Title of invention: Manufacturing method of grain-oriented electrical steel sheet and grain-oriented electrical steel sheet
Technical field
[0001]
　The present invention relates to a method for manufacturing a grain-oriented electrical steel sheet and a grain-oriented electrical steel sheet.
　The present application claims priority based on Japanese Patent Application No. 2018-052899 filed in Japan on March 20, 2018, the contents of which are incorporated herein by reference.
Background technology
[0002]
　The grain-oriented electrical steel sheet contains Si in an amount of about 2% by mass to 5% by mass, and the orientation of the crystal grains of the steel sheet is highly integrated in the {110} <001> orientation called the Goss orientation. The grain-oriented electrical steel sheet has excellent magnetic characteristics and is used, for example, as an iron core material for a static induction device such as a transformer.
[0003]
　Various developments have been made for such grain-oriented electrical steel sheets in order to improve their magnetic properties. In particular, with the recent demand for energy saving, further reduction of iron loss is required for grain-oriented electrical steel sheets.
[0004]
　In the production of grain-oriented electrical steel sheets, the crystal orientation is controlled by utilizing a catastrophic grain growth phenomenon called secondary recrystallization. However, in order to appropriately control the crystal orientation in the secondary recrystallization, it is important to appropriately control the primary recrystallization performed prior to the secondary recrystallization.
[0005]
　For example, Patent Document 1 discloses a technique for reducing the iron loss value of grain-oriented electrical steel sheets by controlling the retention time and the interval of magnetic domain subdivision processing in the temperature raising process of primary recrystallization annealing. Patent Document 2 discloses a technique for reducing the iron loss value of a grain-oriented electrical steel sheet by controlling the conditions for forming an insulating film that applies tension to the grain-oriented electrical steel sheet. Patent Document 3 discloses a technique for producing a grain-oriented electrical steel sheet having low iron loss over the entire length of the coil by controlling the heat pattern in the temperature raising process of primary recrystallization annealing. Patent Document 4 discloses a technique for reducing the iron loss value of grain-oriented electrical steel sheets by strictly controlling the average grain size of crystal grains after secondary recrystallization and the deviation angle from the ideal orientation. ..
Prior art literature
Patent documents
[0006]
Patent Document 1: Japanese Patent Application Laid-Open No. 2014-194703
Patent Document 2: International Publication No. 2013/175733
Patent Document 3: International Publication No. 2014/0497770
Patent Document 4: Japanese Patent Application Laid-Open No. 7-268567
Outline of the invention
Problems to be solved by the invention
[0007]
　As disclosed in Patent Document 3, in the temperature raising process of primary recrystallization annealing, the magnetic properties of grain-oriented electrical steel sheets are improved by rapidly raising the temperature between 500 ° C. and 600 ° C. at 100 ° C./s or higher. It has been confirmed that it can be done.
[0008]
　However, in Patent Documents 1 to 4, it is examined in detail how the magnetic properties of the grain-oriented electrical steel sheet are affected when the rate of rapid temperature rise in the primary recrystallization annealing is further increased. It has not been.
[0009]
　The rapid temperature rise in the primary recrystallization annealing increases the variation in the iron loss value of the grain-oriented electrical steel sheet for each coil. Therefore, when the rapid temperature rise is performed at a faster temperature rise rate than before, a grain-oriented electrical steel sheet with low iron loss may not be obtained depending on other conditions of primary recrystallization annealing and the conditions of the subsequent process. ..
[0010]
　The present invention has been made in view of the above problems and the like, and a grain-oriented electrical steel sheet having a lower iron loss is produced when a rapid temperature rise is performed at a faster temperature rise rate than before by primary recrystallization annealing. It is an object of the present invention to provide a method for producing a new and improved grain-oriented electrical steel sheet, and a grain-oriented electrical steel sheet produced by the method.
Means to solve problems
[0011]
　The gist of the present invention is as follows.
[1] In the method for producing a directional electromagnetic steel sheet according to one aspect of the present invention, the component composition is mass%,
C: 0.02% or more and 0.10% or less,
Si: 2.5% or more and 4.5. %
Or less, Mn: 0.01% or more and 0.15% or less,
total of S and Se: 0.001% or more and 0.050% or less,
acid-soluble Al: 0.01% or more and 0.05% or less,
N: 0.002% or more and 0.015% or less,
Cu: 0% or more and 0.30% or less,
Sn: 0% or more and 0.30% or less,
Ni: 0% or more and 0.30% or less,
Cr: 0% or more and 0 A slab containing .30% or less and
Sb: 0% or more and 0.30% or less
and the balance consisting of Fe and impurities is heated to 1280 to 1450 ° C. and hot-rolled to obtain a hot-rolled steel sheet. After the step of obtaining the
　hot-rolled steel sheet and pickling the hot-rolled steel sheet to obtain a pickled steel sheet, or by subjecting the hot-rolled steel sheet to hot-rolled sheet annealing to obtain a hot-rolled and blunted sheet, the hot-rolled steel sheet is subjected to A step of obtaining a pickled
　steel sheet by performing pickling, a step of obtaining a cold-rolled steel sheet by cold-rolling the pickled
　steel sheet, and a step of performing primary recrystallization annealing on the cold-rolled steel sheet.
　After applying an annealing separator containing MgO to the surface of the cold-rolled steel sheet after primary recrystallization annealing, a step of obtaining a finish annealing plate by
　performing finish annealing, and after applying an insulating film to the finish annealing plate, Including the step of performing flattening annealing, the
　thickness loss of the hot-rolled steel plate or the hot-rolled annealed plate is 5 μm or more and 150 μm or less in the pickling,
　and the atmosphere in the rapid temperature rise of the primary recrystallization annealing. The dew point temperature of the annealed steel sheet is 0 ° C. or lower, and the average heating rate Va (° C./s) in the temperature range of 550 ° C. to 700 ° C. is 400 ≦ Va ≦ 3000. When the tension Sa (N / mm 2 ) is Va ≦ 1000, 1.96 ≦ Sa ≦ (25.5-0.0137 × Va), and when the tension Sa is Va> 1000, 1. 96 ≦ Sa ≦ 11.8, in the
　flattening annealing, the reached temperature Af (° C.) at the time of annealing is 800 ≦ Af ≦ 950, and the holding time Tf (seconds) of 800 ° C. or higher is 10 ≦ Tf ≦ 100. The tension Cf (N / mm 2 ) applied in the plate-passing direction of the finish annealing plate during the flattening annealing is 3.92 ≦ Cf ≦ 11.8.
[2] In the method for producing a grain-oriented electrical steel sheet according to the above [1], the component composition of the slab is, in mass%,
Cu: 0.01% or more and 0.30% or less,
Sn: 0.01%. More than 0.30% or less,
Ni: 0.01% or more and 0.30% or less,
Cr: 0.01% or more and 0.30% or less, and
Sb:
One or more of 0.01% or more and 0.30% or less may be contained.
[3] The grain-oriented electrical steel sheet according to another aspect of the present invention has a
　silicon steel sheet, a
　forsterite film arranged on the silicon steel sheet, and
　an insulating film arranged on the forsterite film. The
　silicon steel sheet is an electromagnetic steel sheet having a component composition of mass%,
Si: 2.5% or more and 4.5% or less,
Mn: 0.01% or more and 0.15% or less,
C: 0% or more. 0.0050% or less,
total of S and Se: 0% or more and 0.005% or less,
acid-soluble Al: 0% or more and 0.01% or less,
N: 0% or more and 0.005% or less,
Cu: 0% or more 0.30% or less,
Sn: 0% or more and 0.30% or less,
Ni: 0% or more and 0.30% or less,
Cr: 0% or more and 0.30% or less, and
Sb: 0% or more and 0.30% or less
The balance is
　composed of Fe and impurities, and the average grain size of the secondary recrystallized grains of the silicon steel sheet is 10 mm or more and 50 mm or less
　.
　　The plate thickness is 0.15 mm or more and
　　0.23 mm or less, the iron loss Wp is 0.800 W / kg or less at W17 / 50,
　　and the ratio of the iron loss Wp to the iron loss Wd when the magnetic domain is controlled A certain Wp / Wd is 1.03 or more and 1.15 or less at W17 / 50, and the
　　magnetic flux density B8 value is 1.930T or more.
[4] In the grain-oriented electrical steel sheet according to the above [3], the component composition of the silicon steel sheet is, in mass%,
Cu: 0.01% or more and 0.30% or less,
Sn: 0.01% or more and 0. .30% or
less, Ni: 0.01% or more than
0.30%, Cr: 0.01% 0.30% or less, and
Sb: 0.01% 0.30% or less
one or two of The above may be contained.
Effect of the invention
[0012]
　According to the above aspect according to the present invention, it is possible to manufacture a directional electric steel sheet having a lower iron loss. Specifically, according to the above aspect according to the present invention, after the primary recrystallization annealing, the number of crystal grains having a Goss orientation with good magnetic characteristics increases, so that the crystal grains after the secondary recrystallization have a Goss orientation. It is possible to manufacture a directional electromagnetic steel plate having a smaller diameter of crystal grains while improving the degree of integration. Therefore, it is possible to manufacture a grain-oriented electrical steel sheet having a further reduced iron loss value. Further, according to another aspect of the present invention, it is possible to provide a grain-oriented electrical steel sheet with reduced iron loss without performing magnetic domain control processing.
A brief description of the drawing
[0013]
FIG. 1 is a graph plotting the results shown in Table 1 of Examples, with the average heating rate Va on the horizontal axis and the steel plate tension Sa on the vertical axis.
Mode for carrying out the invention
[0014]
　Hereinafter, preferred embodiments of the present invention will be described in detail. However, the present invention is not limited to the configuration disclosed in the present embodiment, and various modifications can be made without departing from the spirit of the present invention.
[0015]
　The present inventors have obtained the following findings as a result of diligent studies on a grain-oriented electrical steel sheet and a method for manufacturing the grain-oriented electrical steel sheet in order to improve the magnetic properties of the grain-oriented electrical steel sheet.
