  • N and S which are light elements, are difficult to remove completely at the time of adjusting the components before making the steel slab, and if no special treatment is performed, about 20 ppm each remains in the steel plate. It is common.
  • the mass ratio of Al to N (Al / N) is required to be 1.4 or more for the reasons described above, and in particular, when Al / N is set to 2.0 or more, the magnetic properties are improved. More desirable. Further, as described above, since it is difficult to completely remove N, addition of a trace amount of Al in the range of 100 ppm or less to satisfy Al / N ⁇ 1.4 is not prevented.
  • the upper limit of Al / N is not necessary from the viewpoint of the effect, but generally does not exceed 5 from the lower limit of 20 ppm of the industrial N amount.
  • One or more selected from B, Nb and V 10 to 150 ppm in total Furthermore, in order to sufficiently obtain the effect of improving the magnetic characteristics in the present invention, it is necessary to add 10 ppm or more of one or more of B, Nb and V. The reason is as described above. If the total addition amount is less than 10 ppm, the addition effect is small. Preferably, when each addition amount is 10 ppm or more, the effect of the present invention can be obtained more reliably. More preferably, each is 20 ppm or more. However, since these trace additive elements remain in the base iron even in the final product and cause deterioration of iron loss, the total amount is limited to 150 ppm or less.
  • the total amount is preferably 100 ppm or less, and more preferably 50 ppm or less.
  • the most preferable element is Nb, which is superior to others in the effect of making the crystal grain size uniform after recrystallization annealing.
  • the essential element and the suppressing element have been described.
  • at least one selected from Ni, Cr, Cu, P, Sn, Sb, Bi, and Mo as other magnetic property improving elements is described below. It can contain suitably in the range.
  • Ni 0.01-1.50%
  • Ni is an element useful for improving the magnetic properties by improving the hot-rolled sheet structure, but if the addition amount is less than 0.01%, the addition effect is poor. On the other hand, if it exceeds 1.50%, the secondary recrystallization becomes unstable and the magnetic properties deteriorate. Preferably it is 0.010% or more.
  • Sn 0.005 to 0.50%
  • Sb 0.005 to 0.50%
  • Bi 0.005 to 0.50%
  • Mo 0.005 to 0.10%
  • the upper limit of Mo is preferably 0.100% or less.
  • the molten steel adjusted to the above preferred component composition is made into a slab by a normal ingot-making method or a continuous casting method. Further, a thin cast piece having a thickness of 100 mm or less may be manufactured by a direct casting method. In the case of a slab, it is heated and rolled by a normal method, but may be immediately subjected to hot rolling without heating after casting. In the case of a thin slab, hot rolling may be performed, or the hot rolling may be omitted and the process may proceed as it is.
  • the slab heating temperature before hot rolling is a component system that does not contain an inhibitor component with reduced Al, N, S, and Se
  • high temperature annealing is required to dissolve the inhibitor, which has been essential in the past. do not do. Therefore, a low temperature of 1250 ° C. or lower is desirable in terms of cost.
  • the hot-rolled sheet annealing temperature for obtaining good magnetic properties is preferably about 800 to 1150 ° C. If the hot-rolled sheet annealing temperature is less than 800 ° C., a band texture in hot rolling remains, making it difficult to achieve a sized primary recrystallized structure and inhibiting the development of secondary recrystallization. (When a band structure that requires hot-rolled sheet annealing is present in advance). On the other hand, if the hot-rolled sheet annealing temperature exceeds 1150 ° C., the grain size after the hot-rolled sheet annealing is excessively coarsened, which is extremely disadvantageous in realizing a sized primary recrystallized structure.
  • hot-rolled sheet annealing After hot-rolled sheet annealing, it is subjected to recrystallization annealing after cold rolling at least once with intermediate or intermediate annealing.
  • the temperature is raised to 100 to 300 ° C., and the aging treatment at 100 to 300 ° C. is performed once or a plurality of times in the course of cold rolling in order to improve the magnetic properties. It is advantageous.
  • Recrystallization annealing is performed in a wet atmosphere when decarburization is required, but may be performed in a dry atmosphere when decarburization is not required.
  • the soaking temperature in this recrystallization annealing is not particularly limited as long as it is equal to or higher than the recrystallization temperature, but there is a concern that annealing at an excessively high temperature results in a coarse crystal grain size and unstable secondary recrystallization. Therefore, the upper limit of the annealing temperature is preferably about 1050 ° C.
  • a technique for increasing the amount of Si by a siliconization method may be used in combination.
  • the average temperature increase rate from 600 ° C. to 800 ° C. is 15 ° C./s or more. This is because when the average value of the heating rate is 15 ° C./s or more, as shown in FIG. 5, the standard deviation when the average particle size is normalized to 1.0 is extremely small. This is because the variation in the particle size becomes very small, which is further advantageous in obtaining excellent magnetic characteristics stably.
