Abstract: This grain-oriented electrical steel sheet comprises: a base material steel sheet having a chemical composition containing, in mass%, 0.010% or less of C, 2.50-4.00% of Si, 0.050-1.000% of Mn, a total of 0.005% or less of S and Se, 0.005% or less of soluble Al, 0.005% or less of N, a total of 0-0.0300% of Bi, Te, and Pb, 0-0.50% of Sb, 0-0.50% of Sn, 0-0.50% of Cr, and 0-1.0% of Cu, the balance being Fe and impurities; and a tension-imparting insulating coating film provided on the surface of the base material steel sheet, wherein the surface of the base material steel sheet has an arithmetic mean roughness Ra of 0.60 µm or less in a rolling-90° direction perpendicular to the rolling direction, and when a cross-section along the rolling-90° direction of the base material steel sheet is observed, there are recessed portions having a depth of 0.1-2.0 µm in the surface of the base material steel sheet at a density of 1.0 to 6.0/100 µm.
Title of invention: Method for manufacturing grain-oriented electrical steel sheet and grain-oriented electrical steel sheet
Technical field
[0001]
The present invention relates to a grain-oriented electrical steel sheet and a method for manufacturing a grain-oriented electrical steel sheet.
The present application claims priority based on Japanese Patent Application No. 2018-054675 filed in Japan on March 22, 2018, the contents of which are incorporated herein by reference.
Background technology
[0002]
The grain-oriented electrical steel sheet contains about 0.5 to 7% by mass of silicon (Si), and the crystal orientation is integrated in the {110} <001> orientation (Goss orientation) by utilizing a phenomenon called secondary recrystallization. It is a steel sheet and is mainly used as a soft magnetic material for iron cores such as transformers. Since the characteristics of grain-oriented electrical steel sheets have a great influence on the performance of transformers, diligent studies have been carried out on grain-oriented electrical steel sheets in order to achieve good excitation characteristics and low iron loss characteristics.
[0003]
The general manufacturing method of grain-oriented electrical steel sheets is as follows.
First, a steel piece having a predetermined chemical composition is heated and hot-rolled to produce a hot-rolled steel sheet. If necessary, the obtained hot-rolled steel sheet is annealed, and then the hot-rolled steel sheet is pickled. The hot-rolled steel sheet after pickling is cold-rolled to produce a cold-rolled steel sheet. The obtained cold-rolled steel sheet is decarburized and annealed to develop primary recrystallization.
Then, an aqueous slurry containing an annealing separator containing MgO as a main component is applied to the surface of the cold-rolled steel sheet after decarburization and annealing, and dried. Then, the steel sheet is wound around a coil and finish-annealed to develop secondary recrystallization. At the time of finish annealing, MgO in the annealing separator reacts with SiO 2 in the internal oxide layer formed on the surface of the cold-rolled steel sheet at the same time as the secondary recrystallization appears in the steel sheet. Then, a primary coating (also referred to as "glass coating") containing forsterite (Mg 2 SiO 4 ) as a main component is formed on the surface of the steel sheet.
After finish annealing (after forming a glass film), a solution containing colloidal silica and phosphate as main components is applied to the upper layer and baked to obtain a tension-imparting insulating film (also referred to as "secondary film"). ) Is formed.
[0004]
In addition to functioning as an insulating film, such a glass film has a function of improving the adhesion of the tension-applying insulating film formed on the upper layer of the glass film, and both the glass film and the tension-applying insulating film are provided. Iron loss is reduced by the tension caused by. However, the glass coating has a non-magnetic phase, which is not preferable from the viewpoint of magnetic properties. Further, the interface between the steel plate and the glass coating has an intricately fitted structure in which the roots of the glass coating are intricate, and may cause an increase in iron loss through inhibition of domain wall movement. When such a fitting structure is reduced, the adhesion between the glass coating and the steel plate deteriorates, and as a result, the adhesion of the tension-applying insulating coating also deteriorates. Therefore, when the surface of the steel sheet is smoothed by removing the glass film or suppressing the formation of the glass film, excellent magnetic properties can be obtained, but the adhesion of the tension-applying insulating film is further inferior. Become.
[0005]
In a directional electromagnetic steel sheet that does not have such a glass film, as a means for improving the adhesion of the tension-applying insulating film, for example, Patent Document 1 describes a steel sheet before applying the tension-applying insulating film. A technique for washing by immersing in an aqueous solution containing sulfuric acid or sulfate as a sulfuric acid concentration of 2 to 30% is disclosed. Further, Patent Document 2 discloses a technique for forming a tension-applying insulating film after pretreating the surface of a steel sheet with an oxidizing acid when applying a tension-applying insulating film. Further, Patent Document 3 discloses a directional silicon steel plate having an external oxide-type oxide film mainly composed of silica and containing metallic iron having a cross-sectional area ratio of 30% or less in the external oxide-type oxide film. Has been done. Further, Patent Document 4 describes a grain-oriented electrical steel sheet having fine streaky grooves having a depth of 0.05 μm or more and 2 μm or less directly applied to the surface of the grain steel of the grain-oriented electrical steel sheet at intervals of 0.05 μm or more and 2 μm or less. Is disclosed.
[0006]
The tension-applying insulating film formed on the surface of the grain-oriented electrical steel sheet having no glass film may be peeled off while being left to stand if the adhesiveness is poor. From the viewpoint of industrially stable production of grain-oriented electrical steel sheets, it is extremely important to improve the adhesion of the tension-applying insulating coating. In this regard, the techniques disclosed in Patent Documents 1 to 4 are all disclosed in Patent Documents 1 to 4 although they are intended to improve the adhesion of the tension-imparting insulating coating. It is not always clear whether the technology can obtain a stable iron loss reduction effect, and there is still room for consideration.
Prior art literature
Patent documents
[0007]
Patent Document 1: Japanese Patent Application Laid-Open No. 5-311453
Patent Document 2: Japanese Patent Application Laid-Open No. 2002-249880
Patent Document 3: Japanese Patent Application Laid-Open No. 2003-313644
Patent Document 4: Japanese Patent Application Laid-Open No. 2001-303215 Publication No.
Outline of the invention
Problems to be solved by the invention
[0008]
The present invention has been made in view of the above problems. An object of the present invention is to industrialize a grain-oriented electrical steel sheet having no glass coating, a grain-oriented electrical steel sheet having excellent adhesion of a tension-applying insulating film and excellent magnetic properties, and such grain-oriented electrical steel sheet. It is an object of the present invention to provide a method for producing a grain-oriented electrical steel sheet capable of stable production.
Means to solve problems
[0009]
As a method for obtaining a grain-oriented electrical steel sheet having no glass film, a method of removing the generated glass film by chemical polishing or electrolytic polishing is known. However, from the viewpoint of productivity, it is preferable to obtain a grain-oriented electrical steel sheet having no glass film by suppressing the formation of the glass film at the time of finish annealing, rather than removing the formed glass film.
Conventionally, it has been considered that the magnetic properties of grain-oriented electrical steel sheets are greatly affected by strain, and the formation of mechanical irregularities causes deterioration of magnetic properties due to strain. Therefore, in the case of suppressing the formation of the glass film, the surface state of the steel sheet is a smooth surface. However, the present inventors have conceived to intentionally impart appropriate mechanical unevenness to the surface of the grained steel sheet, rather than maintaining the surface state as a smooth surface in the grain-oriented electrical steel sheet having no glass coating as in the past. .. Further, it is presumed that the magnetic characteristics are improved by improving the adhesion of the tension-applying coating due to the mechanical unevenness and increasing the tension applied by the tension-applying insulating coating. It was investigated.
[0010]
In recent years, a wet blast method in which a slurry in which particles and a liquid are mixed is injected using compressed air to process the surface has attracted attention. Such a technique can use a finer abrasive as compared with the dry shot blasting method, and is being applied to control the surface texture of glass and lenses, for example.
The present inventors have focused on the wet blast method as a method for imparting mechanical unevenness to a smooth surface, and have diligently studied its application to grain-oriented electrical steel sheets having no glass coating.
[0011]
As described above, conventionally, it has been considered that the magnetic properties of grain-oriented electrical steel sheets are greatly affected by strain, and the formation of mechanical irregularities causes deterioration of magnetic properties due to strain. However, as a result of the studies by the present inventors, it has been found that not only the adhesion of the tension-applying insulating film is remarkably improved by wet blasting, but also the magnetic properties of the grain-oriented electrical steel sheet are further improved. The reason for this is not clear, but if the mechanical unevenness is uniformly formed in the plane with an appropriate size and number density by the wet blast method, the deterioration of the magnetic properties due to distortion is small even if it is formed, but rather the anchor effect. It is presumed that this occurred, and as a result of improving not only the adhesion but also the film tension, the magnetic characteristics were improved.
In grain-oriented electrical steel sheets that do not have a glass coating on the premise that they have such mechanical irregularities, the base metal has an effect on the magnetic properties after the formation of the tension-applying insulating coating and after the magnetic domain subdivision treatment. It was also clarified that the influence of the degree of azimuth integration was larger than expected. Therefore, the present invention has been completed with the finding that the control of the temperature rising rate at the time of decarburization annealing and the inclusion of the inhibitor strengthening element in the steel piece are effective for further improving the magnetic properties.
The gist of the present invention completed based on the above findings is as follows.
[0012]
[1] The grain-oriented electrical steel sheet according to one aspect of the present invention has a mass% of C: 0.010% or less, Si: 2.50 to 4.00%, Mn: 0.050 to 1.000%, and so on. S + Se: 0.005% or less in total, Sol. Al: 0.005% or less, N: 0.005% or less, Bi + Te + Pb: 0 to 0.0300% in total, Sb: 0 to 0.50%, Sn: 0 to 0.50%, Cr: 0 to 0 A base steel sheet containing .50% and Cu: 0 to 1.0% and having a chemical composition in which the balance is Fe and impurities, and a tension-imparting insulating coating provided on the surface of the base steel sheet. The arithmetic average roughness Ra along the rolling 90 ° direction, which is a direction perpendicular to the rolling direction, is 0.60 μm or less on the surface of the base steel sheet, and is along the rolling 90 ° direction. When observing the cross section of the base steel sheet, there are 1.0 / 100 μm or more and 6.0 / 100 μm or less recesses on the surface of the base steel sheet having a depth of 0.1 μm or more and 2.0 μm or less. Exists.
[0013]
[2] In the grain-oriented electrical steel sheet according to the above [1], the base steel sheet may contain Bi + Te + Pb: 0.0005 to 0.0300% in total as the chemical composition.