[0016]
　The present inventors set the temperature rise rate in primary recrystallization annealing to 400 ° C./s or more, control the atmosphere and steel sheet tension at the time of rapid temperature rise, and further, hot-rolled steel sheet (or hot-rolled annealed sheet). It has been found that the reduction of the iron loss value of the grain-oriented electrical steel sheet desired by the present inventors can be realized only by strictly controlling the thickness reduction when pickling the steel sheet and the conditions for flattening annealing. ..
　The flattening annealing is an annealing step in which an insulating film is applied to a steel sheet, and then the applied insulating film is annealed and the steel sheet is flattened at the same time.
[0017]
　The present inventors have come up with the present invention by considering the above findings. The gist of the present invention is as follows.
[0018]
　A method for producing a directional electromagnetic steel sheet, in which the component composition is mass%,
C: 0.02% or more and 0.10% or less,
Si: 2.5% or more and 4.5% or less,
Mn: 0.01. % Or more and 0.15% or less,
total of S and Se: 0.001% or more and 0.050% or less,
acid-soluble Al: 0.01% or more and 0.05% or less,
N: 0.002% or more and 0.015 %
Or less, Cu: 0% or more and 0.30% or less,
Sn: 0% or more and 0.30% or less,
Ni: 0% or more and 0.30% or less,
Cr: 0% or more and 0.30% or less, and
Sb: A
step of obtaining a hot-rolled steel sheet by heating a slab containing 0% or more and 0.30% or less and the balance of Fe and impurities to 1280 to 1450 ° C. and hot-rolling the slab and the
　hot-rolled steel sheet. Is pickled to obtain a pickling plate, or the hot-rolled steel plate is annealed to obtain a hot-rolled fired plate, and then the hot-rolled fired plate is pickled to obtain a pickling plate. A step of obtaining a plate, a step of obtaining a
　cold-rolled steel plate by cold-rolling the pickled plate, a step of
　subjecting the cold-rolled steel plate to primary recrystallization, and a step of
　primary re-crystallizing the cold-rolled steel plate. A process of obtaining a finished annealed plate by applying a precipitating separator containing MgO to the surface of
　In the
　pickling, the thickness loss of the hot-rolled steel sheet or the hot-rolled annealed sheet is 5 μm or more and 150 μm or less.
　In the rapid temperature rise of the primary recrystallization annealing, the dew point temperature of the atmosphere is 0 ° C. or lower, and the average temperature rise rate Va (° C./s) in the temperature range of 550 ° C. to 700 ° C. is 400 ≦ Va ≦ 3000. When the tension Sa (N / mm 2 ) applied in the sheeting direction of the cold-rolled steel sheet is Va ≦ 1000, it is 1.96 ≦ Sa ≦ (25.5-0.0137 × Va). When the tension Sa is Va> 1000, 1.96 ≦ Sa ≦ 11.8, and in the
　flattening annealing, the reached temperature Af (° C.) at the time of annealing is 800 ≦ Af ≦ 950, which is 800 ° C. or higher. The holding time Tf (seconds) is 10 ≦ Tf ≦ 100, and the tension Cf (N / mm 2 ) applied in the passing direction of the finished annealed sheet during the flattening annealing is 3.92 ≦ Cf ≦ 11. It is 8.
[0019]
　Further, in the grain-oriented electrical steel sheet according to the present embodiment, the average particle size of the secondary recrystallized grains of the silicon steel sheet is 10 mm or more and 50 mm or less, the plate thickness is 0.15 mm or more and 0.23 mm or less, and the magnetic domain control treatment is performed. Wp / Wd is 0.800 W / kg or less at W 17/50 , and Wp / Wd, which is the ratio of Wp to iron loss Wd when magnetic domain control processing is applied, is W 17/50. It is 1.03 or more and 1.15 or less, and the magnetic flux density B8 value is 1.930T or more. As described above, the grain-oriented electrical steel sheet according to the present embodiment has a small Wp / Wd. This is because the grain-oriented electrical steel sheet according to the present embodiment is efficiently reduced in iron loss, so that the effect of reducing the iron loss value by the magnetic domain control process is small. That is, the grain-oriented electrical steel sheet according to the present embodiment has sufficiently reduced iron loss even if the magnetic domain control treatment is not performed.
[0020]
　Although the magnetic domain control process can reduce the iron loss value of the grain-oriented electrical steel sheet, it increases the noise of the transformer using the grain-oriented electrical steel sheet as the iron core material. Therefore, according to the grain-oriented electrical steel sheet according to the present embodiment, noise can be reduced while improving the magnetic characteristics of the transformer.
[0021]
　Hereinafter, the method for manufacturing the grain-oriented electrical steel sheet according to the present embodiment will be specifically described.
　First, the component composition of the slab used for the grain-oriented electrical steel sheet according to the present embodiment will be described. In the following, unless otherwise specified, the notation "%" indicates "mass%". The numerical limitation range described below includes the lower limit value and the upper limit value. Numerical values ​​indicated as "super" and "less than" do not include the value in the numerical range. All% of the chemical composition of the steel sheet indicates mass%, and all% of the gas composition indicates vol%.
[0022]
　The content of C (carbon) is 0.02% or more and 0.10% or less. C has various roles, but when the C content is less than 0.02%, the crystal grain size becomes excessively large when the slab is heated, which increases the iron loss value of the grain-oriented electrical steel sheet. Let me. When the C content is more than 0.10%, the decarburization time becomes long during decarburization after cold rolling, and the manufacturing cost increases. Further, when the C content is more than 0.10%, decarburization tends to be incomplete, and the grain-oriented electrical steel sheet may cause magnetic aging. Therefore, the content of C is 0.02% or more and 0.10% or less. Preferably, it is 0.05% or more, or 0.09% or less.
[0023]
　The content of Si (silicon) is 2.5% or more and 4.5% or less. Si increases the electrical resistance of the steel sheet to reduce the eddy current loss of the grain-oriented electrical steel sheet and reduce the iron loss. When the Si content is less than 2.5%, it becomes difficult to sufficiently reduce the eddy current loss of the grain-oriented electrical steel sheet. When the Si content is more than 4.5%, the workability of the grain-oriented electrical steel sheet is lowered. Therefore, the Si content is 2.5% or more and 4.5% or less. Preferably, it is 2.7% or more, or 4.0% or less.
[0024]
　The content of Mn (manganese) is 0.01% or more and 0.15% or less. Mn forms MnS, MnSe, and the like, which are inhibitors that influence secondary recrystallization. When the Mn content is less than 0.01%, the absolute amounts of MnS and MnSe that cause secondary recrystallization are insufficient, and the orientation cannot be preferably controlled. When the Mn content is more than 0.15%, it becomes difficult to dissolve Mn during slab heating, and the inhibitor cannot be preferably controlled. Further, when the Mn content is more than 0.15%, the precipitation sizes of the inhibitors MnS and MnSe tend to be coarse, the optimum size distribution as the inhibitor is impaired, and the orientation cannot be preferably controlled. Therefore, the Mn content is 0.01% or more and 0.15% or less. Preferably, it is 0.03% or more, or 0.13% or less.
[0025]
　The total content of S (sulfur) and Se (selenium) is 0.001% or more and 0.050% or less. S and Se form an inhibitor together with Mn described above. Both S and Se may be contained in the slab, but at least one of them may be contained in the slab. When the total content of S and Se is less than 0.001% or more than 0.050%, a sufficient inhibitory effect cannot be obtained and the orientation cannot be preferably controlled. Therefore, the total contents of S and Se are 0.001% or more and 0.050% or less. Preferably, it is 0.005% or more, or 0.040% or less.
[0026]
　The content of acid-soluble Al (acid-soluble aluminum) is 0.01% or more and 0.05% or less. Acid-soluble Al forms the inhibitors required to produce grain-oriented electrical steel sheets with high magnetic flux density. When the content of the acid-soluble Al is less than 0.01%, the inhibitor strength is insufficient and the orientation cannot be preferably controlled. When the content of the acid-soluble Al is more than 0.05%, AlN precipitated as an inhibitor is coarsened, the strength of the inhibitor is lowered, and the orientation cannot be preferably controlled. Therefore, the content of acid-soluble Al is 0.01% or more and 0.05% or less. Preferably, it is 0.02% or more, or 0.04% or less.
[0027]
　The content of N (nitrogen) is 0.002% or more and 0.015% or less. N forms the inhibitor AlN together with the acid-soluble Al described above. When the content of N is out of the above range, a sufficient inhibitory effect cannot be obtained and the orientation cannot be preferably controlled. Therefore, the content of N is 0.002% or more and 0.015% or less. Preferably, it is 0.005% or more, or 0.012% or less.
[0028]
　The rest of the slab used in the production of grain-oriented electrical steel sheets according to this embodiment is Fe and impurities. However, in addition to the above-mentioned elements, the slab used for producing the grain-oriented electrical steel sheet according to the present embodiment is Cu as an element for stabilizing secondary recrystallization in place of a part of Fe which is the remainder. , Sn, Ni, Cr and Sb may be contained in any one or more. It is not necessary to limit the lower limit of these selective elements, and the lower limit may be 0%.
[0029]
　The content of each of Cu, Sn, Ni, Cr and Sb may be 0.01% or more and 0.30% or less. When the content of even one of these elements is 0.01% or more, the effect of stabilizing secondary recrystallization can be sufficiently obtained, and the iron loss value of the grain-oriented electrical steel sheet can be further reduced. Can be done. If the content of any one of these elements exceeds 0.30%, the effect of stabilizing secondary recrystallization is saturated and the production cost increases, which is not preferable.
[0030]
　Next, a method for manufacturing a grain-oriented electrical steel sheet using the above-mentioned slab will be described.
　A slab is manufactured by casting molten steel adjusted to the above-mentioned composition. The slab casting method is not particularly limited. For example, the slab may be cast by a casting method such as a normal continuous casting method, an ingot method, or a thin slab casting method. In the case of continuous casting, the steel may be once cooled to a low temperature (for example, room temperature), reheated, and then hot-rolled, or the steel immediately after casting (casting slab) may be used. It may be continuously hot rolled. Further, in research and development, even when a steel ingot is formed in a vacuum melting furnace or the like, the same effect as that when a slab is formed has been confirmed with respect to the above-mentioned component composition.