  • the upper limit value of the average temperature increase rate is not particularly limited and is preferably as large as possible. However, from the viewpoint of temperature control, it is preferable to adjust the temperature increase rate within a range of 300 ° C./s or less.
  • the average rate of temperature rise may be determined by measuring the surface temperature of the plate with a radiation thermometer and dividing the temperature rise (200 ° C.) by the time from 600 ° C. to 800 ° C.
  • a secondary recrystallized structure is developed by applying a final annealing after applying an annealing separator mainly composed of MgO. It is possible to form a forsterite film.
  • the main component is silica or alumina that inhibits the formation of the forsterite film even if it is used or not used. Use things. When these annealing separators are applied, it is effective to perform electrostatic coating that does not carry moisture, and a heat-resistant inorganic material sheet (silica, alumina, mica) may be used.
  • the finish annealing is desirably performed at 800 ° C. or higher for secondary recrystallization.
  • the holding temperature is preferably about 850 to 950 ° C., and the finish annealing is finished at the holding stage. It is also possible.
  • finish annealing also has the meaning of purification annealing.
  • This insulating coating is desirably a coating that can apply tension to the steel sheet in order to reduce iron loss.
  • a coating method that deposits inorganic material on the steel sheet surface by a tension coating application method through a binder, physical vapor deposition method, or chemical vapor deposition method a coating film with excellent adhesion can be obtained, and iron loss reduction effect Will also improve.
  • Example 1 C 0.018 to 0.023%, Si: 3.20 to 3.40%, Mn: 0.10 to 0.15%, Cr: 0.03 to 0.05%, Al: 30 to 140 ppm and A steel slab containing N: 29 to 50 ppm, having an Al / N ratio shown in Table 1, further containing the Nb amount shown in Table 1, and the balance being Fe and inevitable impurities was produced by continuous casting. . Subsequently, the slab was heated at 1200 ° C., and a hot rolled sheet having a thickness of 2.2 mm was formed by hot rolling. Next, hot-rolled sheet annealing was performed at 1060 ° C. for 40 seconds, and finished to a thickness of 0.23 mm by one cold rolling.
  • the collection of the magnetic property measurement sample and the measurement of the magnetic property in this example were performed according to the following procedure.
  • the magnetic properties were collected and measured according to the method of JIS C2550. Of the above five locations, the magnetic flux density B8 and W17 / 50 in the sample having the worst magnetic characteristics is used as a representative value of the coil. Was evaluated.
  • the above measurement evaluation results are also shown in Table 1.
  • the Al / N ratio is the value shown in Table 2, and further contains the amount of Nb shown in Table 2, with the balance being a steel slab composed of Fe and inevitable impurities.
  • the iron loss of the entire length of the coil was measured in advance with an in-line iron loss meter, and a total of 5 samples were collected: 3 places where the iron loss was bad in the full length measurement and 2 ends of the coil: 2 places.
  • the magnetic properties (magnetic flux density B 8 , iron loss W 17/50 ) of the obtained sample were measured by the method described in JIS C 2550, and the value with the worst magnetic properties among the five locations was taken as the representative value of the coil. did. In this method, when the variation in the magnetic characteristics is large, the representative value is deteriorated. Therefore, it can be considered that the variation in the coil can be quantified.
  • Table 2 The obtained results are also shown in Table 2.
  • Example 3 A steel slab containing the components shown in Table 3 with the balance being Fe and inevitable impurities was produced by continuous casting. Subsequently, the slab was heated at 1250 ° C., and a hot-rolled sheet having a thickness of 2.3 mm was formed by hot rolling. Next, hot-rolled sheet annealing was performed at 1000 ° C. for 35 seconds, and a steel sheet having a thickness of 0.82 mm was formed by the first cold rolling. Subsequently, after performing an intermediate annealing at 1000 ° C. for 40 seconds, a final thickness of 0.23 mm was obtained by the second cold rolling. Subsequently, recrystallization annealing was performed at 850 ° C.
  • an annealing separator mainly composed of MgO was applied, and final annealing was performed at 1250 ° C. for 10 hours.
  • the Ar atmosphere was set for the latter half 5 hours out of the 10-hour holding, and the hydrogen atmosphere was set for the rest.
  • planarization annealing was performed at 900 ° C. for 15 seconds, which also served to form a tension-imparting coating mainly composed of magnesium phosphate and boric acid.
  • the iron loss of the entire length of the coil was measured in advance with an in-line iron loss meter, and a total of 5 samples were collected: 3 places where the iron loss was bad in the full length measurement and 2 ends of the coil: 2 places.