[0014]
[3] The method for producing a grain-oriented electrical steel sheet according to another aspect of the present invention is, in terms of mass%, C: 0.020 to 0.100%, Si: 2.50 to 4.00%, Mn: 0. 050 to 1.000%, S + Se: 0.005 to 0.080% in total, Sol. Al: 0.010 to 0.070%, N: 0.005 to 0.020%, Bi + Te + Pb: 0 to 0.0300% in total, Sb: 0 to 0.50%, Sn: 0 to 0.50% , Cr: 0 to 0.50%, Cu: 0 to 1.0%, and the hot rolling step of heating a steel piece whose balance is Fe and impurities and then hot rolling to obtain a hot-rolled steel sheet. , Arbitrarily, a hot-rolled plate annealing step of quenching the hot-rolled steel sheet to obtain a hot-rolled hardened steel sheet, and one cold rolling or intermediate annealing of the hot-rolled steel sheet or the hot-rolled hardened steel sheet. A cold rolling step of obtaining a cold-rolled steel sheet by performing a plurality of cold-rolling sandwiching the steel sheet, a decarburization annealing step of decarburizing the cold-rolled steel sheet to obtain a decarburized and annealed steel sheet, and the decarburization. Wet under the condition that the following formula (i) is satisfied with respect to the finish annealing step of applying the ablation separating agent to the charcoal annealed steel sheet and then the finish ablation, and the entire sheet width direction of the steel sheet surface after the finish ablation step. The annealing separating agent includes MgO and Al 2 O 3 and includes a surface processing step of performing surface processing by blasting and an insulating film forming step of forming a tension-imparting insulating film on the surface of the steel sheet after the surface processing step. preparative as a main component, the Al and the MgO 2 O 3 MgO is a mass ratio of: Al 2 O 3 is 3: 7 to 7: in the range of 3, and a bismuth chloride 0.5 Contains 15% by mass.
0.15 ≤ (S × c × ρ) / (6 × v × W) ≤ 3.00 ・ ・ ・ Formula (i)
Here, in the above formula (i),
S: Flow rate of the slurry used for the wet blasting. (L / min)
c: Concentration of the polishing agent used for the wet blast (% by volume)
ρ: Density of the polishing agent used for the wet blast (kg / m 3 )
v: Nozzle and steel plate to which the slurry is discharged Relative velocity (mm / sec)
W: The width (mm)
of the nozzle from which the slurry is discharged .
[0015]
[4] In the method for manufacturing grain-oriented electrical steel sheets according to the above [3], in the decarburization annealing step, the temperature rise rate S1 in the temperature range of 500 ° C. or higher and lower than 600 ° C. and the temperature rise rate S1 in the temperature range of 600 ° C. or higher and lower than 700 ° C. The heating rate S2 may satisfy the following equations (ii) to (iv), respectively.
300 ≤ S1 ≤ 1000 ... Equation (ii)
1000 ≤ S2 ≤ 3000 ... Equation (iii)
1.0
First, the main configuration of grain-oriented electrical steel sheet according to the present embodiment will be described with reference to FIGS. 1A and 1B. 1A and 1B are diagrams schematically showing the structure of the grain-oriented electrical steel sheet according to the present embodiment.
[0022]
As shown schematically in FIG. 1A, the directional electromagnetic steel sheet 10 according to the present embodiment is a tension-applying insulating film which is an example of the base steel sheet 11 and the insulating film formed on the surface of the base steel sheet 11. There is no glass coating between the base steel plate 11 and the tension-applying insulating coating 13. In the grain-oriented electrical steel sheet 10 according to the present embodiment, the tension-applying insulating coating 13 may be formed on at least one surface of the base steel sheet 11, but is usually as schematically shown in FIG. 1B. , It is formed on both sides of the base steel plate 11.
[0023]
Hereinafter, the grain-oriented electrical steel sheet 10 according to the present embodiment will be described focusing on its characteristic configuration. In the following description, detailed description of known configurations and some configurations that can be implemented by those skilled in the art may be omitted.
[0024]
[About the base steel sheet 11] The
base steel sheet 11 has a predetermined chemical composition by being produced from a steel piece containing a chemical composition as described in detail below. Further, the surface of the base steel plate 11 according to the present embodiment is provided with fine recesses as described in detail below. Due to the presence of such recesses, the grain-oriented electrical steel sheet 10 according to the present embodiment has excellent adhesion of the tension-applying insulating coating 13 and exhibits excellent magnetic characteristics. The chemical composition of the base steel sheet 11 will be described in detail below.
[0025]
[About the tension-applying insulating film 13] The
tension-applying insulating film 13 is located on the surface of the base steel sheet 11, and the eddy current loss is reduced by imparting electrical insulation to the grain-oriented electrical steel sheet 10. , The iron loss of the grain-oriented electrical steel sheet 10 is improved. Further, the tension-imparting insulating coating 13 realizes various properties such as corrosion resistance, heat resistance, and slipperiness in addition to the above-mentioned electrical insulating properties.
[0026]
Further, the tension-applying insulating coating 13 has a function of applying tension to the grain-oriented electrical steel sheet 10. By applying tension to the grain-oriented electrical steel sheet 10 to facilitate the movement of the domain wall in the grain-oriented electrical steel sheet 10, the iron loss of the grain-oriented electrical steel sheet 10 can be improved.
[0027]
The surface of the tension-imparting insulating coating 13 may be subjected to a known magnetic domain subdivision treatment by using a continuous wave laser beam or an electron beam.
[0028]
The tension-imparting insulating coating 13 is formed, for example, by applying a coating liquid containing metal phosphate and silica as main components to the surface of the base steel sheet 11 and baking the coating liquid.
[0029]
The product plate thickness (thickness t in FIGS. 1A and 1B) of the grain- oriented electrical steel sheet 10 according to the present embodiment is not particularly limited, and is, for example, 0.17 mm or more. It can be 0.35 mm or less. Further, in the present embodiment, the effect becomes remarkable when the plate thickness after cold spreading is as thin as less than 0.22 mm (that is, a thin material), and the adhesion of the tension-applying insulating film 13 is further excellent. It will be. The plate thickness after cold spreading is, for example, preferably 0.17 mm or more and 0.22 mm or less, and more preferably 0.17 mm or more and 0.20 mm or less.
[0030]
Next , the chemical composition of the base steel sheet 11 of the grain-oriented electrical steel sheet 10 according to the present embodiment will be described in detail. In the following, unless otherwise specified, the notation "%" means "mass%".
[0031]
The base steel sheet 11 according to the present embodiment has a mass% of C: 0.010% or less, Si: 2.50 to 4.00%, Mn: 0.050 to 1.000%, S + Se: 0.005. % Or less, Sol. Al: 0.005% or less, N: 0.005% or less, optionally Bi + Te + Pb: 0.03% or less, Sb: 0.50% or less, Sn: 0.50% or less, Cr: 0. It contains 50% or less, Cu: 1.0% or less, and has a chemical composition in which the balance is composed of Fe and impurities.
[0032]
[C: 0.010% or less]
C (carbon) is an element effective for structure control until the completion of the decarburization annealing step in the manufacturing process. However, if the C content exceeds 0.010%, the magnetic properties of the grain-oriented electrical steel sheet, which is the product plate, deteriorate. Therefore, in the base steel sheet 11 of the grain-oriented electrical steel sheet 10 according to the present embodiment, the C content is 0.010% or less. The C content is preferably 0.005% or less. The lower the C content, the better, but even if the C content is reduced to less than 0.0001%, the effect of tissue control is saturated and the production cost is increased. Therefore, the C content is preferably 0.0001% or more.
[0033]
[Si: 2.50 to 4.00%]
Si (silicon) is an element that increases the electrical resistance of steel and reduces eddy current loss. When the Si content is less than 2.50%, the above-mentioned eddy current loss reduction effect cannot be sufficiently obtained. Therefore, the Si content is set to 2.50% or more. The Si content is preferably 2.70% or more, more preferably 2.80% or more.
On the other hand, when the Si content exceeds 4.00%, the cold workability of the steel deteriorates. Therefore, in the base steel sheet 11 of the grain-oriented electrical steel sheet 10 according to the present embodiment, the Si content is set to 4.00% or less. The Si content is preferably 3.90% or less, more preferably 3.80% or less.
[0034]
[Mn: 0.050 to 1.000%]
Mn (manganese) combines with S and Se described later to form MnS and MnSe during the manufacturing process. These precipitates function as inhibitors (inhibitors of normal grain growth) and cause secondary recrystallization in steel. Mn is an element that further enhances the hot workability of steel. When the Mn content is less than 0.050%, the above effects cannot be sufficiently obtained. Therefore, the Mn content is set to 0.050% or more. The Mn content is preferably 0.060% or more.
On the other hand, when the Mn content exceeds 1.000%, secondary recrystallization does not occur and the magnetic properties of the steel deteriorate. Therefore, the Mn content of the base steel sheet 11 of the grain-oriented electrical steel sheet 10 according to the present embodiment is 1.000% or less. The Mn content is preferably 0.500% or less.
[0035]
[One or more of S and Se (S + Se): 0.005% or less in total]
S (sulfur) and Se (selenium) combine with Mn in the manufacturing process to form MnS and MnSe that function as inhibitors. .. However, when the total of the S content and the Se content exceeds 0.005%, the magnetic properties are deteriorated due to the remaining inhibitors. Therefore, in the base steel sheet 11 according to the present embodiment, the total content of S and Se is 0.005% or less. The total content of S and Se in the grain-oriented electrical steel sheet is preferably as low as possible. However, even if the total content of S and Se in the grain-oriented electrical steel sheet is reduced to less than 0.0001%, the manufacturing cost is only increased. Therefore, the total content of S and Se in the grain-oriented electrical steel sheet is preferably 0.0001% or more.
[0036]
[Acid-soluble Al: 0.005% or less]
Acid-soluble aluminum (sol.Al) combines with N during the manufacturing process of grain-oriented electrical steel sheets to form AlN that functions as an inhibitor. However, when the acid-soluble Al content of the base steel sheet 11 exceeds 0.005%, the inhibitor remains excessively in the base steel sheet 11, so that the magnetic properties deteriorate. Therefore, in the base steel sheet 11 according to the present embodiment, the acid-soluble Al content is set to 0.005% or less. The acid-soluble Al content is preferably 0.004% or less. The lower limit of the acid-soluble Al content is not particularly specified, but even if it is reduced to less than 0.0001%, the production cost will only increase. Therefore, the acid-soluble Al content is preferably 0.0001% or more.