[0031]
　Subsequently, the slab is heated to 1280 ° C. or higher to dissolve the inhibitor component in the slab. When the heating temperature of the slab is less than 1280 ° C., it becomes difficult to sufficiently dissolve the inhibitor components such as MnS, MnSe, and AlN, and the orientation cannot be preferably controlled. The heating temperature of the slab is preferably 1300 ° C. or higher. The upper limit of the heating temperature of the slab is not particularly specified, but may be 1450 ° C. or lower from the viewpoint of equipment protection.
[0032]
　A hot-rolled steel sheet is obtained by hot-rolling the heated slab. The thickness of the hot-rolled steel sheet may be, for example, 1.8 mm or more and 3.5 mm or less. When the thickness of the hot-rolled steel sheet is less than 1.8 mm, the temperature of the steel sheet after hot rolling becomes low, and the amount of AlN precipitated in the steel sheet increases, resulting in unstable secondary recrystallization, resulting in instability. A directional electromagnetic steel sheet having a thickness of 0.23 mm or less is not preferable because the magnetic properties are deteriorated. When the thickness of the hot-rolled steel sheet exceeds 3.5 mm, the rolling load in the cold rolling process becomes large, which is not preferable.
[0033]
　A hot-rolled annealed steel sheet is obtained by subjecting the hot-rolled steel sheet to annealing the hot-rolled steel sheet as needed. When the hot-rolled steel sheet is annealed, the shape of the steel sheet becomes better, so that the possibility of the steel sheet breaking in the subsequent cold rolling can be reduced. Hot-rolled sheet annealing may be omitted when intermediate annealing is performed in cold rolling. However, even in such a case, it is preferable to perform hot-rolled sheet annealing in order to reduce the possibility of the steel sheet breaking during cold rolling. The conditions for hot-rolled sheet annealing are not particularly limited, but general conditions may be used, and for hot-rolled hot-rolled steel sheets, continuous annealing is performed at 750 to 1200 ° C. for 10 seconds to 10 minutes. In the case of heat and box annealing, soaking may be performed at 650 to 950 ° C. for 30 minutes to 24 hours.
[0034]
　When the hot-rolled steel sheet is annealed, or when the hot-rolled steel sheet is annealed, the hot-rolled annealed steel sheet is pickled so that the thickness loss is 5 μm or more and 150 μm or less to obtain a pickled steel sheet. When the sheet thickness loss is less than 5 μm, the oxide (scale) formed on the surface of the steel sheet is not sufficiently removed by hot rolling and hot-rolled sheet annealing, or intermediate annealing described later, and the cold is applied after pickling. During inter-rolling, the rolling rolls are worn and have surface defects. When the plate thickness loss is more than 150 μm, the decarburization property in decarburization annealing deteriorates, the C content in the finally obtained grain-oriented electrical steel sheet increases, causing magnetic aging and deteriorating the magnetic properties.
[0035]
　When the plate thickness loss in pickling exceeds 150 μm, the cause of deterioration in decarburization property in decarburization annealing is desiliconization near the surface of the steel sheet formed in hot rolling and hot-rolled sheet annealing, or intermediate annealing described later. This is because the layer is removed. In hot rolling, hot-rolled sheet annealing and intermediate annealing, iron oxide and firelite (Fe 2 SiO 4 ) are formed on the surface of the steel sheet . Here, since the formation of firelight involves diffusion of Si near the surface of the steel sheet to the surface, a region in which the amount of Si is reduced, that is, a desiliconized layer is formed near the surface of the steel sheet. When the desiliconized layer is cold-rolled and remains even after decarburization annealing , the formation of external oxide SiO 2 on the surface of the steel sheet is suppressed by rapid heating . Therefore, the decarburization property is not inhibited in the decarburization annealing. On the other hand, when the desiliconized layer is removed by pickling, external oxide SiO 2 is formed on the surface of the steel sheet by rapid heating, so that decarburization property is hindered in decarburization annealing.
[0036]
　The type of acid in pickling is not particularly limited, and examples thereof include sulfuric acid, hydrochloric acid, and nitric acid. The plate thickness reduction may be adjusted according to the acid concentration and the immersion time. For example, the immersion in a sulfuric acid solution having a concentration of 10% by mass may be carried out for 10 seconds or more and 10 minutes or less.
[0037]
　The plate thickness reduction in pickling may be obtained by measuring the plate thickness before and after pickling with radiation or the like, or may be converted from the weight of the steel plate. When hot rolling and pickling are continuously performed, it may be obtained from the weight of the steel sheet before and after hot rolling, or may be obtained by converting from the coil diameter and the number of turns of the steel sheet. When hot-rolled sheet annealing and intermediate annealing and pickling, which will be described later, are continuously performed, the weight of the steel sheet before and after hot-rolled sheet annealing, or the steel sheet before intermediate annealing and after pickling, is simply achieved. It may be calculated by converting it from the weight, or it may be calculated by converting it from the coil diameter and the number of steel plate turns. Further, in order to promote pickling property, shot blasting treatment or the like may be performed before the pickling treatment.
[0038]
　A cold-rolled steel sheet is obtained by cold-rolling the pickling plate. Cold rolling may be performed not only once but also multiple times. When cold rolling is performed a plurality of times, intermediate annealing may be performed during the cold rolling. When performing cold rolling multiple times or when performing cold rolling multiple times with intermediate quenching sandwiched between them, the hot-rolled steel sheet or hot-rolled annealed sheet is cold-rolled multiple times, or the hot-rolled steel sheet or hot-rolled steel sheet or hot-rolled sheet A pickling plate is obtained by performing the above-mentioned pickling before the final cold rolling is performed by subjecting the fire-spreading blunt plate to cold rolling a plurality of times with intermediate annealing sandwiched between them, and the pickling plate is subjected to the final cold rolling. Perform inter-rolling. Further, the hot-rolled steel sheet or the hot-rolled annealed sheet may be pickled, then cold-rolled a plurality of times with intermediate annealing sandwiched between them, pickled again, and then finally cold-rolled. Absent. In this case, pickling may be performed so that the weight loss during pickling before the final cold rolling is 5 μm or more and 150 μm or less.
[0039]
　The hot-rolled steel sheet or hot-rolled annealed sheet may be heat-treated at about 300 ° C. or lower between cold rolling passes, between rolling roll stands, or during rolling. In such a case, the magnetic characteristics of the finally obtained grain-oriented electrical steel sheet can be further improved. The hot-rolled steel sheet or hot-rolled annealed sheet may be rolled by cold rolling three or more times, but cold rolling a large number of times increases the manufacturing cost, so that it is cold-rolled once or twice. It is preferably rolled by rolling.
[0040]
　The cold-rolled steel sheet is rapidly heated and then decarburized and annealed. These processes (rapid temperature rise and decarburization annealing) are also referred to as primary recrystallization annealing, and are preferably carried out continuously. By the primary recrystallization annealing, in the cold-rolled steel sheet, the Goss orientation grains before the secondary recrystallization can be increased and the crystal grains after the secondary recrystallization can be reduced.
[0041]
　In the method for producing grain-oriented electrical steel sheet according to the present embodiment, the average temperature rise rate Va in the temperature range of 550 ° C. to 700 ° C. is set to 400 ° C./s or more in the rapid temperature rise of the cold-rolled steel sheet in the primary recrystallization annealing. .. Thereby, in the present embodiment, it is possible to further increase the Goss orientation grains before the secondary recrystallization of the cold-rolled steel sheet and reduce the crystal grains after the secondary recrystallization.
[0042]
　When the average heating rate Va in the temperature range of 550 ° C to 700 ° C is 700 ° C / s or more, the Goss orientation grains before secondary recrystallization can be further increased, and the final obtained grain-oriented electrical steel sheet can be increased. Iron loss can be further reduced. On the other hand, when the average temperature rise rate Va in the above temperature range is less than 400 ° C./s, it becomes difficult to form a sufficient amount of Goss directional grains to reduce the crystal grains after the secondary recrystallization. The iron loss of the finally obtained grain-oriented electrical steel sheet increases. The upper limit of the average heating rate Va in the temperature range of 550 ° C to 700 ° C is not particularly limited, but may be 3000 ° C / s from the viewpoint of equipment and manufacturing cost.
[0043]
　The rapid temperature rise as described above can be carried out by using, for example, an energization heating method or an induction heating method.
[0044]
　In the method for producing a directional electromagnetic steel sheet according to the present embodiment, in the rapid temperature rise of primary recrystallization annealing, the tension Sa (that is, the steel sheet tension) applied in the sheet passing direction of the steel sheet is controlled to rapidly raise the temperature. The effect of increasing the Goss azimuth grains before the secondary recrystallization is sufficiently obtained. In the present embodiment, the steel sheet tension Sa (N / mm 2 ) in the temperature raising process of the primary recrystallization annealing is 1 when Va ≦ 1000 with respect to the average temperature rising rate Va (° C./s) in the rapid temperature rise. When .96 ≦ S ≦ (25.5-0.0137 × Va) and Va> 1000, 1.96 ≦ S ≦ 11.8.
[0045]
　When the steel sheet tension Sa exceeds the upper limit value depending on the average heating rate Va, the tension applied in the sheet passing direction of the cold-rolled steel sheet disturbs the texture of the crystal grains generated by the primary recrystallization, and the direction. It is not possible to reduce the iron loss of electrical steel sheets. On the other hand, when the steel plate tension Sa is less than 1.96 N / mm 2 , the cold-rolled steel plate in the through plate meanders, which may cause breakage of the cold-rolled steel plate and equipment damage.