  • the magnetic properties (magnetic flux density B 8 , iron loss W 17/50 ) of the obtained sample were measured by the method described in JIS C 2550, and the value with the worst magnetic properties among the five locations was taken as the representative value of the coil. did. In this method, when the variation in the magnetic characteristics is large, the representative value is deteriorated. Therefore, it can be considered that the variation in the coil can be quantified.
  • Table 4 The obtained results are also shown in Table 4.
  • recrystallization annealing was performed at 835 ° C. for 90 seconds in a wet atmosphere of 60% N 2 -40% H 2 .
  • the average temperature increase rate between 600 and 800 ° C. was variously changed as shown in Table 5.
  • purification annealing was performed at 1200 ° C. for 25 hours.
  • flattening annealing was performed at 900 ° C. for 15 seconds under the condition of forming a tension-imparting coating mainly composed of magnesium phosphate and boric acid.
  • the iron loss of the entire length of the coil was measured in advance with an in-line iron loss meter, and a total of 5 samples were collected: 3 places where the iron loss was bad in the full length measurement and 2 ends of the coil: 2 places.
  • the magnetic properties (magnetic flux density B 8 , iron loss W 17/50 ) of the obtained sample were measured by the method described in JIS C 2550, and the value with the worst magnetic properties among the five locations was taken as the representative value of the coil. did. In this method, when the variation in the magnetic characteristics is large, the representative value is deteriorated. Therefore, it can be considered that the variation in the coil can be quantified.
  • Table 5 The obtained results are also shown in Table 5.
  • the average temperature increase rate between 600 to 800 ° C. in the recrystallization annealing step to 15 ° C./s or more, even better magnetic properties can be obtained.
  • the average temperature rising rate is less than 15 ° C./s, the magnetic properties deteriorate due to variations.
  • the magnetic properties can be improved by making Al / N 1.4 or more and containing a predetermined amount of trace elements. Can do.
  • the present invention in a component system that does not contain an inhibitor, variation in magnetic characteristics in the longitudinal direction and width direction of the coil can be reduced, and as a result, good magnetic characteristics can be obtained as a whole product coil. That is, it is possible to obtain a grain-oriented electrical steel sheet having excellent magnetic characteristics over the entire length and width of the coil, and this grain-oriented electrical steel sheet is extremely effective for applications such as a coil core that requires a strong magnetic flux density.

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Abstract

La présente invention concerne un procédé de fabrication d’une tôle d’acier magnétique à grains orientés, présentant des caractéristiques magnétiques de grande stabilité, à l’aide d’un système de composants ne contenant aucun inhibiteur. Lors de la fabrication de tôles d’acier magnétiques à grains orientés, à l’aide d’une brame constituée d’un système de composants ne contenant aucun inhibiteur, la brame contient au total 10 à 150 ppm d’au moins une sorte de micro-élément sélectionné parmi B, Nb et V, le rapport de masse d’Al et N inclus sous forme d’impuretés étant égal à Al/N ≥ 1,4; et de préférence, la vitesse moyenne d’augmentation de la température entre 600 °C et 800 °C pendant le recuit de recristallisation est supérieure ou égale à 15 °C/s.
PCT/JP2009/068444 2008-10-22 2009-10-21 Procédé de fabrication de tôles d’acier magnétiques à grains orientés WO2010047414A1 (fr)

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JP5672273B2 (ja) * 2012-07-26 2015-02-18 Ｊｆｅスチール株式会社 方向性電磁鋼板の製造方法
MX2015005396A (es) * 2012-10-30 2015-07-21 Jfe Steel Corp Metodo para la fabricacion de una lamina de acero electrico de grano orientado que exhibe baja perdida de hierro.
CN103695791B (zh) * 2013-12-11 2015-11-18 武汉钢铁(集团)公司 一种高磁感取向硅钢及生产方法
KR102140991B1 (ko) * 2016-03-09 2020-08-04 제이에프이 스틸 가부시키가이샤 방향성 전자 강판의 제조 방법
CN109477186B (zh) * 2016-07-29 2020-11-27 杰富意钢铁株式会社 取向性电磁钢板用热轧钢板及其制造方法、以及取向性电磁钢板的制造方法
KR101947026B1 (ko) * 2016-12-22 2019-02-12 주식회사 포스코 방향성 전기강판 및 이의 제조방법
WO2020158893A1 (fr) 2019-01-31 2020-08-06 Ｊｆｅスチール株式会社 Tôle d'acier électrique à grains orientés et noyau de fer mettant en œuvre une telle tôle d'acier
CN111763872B (zh) * 2020-08-13 2021-06-01 包头市威丰稀土电磁材料股份有限公司 一种稀土微合金取向硅钢生产工艺

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