[0037]
[N: 0.005% or less]
N (nitrogen) binds to Al in the manufacturing process to form AlN that functions as an inhibitor. However, when the N content exceeds 0.005%, the inhibitor remains excessively in the grain-oriented electrical steel sheet, and the magnetic characteristics deteriorate. Therefore, in the base steel sheet 11 according to the present embodiment, the N content is set to 0.005% or less. The N content is preferably 0.004% or less.
On the other hand, the lower limit of the N content is not particularly specified, but even if it is reduced to less than 0.0001%, the manufacturing cost will only increase. Therefore, the N content is preferably 0.0001% or more.
[0038]
[Remaining part: Fe and impurities]
The chemical composition of the base steel sheet 11 according to the present embodiment is basically containing the above-mentioned elements, and the remaining part is iron (Fe) and impurities. However, for the purpose of enhancing the magnetic properties, Bi, Te, Pb, Sb, Sn, Cr, and Cu may be further contained in the range shown below.
Here, the impurities are those mixed from ore, scrap, or the manufacturing environment as a raw material when the base steel sheet 11 is industrially manufactured, and the action of the directional electromagnetic steel sheet according to the present embodiment. It means an element that is allowed to be contained in a content that does not adversely affect.
[0039]
[At least one type of Bi, Te or Pb (Bi + Te + Pb): 0 to 0.0300% in total]
The base steel sheet 11 according to the present embodiment has Bi as the above optional element instead of a part of the remaining Fe. It may contain at least one of (bismuth), Te (tellurium) or Pb (lead). By containing one or more of these elements, the magnetic properties of the grain-oriented electrical steel sheet can be further enhanced. When this effect is obtained, the total content of at least one of Bi, Te or Pb (one or more selected from Bi, Te and Pb) is preferably 0.0005% or more, more preferably 0. It is 0010% or more.
On the other hand, if the total content of these elements exceeds 0.0300%, hot embrittlement is caused. Therefore, the total content of at least one of Bi, Te or Pb is preferably 0.0300% or less. Since Bi, Te and Pb do not necessarily have to be contained, the lower limit of the total content is 0%.
[0040]
In addition to the above-mentioned optional elements, the base steel sheet 11 according to the present embodiment has Sb (antimony), Sn (tin), Cr (chromium), or Cu (), which is effective for improving the magnetic properties of the grain-oriented electrical steel sheet. Copper) may be contained as an arbitrary element. When these elements are contained, the content of each element is Sb: 0% or more and 0.50% or less, Sn: 0% or more and 0.50% or less, Cr: 0% or more and 0.50% or less, Cu: It is preferably 0% or more and 1.0% or less. The content of each is more preferably 0.005% or more, still more preferably 0.010% or more.
[0041]
In the base steel sheet 11 according to the
present embodiment, the surface serving as the interface with the tension-applying insulating coating 13 has a predetermined arithmetic mean roughness Ra, as briefly mentioned earlier. There are recesses having a predetermined depth and having a predetermined ratio.
[0042]
Hereinafter, the characteristic surface shape of the base steel sheet 11 according to the present embodiment will be described in detail with reference to FIGS. 2 to 4. FIG. 2 is a diagram schematically showing a grain-oriented electrical steel sheet according to the present embodiment. FIG. 3 is a diagram schematically showing the surface of the base steel sheet of the grain-oriented electrical steel sheet according to the present embodiment. FIG. 4 is a diagram for explaining the depth of the recesses on the surface of the base steel plate according to the present embodiment.
[0043]
In the magnetization process of the grain-oriented electrical steel sheet, the domain wall of the magnetic section whose magnetization is oriented in the rolling direction as schematically shown in FIG. 2 moves. The moving direction of the domain wall in such a case is a direction perpendicular to the rolling direction (corresponding to the plate width direction in FIG. 2). Hereinafter, the direction perpendicular to the rolling direction is referred to as a "rolling 90 ° direction". Since the moving direction of the domain wall is the rolling 90 ° direction, the influence of the surface shape on the magnetic characteristics is indexed by the rolling 90 ° direction.
[0044]
The grain-oriented electrical steel sheet 10 which shows excellent adhesion of the tension-imparting insulating film and exhibits excellent magnetic properties even though it does not have a glass film is the surface of the base steel sheet 11 along the rolling 90 ° direction. However, it has a characteristic surface shape.
[0045]
The surface of the base steel plate 11 according to the present embodiment is a case where the directional electromagnetic steel plate 10 (base steel plate 11) is cut along the AA cutting line shown in FIG. The surface of the base steel sheet 11 has an arithmetic mean roughness Ra defined by JIS B0601 (2013) of 0.60 μm or less. When the arithmetic mean roughness Ra of the surface of the base steel sheet 11 along the rolling 90 ° direction exceeds 0.60 μm, the movement of the domain wall as described above is affected, and excellent magnetic characteristics are realized. Can't. The arithmetic mean roughness Ra of the surface of the base steel sheet 11 along the rolling 90 ° direction is preferably 0.30 μm or more and 0.50 μm or less. Such arithmetic mean roughness Ra can be measured using a known surface roughness meter conforming to JIS B0601 (2013). The directional electromagnetic steel plate after forming the tension-applying insulating film is immersed in an aqueous solution having a liquid temperature of 60 to 80 ° C. and a NaOH concentration of 30 to 40%, and the surface after removing the tension-applying insulating film is JIS B. It is possible to measure the arithmetic mean roughness Ra of the surface of the base metal steel plate by measuring using a known surface roughness meter based on 0601 (2013).
[0046]
Further, the surface of the base steel plate 11 according to the present embodiment is schematically shown in FIG. 3 when the directional electromagnetic steel plate 10 (base steel plate 11) is cut along the AA cutting line shown in FIG. As described above, recesses 101 having a predetermined depth are present on the surface of the base steel plate 11 at a predetermined ratio. More specifically, on the surface of the base steel sheet 11 when cut in the rolling 90 ° direction, 1.0 recesses 101 having a depth of 0.1 μm or more and 2.0 μm or less are 1.0 pieces / 100 μm or more. There are 0 pieces / 100 μm or less.
[0047]
That is, on the surface of the base steel plate 11 according to the present embodiment, the number of recesses 101 having a depth of 0.1 μm or more and 2.0 μm or less is 1.0 or more within a range of 100 μm in cross-sectional length. It is 6.0 or less. When the number of the recesses 101 is less than 1.0 / 100 μm, the number of the recesses 101 formed is too small, and the tension-applying insulating coating 13 has excellent adhesion and excellent magnetic properties. It cannot be realized. On the other hand, when the number of the recesses 101 is more than 6.0 / 100 μm, the adhesiveness of the tension-applying insulating film 13 is improved, but excellent magnetic characteristics cannot be realized. By setting the number of the recesses 101 to be 1.0 / 100 μm or more and 6.0 / 100 μm or less, the excellent adhesion of the tension-applying insulating coating 13 is exhibited and the recesses 101 are imparted to the base steel plate 11. By increasing the tension, excellent magnetic properties are exhibited. The number of recesses 101 is preferably 1.0 / 100 μm or more and 5.0 / 100 μm or less.
[0048]
The recess 101 as described above can be observed by using a general scanning electron microscope (SEM) for a cross section in the 90 ° rolling direction. More specifically, the cross section of the base steel plate 11 at an arbitrary position in the rolling 90 ° direction is observed at a magnification of 1000 times, and first, a portion where the surface of the base steel plate 11 is flat is specified. Such a flat portion is used as a "depth reference point" when measuring the depth as shown in FIG.
[0049]
After selecting two or more such depth reference points in the field of view of interest, consider a line segment connecting the selected depth reference lines, and use such a line segment as the "depth reference line". .. As schematically shown in FIG. 4, the depth of the recess 101 according to the present embodiment is defined as the separation distance between the "depth reference line" specified as described above and the deepest position of the recess. Will be done. Such observation may be performed at the same magnification (1000 times) in any three visual fields, and evaluation may be performed using the average value of the obtained numbers.
The surface shape characteristic of the base steel sheet 11 according to the present embodiment as shown in FIGS. 3 and 4 can be formed by using the wet blast method described later. The wet blast method is realized by projecting the slurry mixed with the abrasive onto the surface of the base steel plate 11, and the mechanical unevenness formed on the surface of the base steel plate 11 on which the slurry is projected is uniform. Therefore, it is a characteristic flat surface in which the above-mentioned flat portion exists.
[0050]
In the base steel sheet 11 according to the present embodiment, in order to realize the recess 101 having a depth of 2.0 μm or less, a surface processing treatment by wet blasting is performed under specific conditions as described in detail below. Therefore, there is no recess 101 having a depth of more than 2.0 μm on the surface of the base steel sheet 11 according to the present embodiment. Further, when the recess having a depth of more than 2.0 μm is present, the grain-oriented electrical steel sheet does not exhibit excellent magnetic properties, so that the existence of the recess having a depth of more than 2.0 μm need not be considered.
Further, the concave portion 101 having a depth of less than 0.1 μm and the convex portion having a height of less than 0.1 μm do not affect the adhesion and magnetic properties of the tension-applying insulating coating 13. .. Therefore, it is not necessary to consider it in the above observation, and the depth of the recess 101 of interest is 0.1 μm or more.
[0051]
The number of recesses having a depth of 0.1 μm or more and 2.0 μm or less and the arithmetic mean roughness Ra have different technical meanings. That is, the number of recesses having a depth of 0.1 μm or more and 2.0 μm or less is mechanical unevenness that contributes to the improvement of the adhesion of the tension-imparting insulating coating, and contributes to the improvement of the magnetic characteristics through the improvement of the coating tension. On the other hand, the arithmetic mean roughness Ra represents the average value of the uneven state at the reference length, and does not necessarily match the form of the mechanical unevenness that contributes to the improvement of adhesion. Further, even if Ra is high, the number of recesses having a depth of 0.1 μm or more and 2.0 μm or less is not necessarily large.
[0052]
In addition, as described in detail below, the specific surface shape as described above is subjected to finish annealing using an annealing separator that does not form a glass film, and then subjected to a wet blast method under appropriate conditions. This is achieved only when surface processing is performed. When finish annealing is performed using a general annealing separator that produces a glass film and the formed glass film is removed by chemical polishing or electrolytic polishing, the surface roughness of the base steel sheet 11 is appropriate. The surface becomes too rough without being able to be controlled, and the recess 101 having the above-mentioned depth cannot be realized.
[0053]
The grain-oriented electrical steel sheet 10 according to the present embodiment has been described in detail above.