[0046]
　In the rapid temperature rise of the primary recrystallization annealing, the dew point temperature of the atmosphere is set to 0 ° C. or lower. When the dew point temperature of the atmosphere exceeds 0 ° C., externally oxidized SiO 2 is formed on the surface of the steel sheet, and the decarburization property is hindered in the subsequent decarburization annealing. The lower limit of the dew point temperature of the atmosphere is not particularly limited, but may be −50 ° C. from the viewpoint of equipment and manufacturing cost. The oxygen concentration in the atmosphere may be 0.05% or less, more preferably 0.03% or less. The oxygen concentration is preferably lower, but the lower limit may be 0.0001% from the viewpoint of equipment and manufacturing cost. The atmospheric gas composition may contain nitrogen as a main component, or may further contain argon or helium. Further, hydrogen may be contained in order to improve the reducing property of the atmosphere.
[0047]
　When the dew point temperature in the atmosphere of the plate thickness reduction and the rapid temperature rise during pickling is not strictly controlled, the external oxide SiO 2 is formed on the surface of the steel sheet by the rapid temperature rise . The reason for this is not clear, but it is presumed that when the temperature rise rate is high, the residence time in the low temperature region where iron-based oxides are formed becomes short, and the formation of external oxide SiO 2 on the steel sheet surface is promoted. Will be done. When heating rate is slow, the iron-based oxide on the surface of the steel sheet at a low-temperature region external oxide SiO 2 to be formed prior to, external oxide SiO 2 is estimated that the formation of is inhibited.
[0048]
　The rapidly heated cold-rolled steel sheet is decarburized and annealed in a moist atmosphere containing hydrogen and nitrogen at a temperature of 900 ° C. or lower for 30 seconds to 10 minutes. In the primary recrystallization annealing consisting of rapid temperature rise and decarburization annealing, the cold-rolled steel sheet may be subjected to reduction annealing following decarburization annealing for the purpose of improving magnetic properties and coating properties. The rapid temperature rise and decarburization annealing may be performed as separate steps, but may be performed continuously from the viewpoint of omitting the production line. When rapid temperature rise and decarburization annealing are continuously performed, the rapid temperature rise and decarburization annealing may be connected by a throat or the like, and the dew point temperature at the throat may be set to 0 ° C. or lower.
[0049]
　An annealing separator containing MgO as a main component is applied to the cold-rolled steel sheet after primary recrystallization annealing, and then finish annealing is performed to obtain a finish annealing sheet. In finish annealing, secondary recrystallization occurs. Further, after the annealing separating agent is applied, the finish annealing is performed to form a forsterite film on the surface of the silicon steel plate. Finish annealing may be performed by holding a coiled cold-rolled steel sheet to which an annealing separator has been applied for 20 hours or more at a temperature of 800 ° C. to 1000 ° C. using, for example, a batch type heating furnace or the like. Good. Further, in order to further reduce the iron loss value of the finally obtained grain-oriented electrical steel sheet, a purification treatment may be performed in which the coiled finish annealed plate is heated to a temperature of about 1200 ° C. and then held. ..
[0050]
　The average heating rate in the process of raising the temperature of the finish annealing is not particularly limited, and general finish annealing conditions may be used. For example, the average heating rate in the temperature raising process of finish annealing may be 5 ° C./h to 100 ° C./h from the viewpoint of productivity and general equipment restrictions. Further, the temperature raising process of the finish annealing may be performed by another known heat pattern. The atmospheric gas composition in the finish annealing is not particularly limited. In the secondary recrystallization process at the time of finish annealing, a mixed gas of nitrogen and hydrogen may be used. It may be a dry atmosphere or a moist atmosphere. The atmosphere gas composition of the purification treatment may be dry hydrogen gas.
[0051]
　After finish annealing, an insulating film containing, for example, aluminum phosphate or colloidal silica as a main component is applied to the surface of the finish annealing plate for the purpose of imparting insulation and tension to the steel sheet. After that, flattening annealing is performed for the purpose of flattening the shape of the steel sheet deformed by the baking of the insulating film and the finish annealing. The components of the insulating coating are not particularly limited as long as the finished annealed plate is provided with insulating properties and tension.
[0052]
　In the method for manufacturing grain-oriented electrical steel sheet according to the present embodiment, in order to prevent unnecessary strain from being introduced into the grain-oriented electrical steel sheet, the ultimate temperature of flattening annealing, the holding time of 800 ° C. or higher, and the flattening annealing The tension of the steel sheet is strictly controlled. As a result, in the manufacturing method according to the present embodiment, it is possible to stably manufacture a grain-oriented electrical steel sheet having a reduced iron loss value.
[0053]
　Specifically, the ultimate temperature Af in flattening annealing is 800 ° C. or higher and 950 ° C. or lower. In the flattening annealing, when the ultimate temperature Af is less than 800 ° C., the shape of the grain-oriented electrical steel sheet cannot be completely corrected, and it becomes difficult to sufficiently flatten the grain-oriented electrical steel sheet. When the ultimate temperature Af exceeds 950 ° C., strain is introduced into the grain-oriented electrical steel sheet, which increases the possibility of increasing iron loss.
[0054]
　The holding time Tf at 800 ° C. or higher in the flattening annealing is 10 seconds or more and 100 seconds or less. When the holding time Tf of 800 ° C. or higher is less than 10 seconds, the shape of the grain-oriented electrical steel sheet cannot be completely corrected, and it becomes difficult to sufficiently flatten the grain-oriented electrical steel sheet. When the holding time Tf of 800 ° C. or higher is more than 100 seconds, the possibility that iron loss increases due to the introduction of strain into the grain-oriented electrical steel sheet increases.
[0055]
　The steel sheet tension Cf at the time of flattening annealing is 3.92 N / mm 2 or more and 11.8 N / mm 2 or less. When the steel sheet tension Cf of the flattening annealing is less than 3.92 N / mm 2 , the shape of the grain- oriented electrical steel sheet cannot be completely corrected, and it becomes difficult to sufficiently flatten the grain- oriented electrical steel sheet. When the steel sheet tension Cf of the flattening annealing is more than 11.8 N / mm 2 , the iron loss increases due to the introduction of strain into the grain- oriented electrical steel sheet.
[0056]
　The grain-oriented electrical steel sheet can be manufactured by the manufacturing method described above. The grain-oriented electrical steel sheet according to an embodiment of the present invention produced by the above-mentioned manufacturing method includes a silicon steel sheet, a forsterite film arranged on the silicon steel sheet, and an insulating film arranged on the forsterite film. Has. First, the silicon steel plate will be described.
[0057]
　The composition of the silicon steel sheet is mass%,
Si: 2.5% or more and 4.5% or less,
Mn: 0.01% or more and 0.15% or less,
C: 0% or more and 0.0050% or less,
S. And Se total: 0% or more and 0.005% or less,
acid-soluble Al: 0% or more and 0.01% or less,
N: 0% or more and 0.005% or less,
Cu: 0% or more and 0.30% or less,
Sn : 0% or more and 0.30% or less,
Ni: 0% or more and 0.30% or less,
Cr: 0% or more and 0.30% or less, and
Sb: 0% or more and 0.30% or less
, and the balance is Fe. and consists impurities,
　an average particle size of the secondary recrystallized grains of the silicon steel sheet is not less 10mm or more 50mm or less,
　the grain-oriented electrical steel sheet is
　　has a plate thickness is 0.15mm or 0.23mm or less,
　　the iron loss Wp Is 0.800 W / kg or less at W 17/50 ,
　　and Wp / Wd, which is the ratio of the iron loss Wp to the iron loss Wd when the magnetic domain is controlled, is 1.03 or more at W 17/50 . It is 15 or less, and the
　　magnetic flux density B8 value is 1.930T or more.
[0058]
　In the grain-oriented electrical steel sheet according to the present embodiment, in order to reduce iron loss without performing magnetic domain control treatment, Si, Mn and C are contained in the component composition contained in the silicon steel sheet of the grain-oriented electrical steel sheet. It is important to control the amount.
[0059]
　Si reduces the eddy current loss that forms part of the iron loss by increasing the electrical resistance of the silicon steel plate. It is desirable that Si is contained in the silicon steel sheet in the range of 2.5% or more and 4.5% or less in mass%. Preferably, it is 2.7% or more, or 4.0% or less. When the Si content is less than 2.5%, it becomes difficult to suppress the eddy current loss of the grain-oriented electrical steel sheet. When the Si content is more than 4.5%, the workability of the grain-oriented electrical steel sheet is lowered.
[0060]
　Mn forms MnS and MnSe, which are inhibitors that influence secondary recrystallization. It is desirable that Mn is contained in the silicon steel sheet in the range of 0.01% or more and 0.15% or less in mass%. Preferably, it is 0.03% or more, or 0.13% or less. When the Mn content is less than 0.01%, the absolute amounts of MnS and MnSe that cause secondary recrystallization are insufficient, and the orientation cannot be preferably controlled. When the Mn content exceeds 0.15%, it becomes difficult to dissolve Mn during slab heating, and the precipitation size of the inhibitor becomes coarse, so that the optimum size distribution of the inhibitor is impaired, and the inhibitor is preferably used. I can't control it.
[0061]
　C is an element effective for structure control until the completion of decarburization annealing in the manufacturing process. However, if the C content is more than 0.0050% even after decarburization annealing, magnetic aging is caused and the magnetic properties of the grain-oriented electrical steel sheet are deteriorated. Therefore, the C content is 0.0050% or less. Preferably, it is 0.0030% or less. On the other hand, it is preferable that the C content is low, but even if the C content is reduced to less than 0.0001%, the effect of tissue control is saturated and the production cost increases. Therefore, the C content may be 0.0001% or more.
[0062]
　The rest of the silicon steel plate according to this embodiment is Fe and impurities. However, instead of a part of Fe which is the balance, S, Se, acid-soluble Al and N, and any one of Cu, Sn, Ni, Cr and Sb as an element for stabilizing secondary recrystallization. It may contain seeds or two or more species. It is not necessary to limit the lower limit of these selective elements, and the lower limit may be 0%.
[0063]
　The contents of S and Se are preferably low, but the total content may be 0.005% or less. If the total content of S and Se is more than 0.005%, magnetic aging may occur and the magnetic properties may deteriorate.
The content of acid-soluble Al is preferably low, but may be 0.01% or less. If the content of acid-soluble Al is more than 0.01%, magnetic aging may occur and the magnetic properties may deteriorate.
The N content is preferably low, but may be 0.005% or less. If the N content is more than 0.005%, magnetic aging may occur and the magnetic properties may deteriorate.
[0064]
　The content of each of Cu, Sn, Ni, Cr and Sb may be 0.01% or more and 0.30% or less. When the content of even one of these elements is 0.01% or more, the effect of stabilizing secondary recrystallization can be sufficiently obtained, the iron loss value can be further reduced, and it is better. Magnetic properties can be obtained. When the content of even one of these elements exceeds 0.30%, the effect of stabilizing secondary recrystallization is saturated, which is preferable from the viewpoint of suppressing an increase in the manufacturing cost of grain-oriented electrical steel sheets. Absent.
[0065]
　The composition of the silicon steel sheet may be measured by using ICP-AES (Inductively Coupled Plasma-Atomic Measurement Spectrum) for the obtained silicon steel sheet after removing the insulating film and the forsterite film of the grain-oriented electrical steel sheet. In addition, C and S may be measured by using the combustion-infrared absorption method, and N may be measured by using the inert gas melting-thermal conductivity method.
　Specifically, the method for removing the insulating film and the forsterite film is as follows. NaOH: 20% by mass + H 2 O: to 80% by weight aqueous sodium hydroxide, 20 minutes at 80 ° C., after soaking the grain-oriented electrical steel sheet, followed by drying and washing with water, the insulating film of the grain-oriented electrical steel sheet Remove. Next, HCl: 20% by mass + H 2 O: to the 80 wt% aqueous hydrochloric acid solution, 2 minutes at 50 ° C., after soaking the grain-oriented electrical steel sheet removing the insulating coating, followed by drying and washing with water, directional The forsterite coating on the electromagnetic steel sheet is removed to obtain a silicon steel sheet. The time of immersion in the above-mentioned sodium hydroxide aqueous solution or hydrochloric acid aqueous solution may be changed according to the thickness of the coating film.
[0066]
　In the silicon steel plate according to the present embodiment, the average particle size of the secondary recrystallized grains is controlled. Specifically, in the silicon steel sheet according to the present embodiment, the average particle size of the secondary recrystallized grains is 10 mm or more and 50 mm or less.
[0067]
　When the average particle size of the secondary recrystallized grains of the silicon steel sheet is more than 50 mm, the iron loss value (particularly, eddy current loss) of the grain-oriented electrical steel sheet becomes large. Therefore, the average particle size of the secondary recrystallized grains of the silicon steel sheet is set to 50 mm or less. It is preferably 40 mm or less. The lower limit of the average particle size of the secondary recrystallized grains may be 10 mm in order to satisfy the magnetic characteristics of the grain-oriented electrical steel sheet according to the present embodiment.
[0068]
　The average particle size of the secondary recrystallized grains of the silicon steel sheet can be measured by, for example, the following method.
　First, a silicon steel sheet is obtained by removing the insulating film and the forsterite film of the grain-oriented electrical steel sheet by the same method as described above. Since the obtained silicon steel plate has a pit pattern formed on the surface of the steel plate according to the crystal orientation during immersion in the hydrochloric acid aqueous solution, the steel structure of the silicon steel plate can be observed. A test piece is cut out so that the observation surface has at least a width of 60 mm and a length of 300 mm, and the steel structure of the silicon steel plate exposed by the above method is observed, and the grain boundaries of the crystal grains that can be visually recognized are oil-based pens. Trace with. At least five images of the surface of the grain-oriented electrical steel sheet are acquired using a commercially available image scanner device, and the acquired images are analyzed using commercially available image analysis software. After measuring the equivalent circle diameter of the crystal grains of the directional electromagnetic steel plate in all images by image analysis, the average value of the measured equivalent circle diameters is calculated to average the secondary recrystallized grains of the directional electromagnetic steel plate. Obtain the particle size.
　For example, small crystal grains having a particle size of less than 2 mm, which are difficult to identify visually, are excluded from the measurement of the particle size of the secondary recrystallized grains.
[0069]
　The forsterite film is mainly composed of Mg 2 SiO 4 , and contains a small amount of impurities and additives contained in the silicon steel plate and the annealing separator and their reaction products.
　The insulating film is mainly composed of phosphate and colloidal silica, and contains a small amount of elements and impurities diffused from the silicon steel sheet during purification annealing and their reaction products. In addition, a component other than the above may be used as long as the insulating property and the tension on the steel sheet can be obtained.
[0070]
　The thickness of the grain-oriented electrical steel sheet according to this embodiment is 0.15 mm or more and 0.23 mm or less. When the thickness of the grain-oriented electrical steel sheet is less than 0.15 mm, the load of cold rolling increases remarkably. When the thickness of the grain-oriented electrical steel sheet exceeds 0.23 mm, the iron loss deteriorates.
[0071]
　The thickness of the grain-oriented electrical steel sheet may be determined by measuring with radiation or the like. For simplicity, a sample of a predetermined size may be taken from a grain-oriented electrical steel sheet by shearing and calculated by converting it from the weight of the steel sheet using the iron density. Further, it may be obtained by converting from the coil diameter and the number of steel plate turns. The iron density is preferably selected according to the amount of Si contained.
[0072]
　The magnetic flux density B8 value of the grain-oriented electrical steel sheet according to this embodiment is 1.930 T or more. Here, the magnetic flux density B8 value is an average value of the magnetic flux densities obtained by applying a magnetic field of 800 A / m at 50 Hz to five or more samples collected from grain-oriented electrical steel sheets.
　When the magnetic flux density B8 value of the grain-oriented electrical steel sheet is less than 1.930 T, the iron loss value (particularly, hysteresis loss) of the grain-oriented electrical steel sheet becomes large. Preferably, the lower limit of the magnetic flux density B8 value of the grain-oriented electrical steel sheet is 1.932T. The upper limit of the magnetic flux density B8 value is not particularly limited, but may be 2.000T, for example. The magnetic properties of the grain-oriented electrical steel sheet, such as the magnetic flux density, can be measured by a known method. For example, the magnetic properties of grain-oriented electrical steel sheets include a method based on the Epstein test specified in JIS C 2550: 2011, or a single plate magnetic property test method (Single Sheet Tester: SST) specified in JIS C 2556: 2015. Can be measured by using. In research and development, when steel ingots are formed in a vacuum melting furnace or the like, it becomes difficult to collect test pieces of the same size as those manufactured in the actual machine. In this case, for example, a test piece may be collected so as to have a width of 60 mm and a length of 300 mm, and measurement may be performed in accordance with the single plate magnetic property test method. Further, the obtained result may be multiplied by a correction coefficient so that a measured value equivalent to that of the method based on the Epstein test can be obtained. In the present embodiment, the measurement is performed by a measurement method based on the single plate magnetic property test method.
[0073]
　As described above, the grain-oriented electrical steel sheet according to the present embodiment can reduce the iron loss value. Specifically, in the grain- oriented electrical steel sheet according to the present embodiment, the iron loss Wp when the magnetic domain control treatment is not performed is W 17/50 , which is 0.800 W / kg or less. Preferably, it is 0.790 W / kg or less. The lower limit is not particularly limited, but may be 0.600 W / kg from the viewpoint of industrial stable manufacturability.
[0074]
　In the grain-oriented electrical steel sheet according to the present embodiment, Wp / Wd, which is the ratio of the iron loss Wp when the magnetic domain control treatment is not applied and the iron loss Wd when the magnetic domain control treatment is applied, is W 17/50 . It is 1.15 or less. It is preferably 1.14 or less. The lower limit is not particularly limited, but may be 1.03 from the viewpoint of industrial stable manufacturability.
[0075]
　The grain-oriented electrical steel sheet according to the present embodiment can sufficiently reduce iron loss even if magnetic domain control treatment is not performed. Therefore, the grain-oriented electrical steel sheet according to the present embodiment can have both the magnetic characteristics of the transformer and the noise characteristics.
[0076]
　For the iron loss Wp when the magnetic domain control treatment is not performed, the value measured on the grain-oriented electrical steel sheet after strain annealing is used. For the iron loss Wd when the magnetic domain control treatment is performed, the minimum iron loss value of the grain-oriented electrical steel sheet whose magnetic domain control treatment is performed so that the iron loss is saturated is used. For the minimum iron loss value, for example, the irradiation interval P in the longitudinal direction of the steel plate is 4 mm, the laser irradiation direction is perpendicular to the longitudinal direction of the steel plate, and the irradiation energy density Ua is changed by 0.2 mmJ / mm 2. It is obtained by measuring the iron loss of the laser-irradiated sample. W 17/50 is the average value of iron loss obtained by exciting five or more samples collected from grain- oriented electrical steel sheets to 1.7 T at 50 Hz.
[0077]
　According to the manufacturing method according to the present embodiment, it is possible to manufacture grain-oriented electrical steel sheets with sufficiently reduced iron loss without performing magnetic domain control processing. By using the grain-oriented electrical steel sheet according to the present embodiment as the iron core material of the transformer, both the magnetic characteristics and the noise characteristics of the transformer can be improved.
[0078]
　Needless to say, in the present embodiment, the magnetic domain control treatment may be applied to the grain-oriented electrical steel sheet depending on the purpose of the customer. However, in the grain-oriented electrical steel sheet according to the present embodiment, the reduction of the iron loss value before and after the magnetic domain control process is small, and it is assumed that the noise of the transformer is increased by the magnetic domain control process.
Example
[0079]
　(Example 1) In
　mass%, C: 0.08%, Si: 3.3%, Mn: 0.08%, S: 0.024%, acid-soluble Al: 0.03%, N: 0. A steel ingot containing 008% and having the balance of Fe and impurities was prepared. The ingot was heated at 1350 ° C. for 1 hour and then hot-rolled to obtain a hot-rolled steel sheet having a thickness of 2.3 mm. The obtained hot-rolled steel sheet is annealed at a maximum temperature of 1100 ° C. for 140 seconds, pickled so that the thickness loss is 50 μm, and then cold-rolled to achieve a plate thickness of 0. A .23 mm cold rolled steel sheet was obtained.