Various magnetic properties exhibited by grain-oriented electrical steel sheets according to this embodiment include the Epstein method specified in JIS C2550-1 (2011) and the single-plate magnetic property measurement method (Single Sheet) specified in JIS C2556 (2015). It is possible to measure according to Tester: SST).
[0054]
(About the Manufacturing Method of Electrical Steel Sheet)
Next, the manufacturing method of the grain-oriented electrical steel sheet according to the present embodiment will be described in detail with reference to FIG. FIG. 5 is a flow chart showing an example of the flow of the manufacturing method of the grain-oriented electrical steel sheet according to the present embodiment.
[0055]
The overall flow of the manufacturing method of grain-oriented electrical steel sheet according to the
present embodiment will be described below.
[0056]
The overall flow of the method for manufacturing grain-oriented electrical steel sheets according to this embodiment is as follows.
First, a steel piece (slab) having a chemical composition described later is hot-rolled to obtain a hot-rolled steel sheet. Then, the hot-rolled steel sheet is annealed to obtain a hot-rolled annealed steel sheet. Next, the obtained hot-rolled annealed steel sheet is pickled and then cold-rolled once or twice with intermediate annealing in between to be cold-rolled to a predetermined thickness after cold-rolling. Obtain an annealed steel sheet. Then, the obtained cold-rolled steel sheet is decarburized and primary recrystallized by annealing (decarburization annealing) in a wet hydrogen atmosphere to obtain a decarburized annealed steel sheet. In such decarburization annealing, a predetermined oxide film is formed on the surface of the steel sheet. Subsequently, an annealing separator mainly composed of MgO and Al 2 O 3 is applied to the surface of the decarburized annealed steel sheet and then dried to perform finish annealing. By such finish annealing, secondary recrystallization occurs, and the grain structure of the steel sheet is accumulated in the {110} <001> orientation. Further, in the method for manufacturing grain-oriented electrical steel sheet according to the present embodiment, since a specific annealing separator that does not form a glass film is used, no glass film is formed on the surface of the steel sheet after finish annealing, and the surface is flat. become. After that, the surface of the steel sheet after finish annealing is subjected to surface processing using wet blasting. By this surface processing, recesses as described above are formed on the surface of the steel sheet. A tension-imparting insulating film is formed by demineralizing the surface-treated finish annealed plate by washing with water or pickling, and then applying and baking a coating liquid mainly composed of phosphate.
[0057]
That is, in the method for producing a directional electromagnetic steel sheet according to the present embodiment, as shown in FIG. 5, a steel piece having the above chemical components is hot-rolled at a predetermined temperature to obtain a hot-rolled steel sheet. A hot rolling step (step S101), a hot-rolled sheet annealing step (step S103) in which the obtained hot-rolled steel sheet is arbitrarily annealed to obtain a hot-rolled fired steel sheet, and the obtained hot-rolled steel sheet or hot-rolled fired steel sheet. On the other hand, a cold rolling step (step S105) of obtaining a cold-rolled steel sheet by performing one cold-rolling or a plurality of cold-rolling sandwiching intermediate annealing, and removing the obtained cold-rolled steel sheet. A decarburization anneal step (step S107) of performing charcoal annealing to obtain a decarburized annealed steel sheet, and a finish anethaning step (step S109) of applying a quenching separator to the obtained decarburized annealed steel sheet and then performing finish annealing. ), A surface processing step (step S111) in which the surface of the steel sheet surface after finish annealing is subjected to surface processing by wet blasting under predetermined conditions, and an insulating coating on the surface of the steel sheet after surface processing (more details). Includes an insulating coating forming step (step S113) for forming a tension-applying insulating coating).
[0058]
Hereinafter, these steps will be described in detail. In the following description, when some conditions in each step are not described, it is possible to carry out each step by appropriately applying known conditions.
[0059]
The
hot rolling step (step S101) is a step of hot rolling a steel piece having a predetermined chemical component (for example, a steel ingot such as a slab) into a hot-rolled steel sheet. In such a hot rolling step, a piece of silicon steel having a chemical composition as described briefly below is first heat-treated. Here, the heating temperature is preferably in the range of 1200 to 1400 ° C. The heating temperature is more preferably 1250 ° C. or higher and 1380 ° C. or lower. Next, the steel pieces heated to the above temperature are processed into hot-rolled steel sheets by subsequent hot rolling. The thickness of the processed hot-rolled steel sheet is preferably in the range of 2.0 mm or more and 3.0 mm or less, for example.
[0060]
The chemical composition of steel pieces used in the
hot rolling process will be briefly described below. In the following description, unless otherwise specified, the notation "%" shall represent "mass%".
[0061]
[C: 0.020 to 0.100%]
C is an element effective for improving magnetic properties through microstructure control until the completion of the decarburization annealing step in the manufacturing process. When the C content in the steel piece is less than 0.020%, or when the C content in the steel piece exceeds 0.100%, the above-mentioned magnetic property improving effect cannot be obtained. Therefore, the C content in the steel piece is 0.020 to 0.100%. The C content in the steel piece is preferably 0.030 to 0.090%.
[0062]
[Si: 2.50 to 4.00%]
Si is an element that increases the electrical resistance of steel and reduces eddy current loss. When the Si content in the steel piece is less than 2.50%, the effect of reducing the eddy current loss cannot be sufficiently obtained. Therefore, the Si content is set to 2.50% or more. The Si content in the steel piece is preferably 2.70% or more, more preferably 2.80% or more.
On the other hand, when the Si content in the steel piece exceeds 4.00%, the cold workability of the steel is lowered. Therefore, the Si content of the steel piece is set to 4.00% or less. The Si content in the steel piece is preferably 3.90% or less, more preferably 3.80% or less.
[0063]
[Mn: 0.050 to 1.000%]
Mn combines with S and Se during the manufacturing process to form MnS and MnSe. These precipitates act as inhibitors and cause secondary recrystallization in steel. Mn is also an element that enhances the hot workability of steel. When the Mn content in the steel piece is less than 0.050%, these effects cannot be sufficiently obtained. Therefore, the Mn content of the steel piece is set to 0.050% or more. The Mn content is preferably 0.060% or more.
On the other hand, when the Mn content in the steel piece exceeds 1.000%, secondary recrystallization does not occur and the magnetic properties of the steel deteriorate. Therefore, in the steel piece, the Mn content is set to 0.050 to 1.000%. The Mn content is preferably 0.500% or less.
[0064]
[One or more of S and Se (S + Se): 0.005 to 0.080% in total]
S and Se combine with Mn in the manufacturing process to form MnS and MnSe that function as inhibitors. When the total content of S and Se is less than 0.005%, it becomes difficult to exhibit the effect of forming MnS and MnSe. Therefore, the total content of S and Se in the steel piece is 0.005% or more. The total content of S and Se in the steel piece is preferably 0.006% or more.
On the other hand, when the total content of S and Se exceeds 0.080%, not only the magnetic properties are deteriorated but also embrittlement due to heat is caused. Therefore, the total content of S and Se in the steel piece is 0.080% or less. It is preferably 0.070% or less.
[0065]
[Acid-soluble Al: 0.010 to 0.070%]
Acid-soluble Al (sol.Al) combines with N during the manufacturing process of grain-oriented electrical steel sheets to form AlN that functions as an inhibitor. When the acid-soluble Al content is less than 0.010%, AlN is not sufficiently generated and the magnetic properties deteriorate. If the acid-soluble Al content exceeds 0.070%, not only the magnetic properties deteriorate, but also cracks occur during cold rolling. Therefore, the acid-soluble Al content in the steel piece is 0.010 to 0.070%. The acid-soluble Al content is preferably 0.020% to 0.050%.
[0066]
[N: 0.005 to 0.020%]
N binds to Al during the manufacturing process to form AlN that functions as an inhibitor. When the N content is less than 0.005%, AlN is not sufficiently generated and the magnetic characteristics deteriorate. Therefore, the N content of the steel piece is 0.005% or more.
On the other hand, when the N content exceeds 0.020%, AlN becomes difficult to function as an inhibitor, and not only may secondary recrystallization not occur, but also it causes cracking during cold rolling. Therefore, the N content of the steel piece is 0.020% or less. The N content is preferably 0.012% or less, more preferably 0.010% or less.
[0067]
[Remaining part: Fe and impurities]
The chemical composition of the steel piece is basically containing the above-mentioned elements and the remaining part is Fe and impurities. However, for the purpose of enhancing the magnetic properties, Bi, Te, Pb, Sb, Sn, Cr, and Cu may be further contained in the range shown below. Since these elements do not necessarily have to be contained, the lower limit is 0%.
Here, the impurities are those mixed from ore, scrap, or the manufacturing environment as a raw material when a steel piece (for example, a steel slab) is industrially manufactured, and the direction according to the present embodiment. It means a material that is allowed as long as it does not adversely affect the action of the electrical steel sheet.
[0068]
[At least one kind of Bi, Te, Pb (Bi + Te + Pb): 0 to 0.0300% in total] As
an optional element, at least one kind of Bi, Te or Pb is used instead of a part of the remaining Fe. , 0.0300% or less may be contained in total. By containing at least one of these elements, the magnetic properties of the grain-oriented electrical steel sheet can be further improved. The total content of at least one of Bi, Te or Pb is preferably 0.0005% or more, more preferably 0.0010% or more.
However, if the total content of these elements exceeds 0.0300%, it causes embrittlement during heat. Therefore, the total content of at least one of Bi, Te or Pb in the steel piece is preferably 0 to 0.0300%.
[0069]
In addition, the steel piece may further contain at least one of Sb, Sn, Cr, or Cu, which is effective for improving the magnetic properties of the grain-oriented electrical steel sheet. When these elements are contained, the content of each element is Sb: 0% or more and 0.50% or less, Sn: 0% or more and 0.50% or less, Cr: 0% or more and 0.50% or less, Cu: It is preferably 0% or more and 1.0% or less. The content of each is more preferably 0.005% or more, still more preferably 0.010% or more.
[0070]
The hot rolled sheet annealing step (step S103) is a step of annealing a hot rolled steel sheet produced through a hot rolling step to obtain a hot rolled sheet annealed steel sheet. By performing such an annealing treatment, recrystallization occurs in the steel sheet structure, and it becomes possible to realize good magnetic properties.
[0071]
In the hot-rolled sheet annealing step according to the present embodiment, the hot-rolled steel sheet manufactured through the hot-rolling step may be annealed to obtain a hot-rolled hardened steel sheet according to a known method. The means for heating the hot-rolled steel sheet during annealing is not particularly limited, and a known heating method can be adopted. The annealing conditions are also not particularly limited, but for example, the hot-rolled steel sheet can be annealed in a temperature range of 900 to 1200 ° C. for 10 seconds to 5 minutes.
[0072]
Such a hot-rolled plate annealing step can be omitted if necessary.
Further, after the hot-rolled sheet annealing step and before the cold rolling step described in detail below, the surface of the hot-rolled steel sheet may be pickled.
[0073]
In the
cold rolling step (step S105), the hot-rolled steel sheet after the hot-rolling step or the hot-rolled annealed steel sheet after annealing is subjected to one time or two or more times with intermediate annealing sandwiched between them. This is a process of cold rolling to obtain a cold-rolled steel sheet. Further, when the hot-rolled sheet is annealed as described above, the shape of the steel sheet becomes good, so that the possibility of the steel sheet breaking in the first rolling can be reduced. Further, the cold rolling may be carried out in three or more times, but it is preferable to carry out the cold rolling once or twice because the manufacturing cost increases.
[0074]
In the cold rolling step according to the present embodiment, the hot-rolled steel sheet or the hot-rolled annealed steel sheet may be cold-rolled to obtain a cold-rolled steel sheet according to a known method. For example, the final reduction rate can be in the range of 80% or more and 95% or less. If the final rolling reduction is less than 80%, there is a high possibility that a Goss nucleus having a {110} <001> orientation having a high degree of integration in the rolling direction cannot be obtained, which is not preferable. On the other hand, when the final reduction rate exceeds 95%, the secondary recrystallization is likely to become unstable in the final annealing step in the subsequent stage, which is not preferable. By setting the final rolling reduction ratio within the above range, a Goss nucleus having a {110} <001> orientation having a high degree of integration in the rolling direction can be obtained, and destabilization of secondary recrystallization can be suppressed.
The final reduction rate is the cumulative reduction rate of cold rolling, and when intermediate annealing is performed, it is the cumulative reduction rate of cold rolling after intermediate annealing.
[0075]
When cold rolling is performed two or more times with intermediate annealing in between, the first cold rolling has a reduction ratio of about 5 to 50% and a temperature of 950 ° C to 1200 ° C for about 30 seconds to 30 minutes. It is preferable to carry out intermediate annealing.
[0076]
Here, the thickness of the cold-rolled steel sheet (thickness after cold-rolling) is usually the thickness of the grain-oriented electrical steel sheet (thickness of the tension-applying insulating film) finally produced. Product plate thickness including) is different. The product thickness of grain-oriented electrical steel sheets is as mentioned earlier.
[0077]
In the cold rolling step as described above, it is also possible to give an aging treatment in order to further improve the magnetic properties. When cold rolling is performed by a plurality of passes, it is preferable to give the steel sheet a thermal effect of holding the steel sheet in a temperature range of 100 ° C. or higher for 1 minute or longer at any intermediate stage before the final pass. .. Due to such a thermal effect, it becomes possible to form a better primary recrystallization texture in the subsequent decarburization annealing step, and by extension, in the subsequent finish annealing step, the {110} <001> orientations are aligned in the rolling direction. It is possible to sufficiently develop a good secondary recrystallization structure.
[0078]
The decarburization annealing step (step S107) is a step of performing decarburization annealing on the obtained cold-rolled steel sheet to obtain a decarburization annealing steel sheet. In the method for producing grain-oriented electrical steel sheets according to the present embodiment, in the decarburization annealing step, the secondary recrystallized grain structure is controlled by performing an annealing treatment in accordance with predetermined heat treatment conditions.
[0079]
The decarburization annealing step according to the present embodiment is composed of two steps, a temperature raising step and a soaking step, in order to obtain a desired secondary recrystallized grain structure.
[0080]
In the temperature raising step in the decarburization annealing step, the rate of temperature rise until the decarburization annealing temperature is reached affects the Goss orientation accumulation degree after the secondary recrystallization through the change of the primary recrystallization texture. In the grain-oriented electrical steel sheet which is premised on having the recess 101 as described above, the base material which affects the magnetic properties after the tension-applying insulating film is formed and after the magnetic domain subdivision treatment. It is preferable to appropriately control the heating rate at the time of decarburization annealing because the effect of the Goss direction integration degree is large.
[0081]
From the viewpoint of improving the primary recrystallization texture, the temperature rising rate in the temperature range from 500 ° C. to 700 ° C. is preferably 300 ° C./sec or more. Here, the temperature rise rate S1 in the temperature rise process of 500 ° C. or higher and lower than 600 ° C. and the temperature rise rate S2 in the temperature rise process of 600 ° C. or higher and lower than 700 ° C. affect the primary recrystallization texture and decarburization annealing. The preferred range is different from the viewpoint of the influence on the oxide film formed at times. The temperature range of 500 ° C. or higher and lower than 600 ° C. has an effect not only on the primary recrystallization texture but also on the formation of Mn-based oxides, and the temperature range of 600 ° C. or higher and lower than 700 ° C. is only the primary recrystallization texture. It also has an effect on the formation of SiO 2 .
[0082]
In the present embodiment in which the formation of the glass film is suppressed by the annealing separator described later , the residence time is shortened in the temperature range of 600 ° C. or higher and 700 ° C. or lower at which SiO 2 that affects the glass film formation reaction is formed. Is preferable. Therefore, the heating rate S2 in the heating process of 600 ° C. or higher and 700 ° C. or lower is set to 1000 ° C./sec or more and 3000 ° C./sec or less, and is higher than the heating rate S1 in the heating rate process of 500 ° C. or higher and lower than 600 ° C. Is preferable. As described above, the heating rates S1 and S2 are represented by the following formulas (101) to (103) from the viewpoint of improving the primary recrystallization texture and obtaining a grain-oriented electrical steel sheet having no glass coating. It is preferable to satisfy the relationship to be established. By satisfying the relationships represented by the following formulas (101) to (103), it is possible to further improve the magnetic characteristics (iron loss) of the grain-oriented electrical steel sheet.
[0083]
300 ≤ S1 ≤ 1000 ... Equation (101)
1000 ≤ S2 ≤ 3000 ... Equation (102)
1.0 The
finish annealing step (step S109) is a step of applying a predetermined annealing separator to the decarburized annealed steel sheet obtained in the decarburization annealing step and then performing finish annealing. Here, finish annealing is generally performed for a long time in a state where the steel sheet is wound in a coil shape. Therefore, prior to finish annealing, an annealing separator is applied to the decarburized annealed steel sheet and dried for the purpose of preventing seizure between the inside and outside of the coil winding. In the method for producing grain-oriented electrical steel sheets according to the present embodiment, an annealing separator that does not form a glass film is used.
[0091]
As a quenching separator that does not form a glass film as described above, MgO and Al 2 O 3 are the main components (for example, Mg O and Al 2 O 3 contain 85% or more), and the mass ratio (MgO: Al 2 O 3) is used. ) Is in the range of 3: 7 to 7: 3, and an annealed separator containing 0.5 to 15% by mass of bismuth chloride is used. By using an annealing separator having such a mass ratio and a content of bismuth chloride, a base steel sheet having no glass coating and having good smoothness can be obtained.
[0092]
When the proportion of MgO exceeds the above range, a glass coating is formed on the surface of the steel sheet and remains, so that a base steel sheet having good smoothness cannot be obtained. Further, when the ratio of Al 2 O 3 exceeds the above range , seizure of Al 2 O 3 occurs, so that a base steel sheet having good smoothness cannot be obtained. The mass ratio of MgO to Al 2 O 3 (MgO: Al 2 O 3 ) is preferably in the range of 3.5: 6.5 to 6.5: 3.5.
[0093]
Further, since bismuth chloride has an effect of facilitating peeling of the formed glass film, if the content of bismuth chloride is less than 0.5% by mass, the glass film remains. .. On the other hand, when the content of bismuth chloride exceeds 15% by mass, the function of preventing seizure between the steel sheet and the steel sheet as an annealing separator is impaired. The content of bismuth chloride is preferably 3 to 7% by mass.
[0094]
Here, examples of the bismuth chloride include bismuth oxychloride (BiOCl) and bismuth trichloride (BiCl 3 ), and bismuth oxychloride is used from the reaction in the quenching separator during the finish annealing step. Compound species that can be formed may be used. Examples of the compound species capable of forming such bismuth oxychloride include a mixture of a bismuth compound and a metallic chlorine compound. Examples of the above-mentioned bismuth compound include bismuth oxide, bismuth hydroxide, bismuth sulfide, bismuth sulfate, bismuth phosphate, bismuth carbonate, bismuth nitrate, bismuth organic acid, bismuth halide and the like, and are metal chlorine compounds. Examples thereof include iron chloride, cobalt chloride, nickel chloride and the like.
[0095]
The above annealing separator is applied to the surface of the steel sheet after decarburization annealing and dried, and then finish annealing is performed. The heat treatment conditions of the finish annealing step according to the present embodiment are not particularly limited, and may be maintained, for example, in a temperature range of 1100 ° C. or higher and 1300 ° C. or lower for 10 hours or longer and 30 hours or shorter. Further, the atmosphere in the furnace may be a well-known nitrogen atmosphere or nitrogen hydrogen atmosphere. After finish annealing, it is preferable to remove excess annealing separator on the surface of the steel sheet by washing with water or pickling.
[0096]
The
surface processing step (step S111) is a step of performing surface processing by wet blasting on the entire surface of the steel sheet after finish annealing under the condition of satisfying the following formula (104). As a result, recesses 101 showing a characteristic distribution as described above are formed on the surface of the steel sheet after finish annealing.
[0097]
0.15 ≤ (S × c × ρ) / (6 × v × W) ≤ 3.00 ・ ・ ・ Equation (104)
[0098]
Here, in the above formula (104),
S: flow rate of slurry used for wet blasting (L / min)
c: concentration of polishing agent used for wet blasting (volume%)
ρ: density of polishing agent used for wet blasting (kg) / M 3 )
v: Relative speed between the nozzle for discharging the slurry and the steel plate (mm / sec)
W: Width of the nozzle for discharging the slurry (width of the slurry projection port) (mm)
.
[0099]
More specifically, after preparing a known wet blasting apparatus that can satisfy the condition of the above formula (104), such a wet blasting apparatus is installed on the surface processing line according to a conventional method of the wet blasting method. Wet blasting may be applied to the steel sheet after finish annealing. Here, the installation conditions of the wet blasting device and the like are not particularly limited, and the number of nozzles for discharging the slurry may be one or a plurality. ..