[0080]
　Subsequently, the obtained cold-rolled steel sheet was rapidly heated at an average heating rate of Va (° C./s) shown in Table 1A in an atmosphere of 1 vol% hydrogen-99 vol% nitrogen and a dew point temperature of -20 ° C. Primary recrystallization annealing was performed in a moist hydrogen atmosphere at 850 ° C. for 180 seconds. The average heating rate Va (° C./s) is the average value of the heating rate in the temperature range of 550 ° C. to 700 ° C., and during the rapid temperature rise of the primary recrystallization annealing, in the direction of passing the cold-rolled steel sheet. Granted the steel plate tension Sa (N / mm 2 ) shown in Table 1A below .
[0081]
　Next, an annealing separator containing MgO was applied to the surface of the cold-rolled steel sheet after primary recrystallization annealing, and then finish annealing was performed to obtain a finish annealing plate, and the finish annealing plate was washed with water. Then, an insulating film containing aluminum phosphate and colloidal silica as main components is applied to the surface of the finished annealed sheet, and then flattened and annealed for the purpose of baking the insulating film and flattening the steel sheet under the conditions shown in Table 1A. A directional electromagnetic steel sheet having a plate thickness of 0.15 mm or more and 0.23 mm or less was obtained. Here, in the flattening annealing, the ultimate temperature Af (° C.) of the flattening annealing, the holding time Tf (s) of 800 ° C. or higher, and the steel plate tension Sf (N / mm 2 ) are set for each of the examples of the present invention and the comparative example. Each was controlled.
[0082]
　Five samples were taken by shearing from the grain-oriented electrical steel sheets obtained by the above method, and after strain-removal annealing was applied to these samples, the single-plate magnetic property test method described in JIS C 2556: 2015 was applied. The magnetic flux density B8 value and the iron loss Wp were measured. The iron loss Wp was measured at W 17/50 for 5 samples, and was taken as the average value of the iron loss obtained by exciting to 1.7 T at 50 Hz. The magnetic flux density B8 value was taken as the average value of the magnetic flux densities obtained by applying a magnetic field of 800 A / m at 50 Hz to five samples.
[0083]
　Further, the above sample was subjected to magnetic domain control treatment, and the iron loss Wd when the magnetic domain control treatment was performed was measured at W 17/50 in accordance with the single plate magnetic property test method described in JIS C 2556: 2015 . The magnetic domain control process was performed by laser irradiation. The direction of laser irradiation was set to be perpendicular to the longitudinal direction of the grain-oriented electrical steel sheet, and the laser irradiation interval P was set to 4 mm. The laser irradiation energy density Ua was 1.5 mJ / mm 2 . The irradiation energy density Ua described above is a condition in which it was confirmed in a preliminary test that W 17/50 of the sample was saturated. The iron loss Wd was also taken as the average value of 5 samples.
[0084]
　With respect to the obtained grain-oriented electrical steel sheet, after removing the insulating film and the forsterite film by the above method, the component composition of the silicon steel sheet was measured using ICP-AES. The C content was measured using the combustion-infrared absorption method. Further, the secondary recrystallized grains of the silicon steel sheet were measured by the above method.
[0085]
　When the magnetic flux density B8 value was 1.930 T or more, the iron loss Wp was 0.800 or less, and the Wp / Wd was 1.03 or more and 1.15 or less, it was judged as acceptable. If any one of these conditions was not met, it was judged to be unacceptable and "C" was entered in the evaluation column in the table. In addition, if the shape is not sufficiently flattened, it is judged as unacceptable because it cannot be used for grain-oriented electrical steel sheets, measurement of magnetic flux density B8 value, etc. is omitted, and "C (C (" Shape) ”. The iron loss Wp of the example judged to be acceptable was evaluated based on the following criteria.
S (extremely good): Iron loss Wp is 0.785 or less.
A (better): Iron loss Wp is more than 0.785 W / kg and 0.790 W / kg or less.
B (good): Iron loss Wp 0.790 W / kg or more and 0.800 W / kg or less.
[0086]
　Table 1A and Table 1B show the manufacturing conditions, measurement results, and evaluation results of grain-oriented electrical steel sheets. In the example of the present invention, in the composition of the silicon steel sheet, the total content of S and Se is 0.005% or less, the acid-soluble Al content is 0.01% or less, and the N content is 0. It was less than .005%, and the balance was Fe and impurities.
[0087]
[Table 1A]

[0088]
[Table 1B]

[0089]
　Looking at Table 1B, it was found that the grain-oriented electrical steel sheet (example of the present invention) satisfying the conditions of the present embodiment had an evaluation of B (good) or higher. Further, in the example of the present invention in which the average heating rate Va at 550 ° C. to 700 ° C. in the primary recrystallization annealing was 700 ° C./s or more, the iron loss Wp was 0.790 W / kg or less, so the judgment was A or more. It turned out to be (better or better). Further, in the example of the present invention in which the average heating rate Va at 550 ° C. to 700 ° C. in the primary recrystallization annealing was 1000 ° C./s or more, the iron loss Wp was 0.785 W / kg or less, so the determination was S ( It turned out to be very good).
[0090]
　Here, FIG. 1 shows a graph in which the results shown in Tables 1A and 1B are plotted with the average temperature rise rate Va on the horizontal axis and the steel plate tension Sa on the vertical axis. As shown in FIG. 1, when the example of the present invention is plotted with round dots and the comparative example is plotted at intersections, the average rate of temperature rise Va (° C./s) in the rapid temperature rise of the primary recrystallization annealing and the steel plate tension Sa ( It was found that there is a relationship between the following formulas 1 and 2 defined in the conditions according to the present embodiment with N / mm 2 ). Note that FIG. 1 does not plot the condition A1 in which the average temperature rising rate Va of 550 ° C. to 700 ° C. in the primary recrystallization annealing deviates from the condition according to the present embodiment.
[0091]
　1.96 ≤ Sa ≤ (25.5-0.0137 x Va) (Va ≤ 1000) ... Equation 1
　1.96 ≤ Sa ≤ 11.8 (Va> 1000) ... Equation 2
[0092]
　(Example 2) In
　mass%, C: 0.08%, Si: 3.2%, Mn: 0.08%, S: 0.025%, acid-soluble Al: 0.03%, N: 0. A steel ingot containing 008% and having the balance of Fe and impurities was prepared. The ingot was heated at 1350 ° C. for 1 hour and then hot-rolled to obtain a hot-rolled steel sheet having a thickness of 2.3 mm. The obtained hot-rolled steel sheet is annealed at a maximum temperature of 1100 ° C. for 140 seconds, then pickled so as to reduce the thickness shown in Table 2A, and then cold-rolled. A cold-rolled steel sheet having a thickness of 0.23 mm was obtained.
[0093]
　Subsequently, the obtained cold-rolled steel sheet was rapidly heated at the average heating rate Va (° C./s) shown in Table 2A in an atmosphere of hydrogen 2vol% -nitrogen 98vol% and the dew point temperature shown in Table 2A. The primary recrystallization annealing was performed at 850 ° C. for 180 seconds in a wet hydrogen atmosphere. During the rapid temperature rise of the primary recrystallization annealing, the steel sheet tension Sa (N / mm 2 ) shown in Table 2A was applied in the sheet passing direction of the cold-rolled steel sheet .
[0094]
　Next, an annealing separator containing MgO was applied to the surface of the cold-rolled steel sheet after primary recrystallization annealing, and then finish annealing was performed to obtain a finish annealing plate, and the finish annealing plate was washed with water. Then, after applying an insulating film containing aluminum phosphate and colloidal silica as main components to the surface of the finished annealed sheet, the sheet thickness is obtained by baking the insulating film and performing flattening annealing for the purpose of flattening the steel sheet. A grain-oriented electrical steel sheet having a thickness of 0.15 mm or more and 0.23 mm or less was obtained. Here, the ultimate temperature Af for flattening annealing was 850 ° C., the holding time Tf at 800 ° C. or higher was 40 seconds, and the steel plate tension Cf was 9.8 N / mm 2 .
[0095]
　With respect to the grain-oriented electrical steel sheet obtained by the above method, the magnetic flux density B8 value, iron loss Wp, Wd, the component composition of the silicon steel sheet, and the average particle size of the secondary recrystallized grains were measured by the same method as in Example 1. did.
[0096]
　When the magnetic flux density B8 value was 1.930 T or more, the iron loss Wp was 0.800 or less, and the Wp / Wd was 1.03 or more and 1.15 or less, it was judged as acceptable. If any one of these conditions was not met, it was judged to be unacceptable, and "C" was entered in the evaluation column in the table. In condition B1, the weight loss during pickling is small, the oxide (scale) formed on the surface of the steel sheet is not sufficiently removed, and the rolling roll is worn during the cold rolling performed after pickling. Therefore, cold rolling was stopped and "C (roll wear)" was described in the evaluation column. Further, the iron loss Wp of the example judged to be acceptable was evaluated as S (extremely good), A (better), and B (good) based on the same criteria as in Example 1.
[0097]
　Table 2A and Table 2B show the manufacturing conditions, measurement results, and evaluation results of grain-oriented electrical steel sheets. In the example of the present invention, in the composition of the silicon steel sheet, the total content of S and Se is 0.005% or less, the acid-soluble Al content is 0.01% or less, and the N content is 0. It was less than .005%, and the balance was Fe and impurities.
[0098]
[Table 2A]

[0099]
[Table 2B]

[0100]
　Looking at Table 2B, it was found that the grain-oriented electrical steel sheet (example of the present invention) satisfying the conditions of the present embodiment had an evaluation of B (good) or higher. Further, in the example of the present invention in which the average heating rate Va at 550 ° C. to 700 ° C. in the primary recrystallization annealing was 700 ° C./s or more, the iron loss Wp was 0.790 W / kg or less, so the judgment was A or more. It turned out to be (better or better). Further, in the example of the present invention in which the average heating rate Va at 550 ° C. to 700 ° C. in the primary recrystallization annealing was 1000 ° C./s or more, the iron loss Wp was 0.785 W / kg or less, so the determination was S ( It turned out to be very good).