[0100]
The value represented by the central term of the above formula (104) corresponds to the amount of abrasive material projected per unit area. If the value represented by the central term exceeds 3.00, excessive recesses 101 are formed on the surface of the steel sheet (the number of recesses 101 having a depth of 0.1 μm or more and 2.0 μm or less is present). , 6.0 pieces / exceeding 100 μm), the magnetic properties of grain-oriented electrical steel sheets deteriorate. Further, the arithmetic average roughness Ra exceeds 0.60 μm, and the special magnetic zone property deteriorates. On the other hand, when the value represented by the central term is less than 0.15, the adhesion of the tension-applying insulating film and the effect of reducing iron loss due to the tension application are insufficient.
[0101]
Regarding the variable v in the above formula (104), in the case of a form in which the slurry is projected while the nozzle moves with respect to the stopped steel plate, the variable v corresponds to the moving speed of the nozzle. Further, in the case where the slurry is projected from the fixedly arranged nozzles on the steel plate conveyed on the continuous line, the variable v corresponds to the line speed.
[0102]
The solvent constituting the slurry is not particularly limited, but from the viewpoint of cost, for example, water can be used. Further, since the adhesion of the tension-imparting insulating film and the effect of reducing iron loss can be obtained by forming the desired recess 101, the type of abrasive used for wet blasting is not particularly limited, but the cost. From the viewpoint of the obtained effect, for example, it is preferable to use alumina having a central particle size of 40 to 60 μm.
[0103]
The
insulating film forming step (step S113) is a step of forming a tension-applying insulating film on one side or both sides of the cold-rolled steel sheet after surface processing. Here, the step of forming the insulating coating is not particularly limited, and the treatment liquid may be applied and dried by a known method using a known insulating coating treatment liquid as described below. By forming a tension-applying insulating film on the surface of the steel sheet, it is possible to further improve the magnetic properties of the grain-oriented electrical steel sheet.
[0104]
The surface of the steel sheet on which the insulating film is formed is a surface that has undergone any pretreatment such as degreasing with alkali or pickling with hydrochloric acid, sulfuric acid, phosphoric acid, etc. before applying the treatment liquid. It may be the surface as it is after finish annealing without these pretreatments.
[0105]
Here, the insulating film formed on the surface of the steel sheet is not particularly limited as long as it is used as the insulating film of the grain-oriented electrical steel sheet, and a known insulating film can be used. Examples of such an insulating film include a composite insulating film mainly composed of an inorganic substance and further containing an organic substance. Here, the composite insulating coating is mainly composed of at least one of an inorganic substance such as a metal chromate salt, a metal phosphate salt or a colloidal silica, a Zr compound, and a Ti compound, and fine organic resin particles are dispersed. It is an insulating film. In particular, from the viewpoint of reducing the environmental load during manufacturing, which has been in increasing demand in recent years, an insulating film using a metal phosphate, a Zr or Ti coupling agent, or these carbonates or ammonium salts as a starting material is used. It is preferably used.
[0106]
Further, following the insulating film forming step as described above, flattening annealing for shape correction may be performed. By flattening and annealing the steel sheet, it is possible to further reduce iron loss.
[0107]
In the method for producing grain-oriented electrical steel sheets according to the present embodiment, the magnetic domain subdivision treatment may be performed after the finish annealing step or the insulating film forming step. The magnetic domain subdivision treatment is a process of irradiating the surface of a grain-oriented electrical steel sheet with a laser beam having a magnetic domain subdivision effect or forming a groove on the surface. By such magnetic domain subdivision treatment, a grain-oriented electrical steel sheet having further excellent magnetic properties can be manufactured.
[0108]
By going through the steps as described above, the grain-oriented electrical steel sheet according to the present embodiment can be manufactured.
[0109]
The method for manufacturing the grain-oriented electrical steel sheet according to the present embodiment has been described in detail above.
Example
[0110]
Hereinafter, the technical contents of the present invention will be further described with reference to Examples and Comparative Examples. The conditions of the examples shown below are one-condition examples adopted for confirming the feasibility and effect of the present invention, and the present invention is not limited to this one-condition example. Further, the present invention can adopt various conditions as long as the gist of the present invention is not deviated and the object of the present invention is achieved.
[0111]
(Experimental Example 1)
C: 0.082% by mass, Si: 3.30% by mass, Mn: 0.082% by mass, S: 0.023% by mass, acid-soluble Al: 0.025% by mass, N: 0 Steel slab A containing .008 mass% and the balance consisting of Fe and impurities, C: 0.081 mass%, Si: 3.30 mass%, Mn: 0.083 mass%, S: 0.022 mass %, Acid-soluble Al: 0.025% by mass, N: 0.008% by mass, Bi: 0.0025% by mass, and steel slab B containing Fe and impurities as the balance was heated to 1350 ° C., respectively. Hot rolling was performed to obtain a hot-rolled steel sheet having a thickness of 2.3 mm. Each of the obtained hot-rolled steel sheets was annealed at 1100 ° C. for 120 seconds and then pickled. The hot-rolled steel sheet after pickling was finished to 0.23 mm by cold rolling to obtain a cold-rolled steel sheet. Then, the obtained cold-rolled steel sheet was subjected to decarburization annealing. In such decarburization annealing, each cold-rolled steel sheet has a temperature rise rate S1 of 400 ° C./sec in the temperature rise process of 500 ° C. or higher and lower than 600 ° C., and a temperature rise rate S2 in the temperature rise process of 600 ° C. or higher and 700 ° C. or lower. It was heated at 1100 ° C./sec (S2 / S1 = 2.75) and held at 850 ° C. for 120 seconds. Then, an annealing separator having a composition of MgO and Al 2 O 3 having a mass ratio of 50%: 50% (mass ratio 1: 1) and containing 5% by mass of BiOCl was applied and dried. It was subjected to finish annealing at 1200 ° C. for 20 hours.
[0112]
When the excess annealing separator of each of the obtained steel sheets was removed by washing with water, no glass film was formed on any of the steel sheets. Further, when a chemical analysis was carried out after removing the excess annealing separator by washing with water, all the steel sheets had a C content of 0.001% or less, sol. Al content: 0.005% or less, S content: 0.005% or less, N content: 0.005% or less. The Si content was 3.30%, the Mn content was 0.050 to 0.083%, and the Bi content was 0 to 0.0025%.
[0113]
A test piece was cut out from a steel sheet from which excess annealing separator was removed by washing with water, and after strain removal annealing was performed, alumina abrasive grains having a central particle size of 50 μm using water as a solvent were used as a slurry, and a nozzle movement speed v: 200 mm. After fixing the conditions of / sec and nozzle width w: 250 mm, the slurry flow rate and the abrasive concentration were changed, and the slurry was projected onto both sides of the steel sheet by wet blasting. In test numbers 1-10 to 1-13, 1-22 to 1-25, 1-28, and 1-29 shown below, the amount of slurry projected was changed by performing the projection a plurality of times. Further, in Test Nos. 1-26 and 1-27, the surface texture was made smooth without performing wet blasting.
[0114]
Then, an aqueous solution containing aluminum phosphate and colloidal silica as main components is applied to each test piece and baked at 850 ° C. for 1 minute to impart a tension of 4.5 g / m 2 to the surface of the test piece. A sex insulating film was formed. The obtained test piece was irradiated with a laser beam to carry out magnetic domain subdivision treatment.
[0115]
Each of the obtained test pieces was evaluated from the viewpoints of magnetic properties, surface shape of the base steel sheet, and adhesion of the tension-applying insulating film. The evaluation method is as follows.
[0116]
[Magnetic characteristics] A
method for measuring magnetic characteristics using a single plate tester specified in JIS C 2556 (2015). Magnetic flux density B8 (magnetic flux density at 800 A / m) and iron loss W17 / 50 (at 50 Hz) in the rolling direction. Iron loss when magnetized to 1.7T) was evaluated respectively.
[0117]
[Surface shape of base steel sheet]
Arithmetic mean of rolling 90 ° direction after wet blasting for recesses formed on the surface of base steel sheet by wet blasting using a surface roughness meter (Surf coder manufactured by Kosaka Research Institute). Roughness Ra was measured. In addition, the 90 ° rolling cross section of the steel sheet after wet blasting was observed with a scanning electron microscope (JSM-IT300), and the number of recesses having a depth of 0.1 μm or more and 2.0 μm or less was evaluated. As described above, the observation was carried out in three fields at 1000 times, and the average value was calculated from the obtained measurement results.
[0118]
[Adhesion of
Tension-Applying Insulation Coating ] The adhesion of the tension-applying insulating coating is determined by using a test piece collected with the rolling direction as the longitudinal direction and using a cylindrical mandrel bending tester with a bending diameter of φ10 and a bending diameter of φ20. It was evaluated by the bending test of. For the evaluation, the ratio of the area of the tension coating remaining without peeling (coating residual ratio) to the area of the bent portion on the surface of the test piece after the bending test was calculated, and the judgment was made based on the coating residual ratio. .. The judgment criteria are as follows, and the scores A and B were accepted.
[0119]
Score A: Film residual rate 90% or more
B: Film residual rate 70% or more and less than 90%
C: Film residual rate less than 70%
[0120]
The results obtained are summarized in Table 1 below.
[0121]
[table 1]
[0122]
As is clear from Table 1 above, in test numbers 1-1 to 1-7 and 1-14 to 1-20 in which the wet blast condition is within the range of the present invention, the surface shape of the base steel sheet is within the range of the present invention. Both the magnetic properties and the film adhesion were good. Comparing test numbers 1-1 to 1-7 and 1-14 to 1-20, test numbers 1-14 to 1-20, in which the steel slab has a preferable chemical composition, have excellent magnetic properties. Was.
[0123]
On the other hand, in the comparative examples of test numbers 1-8 to 1-13, 1-21 to 1-25, 1-28, and 1-29, the wet blast condition is outside the scope of the present invention, and the base material is used. The surface shape of the steel sheet was also outside the scope of the present invention and was particularly inferior in magnetic properties. Test numbers 1-26 and 1-27 are inferior in the adhesion of the tension-applying insulating coating because wet blasting is not performed, and the coating is seized not only on the bent portion but also on the flat portion other than the bent portion. Immediately after, the coating had already peeled off. In addition, the iron loss was inferior to that of the invention example using steels A and B.