[0101]
　(Example 3) In
　mass%, C: 0.08%, Si: 3.2%, Mn: 0.08%, S: 0.005%, Se: 0.019%, acid-soluble Al: 0. A steel ingot containing 03% and N: 0.008% and having the balance of the components shown in Table 3A, Fe and impurities was prepared. The ingot was heated at 1350 ° C. for 1 hour and then hot-rolled to obtain a hot-rolled steel sheet having a thickness of 2.3 mm. The obtained hot-rolled steel sheet is annealed at a maximum temperature of 1100 ° C. for 140 seconds, pickled so that the thickness loss is 10 μm, and then cold-rolled to achieve a plate thickness of 0. A .23 mm cold rolled steel sheet was obtained.
[0102]
　Subsequently, the obtained cold-rolled steel sheet was rapidly subjected to an atmosphere of 1 vol% hydrogen-99 vol% nitrogen and a dew point temperature of -30 ° C so that the average heating rate Va at 550 ° C to 700 ° C became 1000 ° C / s. After the temperature was raised, primary recrystallization annealing was performed in a moist hydrogen atmosphere at 850 ° C. for 180 seconds. During the rapid temperature rise of the primary recrystallization annealing, a steel sheet tension Sa of 7.84 N / mm 2 was applied in the sheet passing direction of the cold-rolled steel sheet .
[0103]
　Next, an annealing separator containing MgO was applied to the surface of the cold-rolled steel sheet after primary recrystallization annealing, and then finish annealing was performed to obtain a finish annealing plate, and the finish annealing plate was washed with water. Then, after applying an insulating film containing aluminum phosphate and colloidal silica as main components to the surface of the finished annealed sheet, the sheet thickness is obtained by baking the insulating film and performing flattening annealing for the purpose of flattening the steel sheet. A grain-oriented electrical steel sheet having a thickness of 0.15 mm or more and 0.23 mm or less was obtained. Here, the ultimate temperature Af for flattening annealing was 850 ° C., the holding time Tf at 800 ° C. or higher was 40 seconds, and the steel plate tension Cf was 9.8 N / mm 2 .
[0104]
　With respect to the grain-oriented electrical steel sheet obtained by the above method, the magnetic flux density B8 value, iron loss Wp, Wd, the component composition of the silicon steel sheet, and the average particle size of the secondary recrystallized grains were measured by the same method as in Example 1. did.
[0105]
　When the magnetic flux density B8 value was 1.930 T or more, the iron loss Wp was 0.800 or less, and the Wp / Wd was 1.03 or more and 1.15 or less, it was judged as acceptable. Further, the iron loss Wp of the example judged to be acceptable was evaluated as S (extremely good), A (better), and B (good) based on the same criteria as in Example 1.
[0106]
　The measurement results and evaluation results obtained by the above method are shown in Tables 3A and 3B. In the example of the present invention, in the composition of the silicon steel sheet, the total content of S and Se is 0.005% or less, the acid-soluble Al content is 0.01% or less, and the N content is 0. It was less than .005%, and the balance was Fe and impurities.
[0107]
[Table 3A]

[0108]
[Table 3B]

[0109]
　Referring to Table 3B, in terms of mass%, Cu: 0.01% or more and 0.30% or less, Sn: 0.01% or more and 0.30% or less, Ni: 0.01% or more and 0.30% or less, Cr A grain-oriented electrical steel sheet having a component composition containing any one or more of 0.01% or more and 0.30% or less, or Sb: 0.01% or more and 0.30% or less has iron loss Wp. Was 0.780 or less, and it was found that the iron loss Wp was further reduced.
[0110]
　(Example 4)
　C: 0.08%, S: 0.023%, acid-soluble Al: 0.03%, N: 0.008% in mass%, and the balance is the content shown in Table 4. A steel ingot composed of Si and Mn of No. 1 and Fe and impurities was prepared. The ingot was heated at 1350 ° C. for 1 hour and then hot-rolled to obtain a hot-rolled steel sheet having a thickness of 2.3 mm. The obtained hot-rolled steel sheet is annealed at a maximum temperature of 1100 ° C. for 140 seconds, pickled so that the thickness loss is 20 μm, and then cold-rolled to achieve a plate thickness of 0. A .23 mm cold rolled steel sheet was obtained.
[0111]
　Subsequently, the obtained cold-rolled steel sheet was rapidly heated at the average temperature rise rate Va (° C./s) shown in Table 4 in a nitrogen atmosphere and an atmosphere of a dew point temperature of −30 ° C., and then in a wet hydrogen atmosphere and 850 ° C. Primary recrystallization annealing was performed by decarburizing and annealing at ° C. for 180 seconds. The average heating rate Va (° C./s) is the average value of the heating rate from 550 ° C. to 700 ° C., and during the rapid temperature rise of the primary recrystallization annealing, the temperature is increased in the passing direction of the cold-rolled steel sheet. A steel plate tension Sa of 7.84 N / mm 2 was applied.
[0112]
　Next, an annealing separator containing MgO was applied to the surface of the cold-rolled steel sheet after primary recrystallization annealing, and then finish annealing was performed to obtain a finish annealing plate, and the finish annealing plate was washed with water. Then, after applying an insulating film containing aluminum phosphate and colloidal silica as main components to the surface of the finished annealed sheet, the sheet thickness is obtained by baking the insulating film and performing flattening annealing for the purpose of flattening the steel sheet. A grain-oriented electrical steel sheet having a thickness of 0.15 mm or more and 0.23 mm or less was obtained. Here, the ultimate temperature Af for flattening annealing was 850 ° C., the holding time Tf at 800 ° C. or higher was 40 seconds, and the steel plate tension Cf was 9.8 N / mm 2 .
[0113]
　With respect to the grain-oriented electrical steel sheet obtained by the above method, the magnetic flux density B8 value, iron loss Wp, Wd, the component composition of the silicon steel sheet, and the average particle size of the secondary recrystallized grains were measured by the same method as in Example 1. did.
[0114]
　When the magnetic flux density B8 value was 1.930 T or more, the iron loss Wp was 0.800 or less, and the Wp / Wd was 1.03 or more and 1.15 or less, it was judged to be acceptable. If any one of these conditions was not met, it was judged to be unacceptable, and "C" was entered in the evaluation column in the table. Condition D5 was judged to be unacceptable because the Si content in the ingot was high and cold rolling could not be performed, measurement of the magnetic flux density B8 value, etc. was omitted, and "C (rolling)" was entered in the evaluation column. Impossible) ”. Further, the iron loss Wp of the example judged to be acceptable was evaluated as S (extremely good), A (better), and B (good) based on the same criteria as in Example 1.
[0115]
　Table 4 shows the manufacturing conditions, measurement results, and evaluation results of grain-oriented electrical steel sheets. In the example of the present invention, regarding the composition of the silicon steel sheet, the total content of S and Se is 0.005% or less, the acid-soluble Al content is 0.01% or less, and the N content is 0. It was less than .005%, and the balance was Fe and impurities.
[0116]
[Table 4]

[0117]
　Referring to Table 4, grain-oriented electrical steel sheets having a Si content of 2.5% or more and 4.5% or less, or a Mn content of 0.01% or more and 0.15% or less in mass%. It was found that the iron loss Wp deteriorated.
[0118]
　(Example 5) In
　mass%, C: 0.08%, Si: 3.3%, Mn: 0.08%, S: 0.024%, acid-soluble Al: 0.03%, N: 0. A steel ingot containing 008% and having the balance of Fe and impurities was prepared. The ingot was heated at 1350 ° C. for 1 hour and then hot-rolled to obtain a hot-rolled steel sheet having a thickness of 2.3 mm. The obtained hot-rolled steel sheet is annealed at a maximum temperature of 1100 ° C. for 140 seconds, pickled so that the thickness loss is 50 μm, and then cold-rolled to achieve a plate thickness of 0. A .23 mm cold rolled steel sheet was obtained.
[0119]
　Subsequently, the obtained cold-rolled steel sheet was rapidly heated at an average heating rate of Va (° C./s) shown in Table 5A in an atmosphere of hydrogen 3 vol% -nitrogen 97 vol% and a dew point temperature of -30 ° C. Primary recrystallization annealing was performed in a moist hydrogen atmosphere at 850 ° C. for 180 seconds by decarburization annealing. The average heating rate Va (° C./s) is the average value of the heating rate from 550 ° C. to 700 ° C., and during the rapid temperature rise of the primary recrystallization annealing, the temperature is increased in the passing direction of the cold-rolled steel sheet. The steel plate tension Sa (N / mm 2 ) shown in Table 5A was applied.
[0120]
　Next, an annealing separator containing MgO was applied to the surface of the cold-rolled steel sheet after primary recrystallization annealing, and then finish annealing was performed to obtain a finish annealing plate, and the finish annealing plate was washed with water. Then, after applying an insulating film containing aluminum phosphate and colloidal silica as main components to the surface of the finished annealed sheet, the sheet thickness is obtained by baking the insulating film and performing flattening annealing for the purpose of flattening the steel sheet. A grain-oriented electrical steel sheet having a thickness of 0.15 mm or more and 0.23 mm or less was obtained. Here, the ultimate temperature Af for flattening annealing was 850 ° C., the holding time Tf at 800 ° C. or higher was 40 seconds, and the steel plate tension Cf was 9.8 N / mm 2 .
[0121]
　With respect to the grain-oriented electrical steel sheet obtained by the above method, the magnetic flux density B8 value, iron loss Wp, Wd, the component composition of the silicon steel sheet, and the average particle size of the secondary recrystallized grains were measured by the same method as in Example 1. did.
[0122]
　When the iron loss Wp is 0.800 or less, the magnetic flux density B8 value is 1.930T or more, and Wp / Wd is 1.03 or more and 1.15 or less, it is judged as acceptable. If any one of these conditions was not met, it was judged to be unacceptable, and "C" was entered in the evaluation column in the table. Further, the iron loss Wp of the example judged to be acceptable was evaluated as S (extremely good), A (better), and B (good) based on the same criteria as in Example 1.