[0124]
(Experimental Example 2) The
steel slab shown in Table 2 below was heated to 1380 ° C. and hot-rolled to obtain a hot-rolled steel sheet having a thickness of 2.3 mm. Some steel cracked and could not proceed to the next process. The hot-rolled steel sheet that was able to proceed to the next step was annealed at 1120 ° C. for 20 seconds and then pickled. However, for test number 2-2, pickling was carried out without annealing the hot-rolled steel sheet. The pickled steel sheet was finished to 0.23 mm by cold rolling to obtain a cold-rolled steel sheet. Some steels cracked during cold rolling and could not proceed to the next process. Decarburization annealing was performed on the cold-rolled steel sheet that could be advanced to the next process. In such decarburization annealing, the temperature rise rate S1 in the temperature rise process of 500 ° C. or higher and lower than 600 ° C. is 900 ° C./sec, and the temperature rise rate S2 in the temperature rise process of 600 ° C. or higher and 700 ° C. or lower is set for each cold-rolled steel sheet. It was heated to 1600 ° C./sec (S2 / S1 = 1.78) and held at 850 ° C. for 150 seconds. After that, it is composed of MgO, Al 2 O 3 and chloride, and the blending ratio of MgO and Al 2 O 3 is 50%: 50% (mass ratio 1: 1) by mass%, and contains 6% by mass of BiOCl. A quenching separator of composition was applied and dried. Then, the decarburized annealed steel sheet was subjected to finish annealing at 1200 ° C. for 20 hours.
[0125]
When the excess annealing separator of the obtained steel sheet was removed by washing with water, no glass film was formed on any of the steel sheets. Further, when a chemical analysis was carried out after removing the excess annealing separator by washing with water, all the steel sheets had a C content of 0.001% or less, sol. Al content: 0.005% or less, S + Se content: 0.005% or less, N content: 0.005% or less. The Si content was the same as in the slab stage, the Mn content was 0.050 to 1.000%, and the Bi + Te + Pb (total content) was 0 to 0.0300%. The contents of Sb, Sn and Cr were 0 to 0.04%, and the content of Cu was 0 to 0.05%.
[0126]
A test piece was cut out from a steel sheet from which excess annealing separator was removed by washing with water, and after strain removal annealing was performed, alumina abrasive grains having a central particle size of 50 μm using water as a solvent were used as a slurry, and a nozzle moving speed v: 200 mm. Conditions are set to / sec, nozzle width w: 250 mm, slurry flow rate S: 15 l / min, abrasive material concentration c: 1 volume% ((S × c × ρ) / (6 × v × W)) = 0.20) After fixing, the slurry was projected onto both sides of the steel sheet by wet blasting. In Test No. 2-24 shown below, wet blasting was not performed and the surface condition was a smooth surface. Then, an aqueous solution containing aluminum phosphate and colloidal silica as main components is applied and baked at 850 ° C. for 1 minute to form a tension-imparting insulating film having a basis weight of 4.5 g / m 2 on the surface of the test piece. It was.
[0127]
[Table 2]
[0128]
The magnetic properties, the surface shape of the base steel sheet, and the adhesion of the tension-applying insulating coating were evaluated for each of the obtained test pieces. The method for evaluating the surface shape of the base steel sheet and the adhesion of the tension-applying insulating film was the same as in Experimental Example 1. The magnetic characteristics were evaluated as follows. The results obtained are summarized in Table 3 below.
[0129]
[Magnetic characteristics] The magnetic characteristics
in the rolling direction were evaluated by the method for measuring the magnetic characteristics using a single plate tester specified in JIS C 2556 (2015). At the time of evaluation, the magnetic flux density B8 (magnetic flux density at 800 A / m) was measured, and it was judged that good secondary recrystallization was expressed under the condition that a value of more than 1.90 T was obtained, and the test piece. Was irradiated with a laser beam to carry out magnetic domain subdivision treatment. Then, the iron loss W17 / 50 (iron loss when magnetized to 1.7 T at 50 Hz) after laser irradiation was evaluated.
[0130]
[Table 3]
[0131]
As is clear from Table 3 above, Test No. 2-12 broke during cold rolling because the Si content exceeded the upper limit of the present invention. Test No. 2-13 was inferior in magnetic properties because the Si content was below the lower limit of the present invention. In test number 2-14, the C content was below the lower limit of the present invention, and in test number 2-15, the C content exceeded the upper limit of the present invention, both of which were inferior in magnetic properties. .. In Test No. 2-16, the acid-soluble Al content was below the lower limit of the present invention, and the magnetic properties were inferior. In Test No. 2-17, the acid-soluble Al content exceeded the upper limit of the present invention and was broken during cold rolling. In test number 2-18, the Mn content was below the lower limit of the present invention, and in test number 2-19, the Mn content exceeded the upper limit of the present invention, both of which were inferior in magnetic properties. .. In Test No. 2-20, the total content of S + Se was below the lower limit of the present invention, and the magnetic properties were inferior. In test number 2-21, the total content of S + Se exceeded the upper limit of the present invention, and cracks occurred during hot rolling. In test number 2-22, the N content exceeded the upper limit of the present invention, and cracks occurred during cold rolling. In Test No. 2-23, the N content was below the lower limit of the present invention, and the magnetic properties were inferior. In Test No. 2-24, since the wet blast was not performed, the film adhesion was inferior, and the film peeling had already occurred not only in the bent portion but also in the flat portion other than the bent portion immediately after the film was baked. In addition, it was inferior in iron loss as compared with other test numbers (2-1 to 2-11) in which laser irradiation was performed.
[0132]
On the other hand, in the test numbers 2-1 to 2-11 and 2-25 to 2-29 whose chemical composition is within the range of the present invention, the surface shape of the base steel sheet is within the range of the present invention, and the magnetic properties and magnetic properties Both film adhesions showed good results. In addition, test numbers 2-3 to 2-11 and 2-25 to 2-29, in which steel slabs have a preferable chemical composition, had superior magnetic properties as compared with test numbers 2-1. ..
[0133]
(Experimental Example 3) The
steel slab shown in Table 4 below was heated to 1380 ° C. and hot-rolled to obtain a hot-rolled steel sheet having a thickness of 2.3 mm. Then, the hot-rolled steel sheet was annealed at 1120 ° C. for 120 seconds and then pickled. The pickled steel sheet was finished to 0.23 mm by cold rolling to obtain a cold-rolled steel sheet. Then, the obtained cold-rolled steel sheet was subjected to decarburization annealing. At that time, heating is performed by changing the heating rate S1 (° C./sec) in the heating process of 500 ° C. or higher and lower than 600 ° C. and the heating rate S2 (° C./sec) in the heating rate process of 600 ° C. or higher and 700 ° C. or lower. Then, it was held at 850 ° C. for 150 seconds. Then, the annealing separator was applied, dried, and subjected to finish annealing at 1200 ° C. for 20 hours. The annealing separator was the following five types.
[0134]
(A) The blending ratio of MgO and Al 2 O 3 was 50%: 50% by mass, and the blending ratio of
(B) MgO and Al 2 O 3 containing BiOCl: 5% by mass was mass%. in 80%: and 20%, BiOCl: 5 wt% annealing separator which contains the
(C) MgO and Al 2 O 3 20% blending ratio in weight%: and 80%, BiOCl: containing 5 wt% The blending ratio of the annealed separating agent
(D) MgO and Al 2 O 3 was 80%: 20% by mass, and the blending ratio of the annealing separator
(E) MgO and Al 2 O 3 containing no BiOCl was mass%. 20%: 80%, and a quenching separator that does not contain BiOCl.
[0135]
When the excess annealing separating agent of the obtained steel sheet was removed by washing with water, no glass film was formed on the steel sheet using the annealing separating agent A. The steel sheet using the annealing separators B, C, D, and E did not have a smooth surface due to the glass coating formed on the surface or the alumina burned on the surface. Chemical analysis was performed on the steel sheets using the annealing separator A after removing the excess annealing separator by washing with water. As a result, the C content of all the steel sheets was 0.001% or less, sol. Al content: 0.005% or less, S content: 0.005% or less, N content: 0.005% or less. The Si content was the same as in the slab stage, the Mn content was 0.050 to 0.082%, and the Bi + Te + Pb (total content) was 0 to 0.0300%.
[0136]
A test piece was cut out from a steel sheet from which excess annealing separator was removed by washing with water, and after strain removal annealing was performed, alumina abrasive grains having a central particle size of 50 μm using water as a solvent were used as a slurry, and a nozzle moving speed v: 200 mm. After fixing the nozzle width w: 250 mm at / sec, the slurry flow rate S and the abrasive concentration c were changed, and the slurry was projected onto both sides of the steel sheet by wet blasting. In Test No. 3-17 shown below, wet blasting was not performed and the surface texture was made smooth. Then, an aqueous solution containing aluminum phosphate and colloidal silica as main components is applied and baked at 850 ° C. for 1 minute to form a tension-imparting insulating film having a basis weight of 4.5 g / m 2 on the surface of the test piece. It was. The obtained test piece was irradiated with a laser beam to carry out magnetic domain subdivision treatment.
[0137]
[Table 4]
[0138]
Each of the obtained test pieces was evaluated from the viewpoints of magnetic properties, surface shape of the base steel sheet, and adhesion of the tension-applying insulating film. The evaluation method was the same as in Experimental Example 1. The results obtained are summarized in Table 5 below.
[0139]
[Table 5]
[0140]
Test numbers 3-13 to 3-16, where the annealing separator is outside the scope of the present invention, have a smooth surface due to the glass coating formed on the surface or the alumina burned onto the surface. There wasn't. In order to remove the glass film or alumina, it was necessary to increase the projection amount by wet blasting, but since the wet blasting conditions are outside the scope of the present invention, the surface shape of the base steel sheet is the present invention. It was out of range and inferior in magnetic characteristics. In Test Nos. 3-17 and 3-18, the annealing separator was within the scope of the present invention, the glass film was not formed on the surface after the washing with water, and the surface was smooth. In Test No. 3-17, since wet blasting was not performed, the film adhesion was inferior, and the film peeling had already occurred not only in the bent portion but also in the flat portion other than the bent portion immediately after the film was baked. In test number 3-18, the wet blast condition exceeded the upper limit of the present invention, the surface shape was not within the range of the present invention, and the magnetic properties were inferior. In Test No. 3-19, the conditions at the time of decarburization annealing were outside the more preferable range of the present invention, and the magnetic properties were slightly inferior to those of other examples. In test number 3-20, the wet blast condition was below the lower limit, and the film adhesion was inferior.