[0123]
　Table 5A and Table 5B show the manufacturing conditions, measurement results and evaluation results of grain-oriented electrical steel sheets. In the example of the present invention, in the composition of the silicon steel sheet, the total content of S and Se is 0.005% or less, the acid-soluble Al content is 0.01% or less, and the N content is 0. It was less than .005%, and the balance was Fe and impurities.
[0124]
[Table 5A]

[0125]
[Table 5B]

[0126]
　With reference to Table 5B, it was found that the iron loss Wp deteriorates when the average particle size of the secondary recrystallized grains is out of the range of 10 mm or more and 50 mm or less, or when the magnetic flux density B8 is less than 1.930 T.
[0127]
　(Example 6) In
　mass%, C: 0.08%, Si: 3.3%, Mn: 0.08%, S: 0.025%, acid-soluble Al: 0.03%, N: 0. A steel ingot containing 008% and having the balance of Fe and impurities was prepared. The ingot was heated at 1350 ° C. for 1 hour and then hot-rolled to obtain a hot-rolled steel sheet having a plate thickness of 2.1 mm. The obtained hot-rolled steel sheet is annealed at a maximum temperature of 1100 ° C. for 140 seconds, pickled so that the thickness loss is 20 μm, and then cold-rolled. Got In the cold rolling, the cumulative rolling reduction was controlled so that the finally obtained grain-oriented electrical steel sheet had the sheet thickness shown in Table 6.
[0128]
　Subsequently, the obtained cold-rolled steel sheet was rapidly subjected to an atmosphere of hydrogen 2 vol% -nitrogen 98 vol% and a dew point temperature -30 ° C so that the average temperature rise rate Va of 550 ° C to 700 ° C became 1000 ° C / s. After the temperature was raised, decarburization annealing was performed at 850 ° C. for 180 seconds in a moist hydrogen atmosphere, and primary recrystallization annealing was performed. During the rapid temperature rise of the primary recrystallization annealing, a steel sheet tension Sa of 7.84 N / mm 2 was applied in the sheet passing direction of the cold-rolled steel sheet .
[0129]
　Next, an annealing separator containing MgO was applied to the surface of the cold-rolled steel sheet after primary recrystallization annealing, and then finish annealing was performed to obtain a finish annealing plate, and the finish annealing plate was washed with water. After that, an insulating film containing aluminum phosphate and colloidal silica as main components is applied to the surface of the finished annealed sheet, and then flattening annealing is performed for the purpose of baking the insulating film and flattening the steel sheet. An electromagnetic steel sheet was obtained. Here, the ultimate temperature Af for flattening annealing was 850 ° C., the holding time Tf at 800 ° C. or higher was 40 seconds, and the steel plate tension Cf was 9.8 N / mm 2 .
[0130]
　With respect to the grain-oriented electrical steel sheet obtained by the above method, the magnetic flux density B8 value, iron loss Wp, Wd, the component composition of the silicon steel sheet, and the average particle size of the secondary recrystallized grains were measured by the same method as in Example 1. did.
[0131]
　When the iron loss Wp is 0.800 or less, the magnetic flux density B8 value is 1.930T or more, and Wp / Wd is 1.03 or more and 1.15 or less, it is judged as acceptable. If any one of these conditions was not met, it was judged to be unacceptable, and "C" was entered in the evaluation column in the table. The iron loss Wp of the example judged to be acceptable was evaluated as S (extremely good), A (better), and B (good) based on the same criteria as in Example 1.
[0132]
　Table 6 shows the manufacturing conditions, measurement results, and evaluation results of grain-oriented electrical steel sheets. In the example of the present invention, in the composition of the silicon steel sheet, the total content of S and Se is 0.005% or less, the acid-soluble Al content is 0.01% or less, and the N content is 0. It was less than .005%, and the balance was Fe and impurities.
[0133]
[Table 6]

[0134]
　With reference to the results in Table 6, it was found that the grain-oriented electrical steel sheet having a plate thickness of 0.15 mm or more and 0.23 mm or less was judged to be B or more (good or more).
[0135]
　Although the preferred embodiments of the present invention have been described in detail with reference to the accompanying drawings, the present invention is not limited to such examples. It is clear that a person having ordinary knowledge in the field of technology to which the present invention belongs can come up with various modifications or modifications within the scope of the technical ideas described in the claims. It is naturally understood that these also belong to the technical scope of the present invention.
Industrial applicability
[0136]
　According to the above aspect according to the present invention, it is possible to manufacture a directional electric steel sheet having a lower iron loss. Specifically, according to the above aspect according to the present invention, after the primary recrystallization annealing, the number of crystal grains having a Goss orientation with good magnetic characteristics increases, so that the crystal grains after the secondary recrystallization have a Goss orientation. It is possible to manufacture a directional electromagnetic steel plate having a smaller diameter of crystal grains while improving the degree of integration. Therefore, it is possible to manufacture a grain-oriented electrical steel sheet having a further reduced iron loss value. Further, according to another aspect of the present invention, it is possible to provide a grain-oriented electrical steel sheet with reduced iron loss without performing magnetic domain control treatment.
The scope of the claims
[Claim 1]
　A method for producing a directional electromagnetic steel sheet, in which the component composition is mass%,
C: 0.02% or more and 0.10% or less,
Si: 2.5% or more and 4.5% or less,
Mn: 0.01. % Or more and 0.15% or less,
total of S and Se: 0.001% or more and 0.050% or less,
acid-soluble Al: 0.01% or more and 0.05% or less,
N: 0.002% or more and 0.015 %
Or less, Cu: 0% or more and 0.30% or less,
Sn: 0% or more and 0.30% or less,
Ni: 0% or more and 0.30% or less,
Cr: 0% or more and 0.30% or less, and
Sb: A
step of obtaining a hot-rolled steel sheet by heating a slab containing 0% or more and 0.30% or less and the balance of Fe and impurities to 1280 to 1450 ° C. and hot-rolling the slab and the
　hot-rolled steel sheet. Is pickled to obtain a pickling plate, or the hot-rolled steel plate is annealed to obtain a hot-rolled fired plate, and then the hot-rolled fired plate is pickled to obtain a pickling plate. A step of obtaining a plate, a step of obtaining a
　cold-rolled steel plate by cold-rolling the pickled plate, a step of
　subjecting the cold-rolled steel plate to primary recrystallization, and a step of
　primary re-crystallizing the cold-rolled steel plate. A process of obtaining a finished annealed plate by applying a precipitating separator containing MgO to the surface of
　In the
　pickling, the thickness loss of the hot-rolled steel sheet or the hot-rolled annealed sheet is 5 μm or more and 150 μm or less.
　In the rapid temperature rise of the primary recrystallization annealing, the dew point temperature of the atmosphere is 0 ° C. or lower, and the average temperature rise rate Va (° C./s) in the temperature range of 550 ° C. to 700 ° C. is 400 ≦ Va ≦ 3000. When the tension Sa (N / mm 2 ) applied in the sheeting direction of the cold-rolled steel sheet is Va ≦ 1000, it is 1.96 ≦ Sa ≦ (25.5-0.0137 × Va). When the tension Sa is Va> 1000, 1.96 ≦ Sa ≦ 11.8, and in the
　flattening annealing, the reached temperature Af (° C.) at the time of annealing is 800 ≦ Af ≦ 950, which is 800 ° C. or higher. The holding time Tf (seconds) is 10 ≦ Tf ≦ 100, and the tension Cf (N / mm 2 ) applied in the passing direction of the finish annealing plate during the flattening annealing is 3.92 ≦ Cf ≦ 11. A method for manufacturing a directional electromagnetic steel sheet, which is characterized by being 8.
[Claim 2]
　In terms of mass%, the component composition of the slab is
Cu: 0.01% or more and 0.30% or less,
Sn: 0.01% or more and 0.30% or less,
Ni: 0.01% or more and 0.30% or less. The direction according to claim 1 , wherein
Cr: 0.01% or more and 0.30% or less, and
Sb: 0.01% or more and 0.30% or less
are contained in one or more kinds. Manufacturing method of electrical steel sheet.
[Claim 3]
　A
　grain-
　oriented electrical steel sheet having a silicon steel sheet, a forsterite film arranged on the silicon steel sheet, and an insulating film arranged on the forsterite film, and the
　silicon steel sheet has a component composition of mass%.
in, Si: 2.5% to 4.5% or
less, Mn: 0.01% or more and 0.15% or
less, C: 0% or more 0.0050% or less,
the total of S and Se: 0% or more 0. 005% or less,
acid-soluble Al: 0% or more and 0.01% or less,
N: 0% or more and 0.005% or less,
Cu: 0% or more and 0.30% or less,
Sn: 0% or more and 0.30% or less,
Ni: 0% or more than
0.30%, Cr: 0% 0.30% or less, and
Sb: 0% or more than 0.30%
and containing the balance being Fe and impurities,
　the silicon steel sheet two The average grain size of the next recrystallized grain is 10 mm or more and 50 mm or less, the grain 　　thickness of the grain-
　oriented electrical steel sheet is
0.15 mm or more and 0.23 mm or less, and the
　　iron loss Wp is 0.800 W / at W 17/50. It is less than kg and
　　Wp / Wd, which is the ratio of the iron loss Wp to the iron loss Wd when the magnetic domain is controlled, is 1.03 or more and 1.15 or less at W 17/50 , and the
　　magnetic flux density B8 value is 1.930 T or more. A grain-oriented electrical steel sheet characterized by being present.　
[Claim 4]
　The component composition of the silicon steel sheet is, in mass%,
Cu: 0.01% or more and 0.30% or less,
Sn: 0.01% or more and 0.30% or less,
Ni: 0.01% or more and 0.30%. Hereinafter, the direction according to claim 3 , wherein
Cr: 0.01% or more and 0.30% or less, and
Sb: 0.01% or more and 0.30% or less
of one type or two or more types are contained. Electrical steel sheet.