[0141]
On the other hand, in Test Nos. 3-1 to 3-12 in which the annealing separator was within the scope of the present invention, no glass film was formed on the surface after the washing with water, and the surface had a smooth surface. Further, since the wet blast condition was within the range of the present invention, the surface shape of the base steel sheet was within the range of the present invention, and excellent magnetic properties and film adhesion were exhibited. Comparing test numbers 3-1 to 3-3, 3-4 to 3-7, and 3-8 to 3-12, test numbers 3-4 to 3-12, in which the steel slab has a preferable chemical composition, are better. It has excellent magnetic properties, and has a heating rate of S1 (° C / sec) in the heating process of 500 ° C or higher and lower than 600 ° C during decarburization annealing, and a heating rate in the heating process of 600 ° C or higher and 700 ° C or lower. Test numbers 3-6 to 12 in which S2 (° C./sec) satisfied the preferable range of the present invention had even better magnetic properties.
[0142]
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. , These are also naturally understood to belong to the technical scope of the present invention.
Description of the sign
[0143]
10 Electrical steel sheet
11 Base steel sheet
13 Tension-applying insulating film
101 Recess
The scope of the claims
[Claim 1]
By mass%,
C: 0.010% or less,
Si: 2.50 to 4.00%,
Mn: 0.050 to 1.000%,
S + Se: 0.005% or less in total,
Sol. Al: 0.005% or less,
N: 0.005% or less,
Bi + Te + Pb: 0 to 0.0300% in total,
Sb: 0 to 0.50%,
Sn: 0 to 0.50%,
Cr: 0 to 0 A base steel sheet containing .50% and
Cu: 0 to 1.0%
and having a chemical composition in which the balance is Fe and impurities, and
a tension-imparting insulating coating provided on the surface of the base steel sheet.
The
arithmetic average roughness Ra along the rolling 90 ° direction, which is a direction perpendicular to the rolling direction, is 0.60 μm or less on the surface of the base steel sheet, and is along the
rolling 90 ° direction. When observing the cross section of the base steel sheet, there are 1.0 / 100 μm or more and 6.0 / 100 μm or less recesses on the surface of the base steel sheet having a depth of 0.1 μm or more and 2.0 μm or less. An existing
directional electromagnetic steel sheet.
[Claim 2]
The
grain-
oriented electrical steel sheet according to claim 1 , wherein the base metal steel sheet contains Bi + Te + Pb: 0.0005 to 0.0300% in total as the chemical composition .
[Claim 3]
By mass%, C: 0.020 to 0.100%, Si: 2.50 to 4.00%, Mn: 0.050 to 1.000%, S + Se: 0.005 to 0.080% in total, Sol. Al: 0.010 to 0.070%, N: 0.005 to 0.020%, Bi + Te + Pb: 0 to 0.0300% in total, Sb: 0 to 0.50%, Sn: 0 to 0.50% , Cr: 0 to 0.50%, Cu: 0 to 1.0%, and the hot rolling step of heating a steel piece whose balance is Fe and impurities and then hot rolling to obtain a hot-rolled steel sheet. ,
Arbitrarily, a hot-rolled sheet steel sheet annealing step of quenching the hot-rolled steel sheet to obtain a hot-rolled burnt steel
sheet, and one cold rolling or intermediate quenching of the hot-rolled steel sheet or the hot-rolled tempered steel sheet. subjected to multiple cold rolling sandwiching and a cold rolling to obtain a cold-rolled steel sheet,
subjected to decarburization annealing to the cold-rolled steel sheet, and decarburization annealing to obtain a decarburization annealed steel sheet,
said de
Wet under the condition that the following formula (1) is satisfied for the finish annealing step of applying the quenching separator to the charcoal-baked steel sheet and then performing the finish annealing and the entire sheet width direction of the steel sheet surface after the finish annealing step. The annealing separator includes MgO and Al 2 O 3 including a surface processing step of performing surface processing by blasting and
an insulating film forming step of forming a tension-imparting insulating film on the surface of the steel sheet after the surface processing step. Is the main component, and the MgO and the Al 2 O 3
A method for producing a directional electromagnetic steel plate, wherein MgO: Al 2 O 3 having a mass ratio of 3 to 7: 3 is in the range of 3: 7 to 7: 3, and 0.5 to 15% by mass of bismuth chloride is contained
.
0.15 ≤ (S × c × ρ) / (6 × v × W) ≤ 3.00 ・ ・ ・ Equation (1)
Here, in the above equation (1),
S: Flow rate of the slurry used for the wet blasting. (L / min)
c: Concentration of the polishing agent used for the wet blast (% by volume)
ρ: Density of the polishing agent used for the wet blast (kg / m 3 )
v: Nozzle and steel plate to which the slurry is discharged Relative velocity (mm / sec)
W: The width (mm)
of the nozzle from which the slurry is discharged .
[Claim 4]
In the decarburization annealing step, the heating rate S1 in the temperature range of 500 ° C. or higher and lower than 600 ° C. and the heating rate S2 in the temperature range of 600 ° C. or higher and 700 ° C. or lower are expressed by the following equations (2) to (2). The
method for manufacturing a directional electromagnetic steel sheet according to claim 3 , which satisfies each of the 4) .
300 ≤ S1 ≤ 1000 ... Equation (2)
1000 ≤ S2 ≤ 3000 ... Equation (3)
1.0
| # | Name | Date |
|---|---|---|
| 1 | 202017039121-IntimationOfGrant28-06-2022.pdf | 2022-06-28 |
| 1 | 202017039121-TRANSLATIOIN OF PRIOIRTY DOCUMENTS ETC. [10-09-2020(online)].pdf | 2020-09-10 |
| 2 | 202017039121-PatentCertificate28-06-2022.pdf | 2022-06-28 |
| 2 | 202017039121-STATEMENT OF UNDERTAKING (FORM 3) [10-09-2020(online)].pdf | 2020-09-10 |
| 3 | 202017039121-REQUEST FOR EXAMINATION (FORM-18) [10-09-2020(online)].pdf | 2020-09-10 |
| 3 | 202017039121-Correspondence-180422.pdf | 2022-04-19 |
| 4 | 202017039121-PROOF OF RIGHT [10-09-2020(online)].pdf | 2020-09-10 |
| 4 | 202017039121-Others-180422-1.pdf | 2022-04-19 |
| 5 | 202017039121-PRIORITY DOCUMENTS [10-09-2020(online)].pdf | 2020-09-10 |
| 5 | 202017039121-Others-180422.pdf | 2022-04-19 |
| 6 | 202017039121-POWER OF AUTHORITY [10-09-2020(online)].pdf | 2020-09-10 |
| 6 | 202017039121-ABSTRACT [14-04-2022(online)].pdf | 2022-04-14 |
| 7 | 202017039121-FORM 18 [10-09-2020(online)].pdf | 2020-09-10 |
| 7 | 202017039121-CLAIMS [14-04-2022(online)].pdf | 2022-04-14 |
| 8 | 202017039121-FORM 1 [10-09-2020(online)].pdf | 2020-09-10 |
| 8 | 202017039121-DRAWING [14-04-2022(online)].pdf | 2022-04-14 |
| 9 | 202017039121-DRAWINGS [10-09-2020(online)].pdf | 2020-09-10 |
| 9 | 202017039121-FER_SER_REPLY [14-04-2022(online)].pdf | 2022-04-14 |
| 10 | 202017039121-DECLARATION OF INVENTORSHIP (FORM 5) [10-09-2020(online)].pdf | 2020-09-10 |
| 10 | 202017039121-OTHERS [14-04-2022(online)].pdf | 2022-04-14 |
| 11 | 202017039121-COMPLETE SPECIFICATION [10-09-2020(online)].pdf | 2020-09-10 |
| 11 | 202017039121-FORM 4(ii) [13-01-2022(online)].pdf | 2022-01-13 |
| 12 | 202017039121-FER.pdf | 2021-10-19 |
| 12 | 202017039121-Verified English translation [09-12-2020(online)].pdf | 2020-12-09 |
| 13 | 202017039121-FORM 3 [08-02-2021(online)].pdf | 2021-02-08 |
| 13 | 202017039121.pdf | 2021-10-19 |
| 14 | 202017039121-FORM 3 [08-02-2021(online)].pdf | 2021-02-08 |
| 14 | 202017039121.pdf | 2021-10-19 |
| 15 | 202017039121-FER.pdf | 2021-10-19 |
| 15 | 202017039121-Verified English translation [09-12-2020(online)].pdf | 2020-12-09 |
| 16 | 202017039121-COMPLETE SPECIFICATION [10-09-2020(online)].pdf | 2020-09-10 |
| 16 | 202017039121-FORM 4(ii) [13-01-2022(online)].pdf | 2022-01-13 |
| 17 | 202017039121-OTHERS [14-04-2022(online)].pdf | 2022-04-14 |
| 17 | 202017039121-DECLARATION OF INVENTORSHIP (FORM 5) [10-09-2020(online)].pdf | 2020-09-10 |
| 18 | 202017039121-DRAWINGS [10-09-2020(online)].pdf | 2020-09-10 |
| 18 | 202017039121-FER_SER_REPLY [14-04-2022(online)].pdf | 2022-04-14 |
| 19 | 202017039121-DRAWING [14-04-2022(online)].pdf | 2022-04-14 |
| 19 | 202017039121-FORM 1 [10-09-2020(online)].pdf | 2020-09-10 |
| 20 | 202017039121-CLAIMS [14-04-2022(online)].pdf | 2022-04-14 |
| 20 | 202017039121-FORM 18 [10-09-2020(online)].pdf | 2020-09-10 |
| 21 | 202017039121-ABSTRACT [14-04-2022(online)].pdf | 2022-04-14 |
| 21 | 202017039121-POWER OF AUTHORITY [10-09-2020(online)].pdf | 2020-09-10 |
| 22 | 202017039121-Others-180422.pdf | 2022-04-19 |
| 22 | 202017039121-PRIORITY DOCUMENTS [10-09-2020(online)].pdf | 2020-09-10 |
| 23 | 202017039121-Others-180422-1.pdf | 2022-04-19 |
| 23 | 202017039121-PROOF OF RIGHT [10-09-2020(online)].pdf | 2020-09-10 |
| 24 | 202017039121-Correspondence-180422.pdf | 2022-04-19 |
| 24 | 202017039121-REQUEST FOR EXAMINATION (FORM-18) [10-09-2020(online)].pdf | 2020-09-10 |
| 25 | 202017039121-STATEMENT OF UNDERTAKING (FORM 3) [10-09-2020(online)].pdf | 2020-09-10 |
| 25 | 202017039121-PatentCertificate28-06-2022.pdf | 2022-06-28 |
| 26 | 202017039121-TRANSLATIOIN OF PRIOIRTY DOCUMENTS ETC. [10-09-2020(online)].pdf | 2020-09-10 |
| 26 | 202017039121-IntimationOfGrant28-06-2022.pdf | 2022-06-28 |
| 1 | 202017039121_SSE_15-07-2021.pdf |