US20260049381A1 - Grain-oriented electrical steel sheet - Google Patents

Grain-oriented electrical steel sheet

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Publication number
US20260049381A1
US20260049381A1 US18/994,823 US202318994823A US2026049381A1 US 20260049381 A1 US20260049381 A1 US 20260049381A1 US 202318994823 A US202318994823 A US 202318994823A US 2026049381 A1 US2026049381 A1 US 2026049381A1
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mass
less
steel sheet
content
grain
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US18/994,823
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Takeshi Imamura
Yukihiro Shingaki
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JFE Steel Corp
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JFE Steel Corp
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    • C21D6/00—Heat treatment of ferrous alloys
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    • C21D8/00—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
    • C21D8/02—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0221—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the working steps
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    • C21D8/00—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
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    • C21D8/00—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
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    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
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    • C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
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    • C22C38/52—Ferrous alloys, e.g. steel alloys containing chromium with nickel with cobalt
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    • C22C38/60—Ferrous alloys, e.g. steel alloys containing lead, selenium, tellurium, or antimony, or more than 0.04% by weight of sulfur
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
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    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
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    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/147—Alloys characterised by their composition
    • H01F1/14766—Fe-Si based alloys
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
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    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
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    • H01F1/147—Alloys characterised by their composition
    • H01F1/14766—Fe-Si based alloys
    • H01F1/14791—Fe-Si-Al based alloys, e.g. Sendust
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    • C21D2201/00—Treatment for obtaining particular effects
    • C21D2201/05—Grain orientation

Definitions

  • the present disclosure relates to a grain-oriented electrical steel sheet advantageously utilized for an iron core of a transformer.
  • Grain-oriented electrical steel sheets are soft magnetic materials used as iron core materials for transformers, and have crystal microstructures in which the ⁇ 001> orientation, which is an easy magnetization axis of iron, is highly accorded with the rolling direction of the steel sheets. Such texture is formed through a phenomenon called secondary recrystallization where crystal grains with ⁇ 110 ⁇ 001> orientation, also known as Goss orientation, grow preferentially to large sizes during purification annealing in the process of producing a grain-oriented electrical steel sheet.
  • Patent Literature 1 describes a method using AlN and MnS
  • PTL 2 describes a method using MnS and MnSe, and both of these methods have been put into industrial use.
  • Grain-oriented electrical steel sheets which are mainly used as iron cores of transformers, are required to have excellent magnetization properties, in particular low iron loss. To achieve this, it is important to highly align the secondary recrystallized grains in a steel sheet to the Goss orientation and to decrease impurities in the product sheet. Further, techniques have been developed for introducing non-uniformity to the steel sheet surfaces by physical means to subdivide magnetic domain width for less iron loss, namely, magnetic domain refining techniques. For example, PTL 4 proposes a technique of irradiating a steel sheet after final annealing with a laser to introduce high-dislocation density regions into a surface layer of the steel sheet, thereby narrowing magnetic domain widths and decreasing iron loss of the steel sheet. Further, PTL 5 proposes a technique of controlling magnetic domain widths by irradiation with an electron beam.
  • grain-oriented electrical steel sheets are mainly used as the iron cores of transformers.
  • the iron loss ratio of the two (the iron loss of the transformer iron core divided by the iron loss value of the material) is called the building factor. That is, even when the iron loss of the material is low, when the building factor is high, the iron loss of the transformer iron core is large, creating a problem of insufficient performance.
  • the building factor affects not only transformer design but also material properties, and therefore there is a demand to lower the building factor as well as the iron loss of the material.
  • a grain-oriented electrical steel sheet that can obtain a low building factor can be produced by controlling, within certain ranges, the Co content in a base steel sheet, on which a base film mainly composed of forsterite is formed, and the Ti content in the grain-oriented electrical steel sheet with the base film formed thereon.
  • steel slabs were produced by continuous casting, containing, in mass %, C: 0.050% to 0.081%, Si: 3.15% to 3.31%, Mn: 0.07% to 0.10%, Al: 0.020% to 0.025%, N: 0.0069% to 0.0085%, S: 0.0011% to 0.0031%, Sb: 0.025% to 0.036%, Co: 0% to 0.123%, and Ti: 0.0080% to 0.0090%, with the balance being Fe and inevitable impurity. After slab heating and soaking at 1400° C. for 20 min, the slabs were hot rolled to a thickness of 2.4 mm. Subsequently, hot-rolled sheet annealing was carried out at 1000° C.
  • the heating rate to 1200° C. was 20° C./h. Further, during the heating process, an N 2 atmosphere was used from room temperature to 700° C., an atmosphere in which the mixing ratio of N 2 and H 2 was varied was used from 700° C. to 1100° C., and an H 2 atmosphere was used from 1100° C. to 1200° C. Further, an H 2 atmosphere was used during the hold time, and an Ar atmosphere was used during cooling. In this way, samples were obtained where a base film consisting mainly of forsterite (hereinafter also referred to as forsterite film) was formed on the surface of each base steel sheet.
  • forsterite film a base film consisting mainly of forsterite
  • the iron loss W 17/50 iron loss when excited at 50 Hz up to 1.7 T
  • W 19/50 iron loss when excited at 50 Hz up to 1.9 T
  • hysteresis loss Wh 17 hysteresis loss when excited up to 1.7 T
  • Wh 19 hysteresis loss when excited up to 1.9 T
  • a three-phase three-leg model transformer simulating a transformer was fabricated having an external shape of 500 mm square and a sheet width of 100 mm for each leg and each yoke, and model transformer iron loss WT 17/50 (transformer iron loss when excited at 50 Hz to 1.7 T) was measured.
  • the number of stacked sheets of each sample was 50, with two sheets stacked alternately.
  • the building factor F17 of the model transformer was then calculated as the model transformer iron loss WT 17/50 divided by the sample iron loss W 17/50 (WT 17/50 /W 17/50 ).
  • the relationship between the building factor F17 and the amount of Co in the base steel sheet is illustrated in FIG. 1 .
  • FIG. 1 The results illustrated in FIG. 1 indicate no clear correlation between the building factor F17 and Co content. However, it can be read from FIG. 1 that the building factor F17 is divided into good values of 1.25 or less and high values of 1.30 or more.
  • FIG. 2 is the result of extracting and redrawing only the group A of the data in FIG. 1 .
  • results illustrated in FIG. 2 indicate that results belonging to group A, that is, having the relationship 0.30 ⁇ R17 ⁇ R19, in a Co content range from 0.005% to 0.050%, indicate a good building factor of 1.25 or less.
  • Steel slabs were produced by continuous casting, containing, in mass %, C: 0.037%, Si: 3.05%, Mn: 0.18%, Al: 0.009%, N: 0.0036%, Se: 0.007%, Sn: 0.062%, and Co: 0.0080%, with the balance being Fe and inevitable impurity.
  • hot-rolled sheet annealing was carried out at 1100° C. for 30 s in an N 2 atmosphere.
  • cold rolling was carried out to a thickness of 0.23 mm, followed by decarburization annealing at 840° C.
  • Ti content in each steel sheet with the forsterite film was measured by the method specified in JIS G1223.
  • the results illustrated in FIG. 3 indicate that when the Ti content in the steel sheet with forsterite film is at least 0.0039% and at most 0.0200%, the steel sheet tends to belong to group A.
  • model transformer iron loss WT 17/50 transformer iron loss when excited at 50 Hz to 1.7 T
  • the building factor F17 of the model transformer was then calculated as the model transformer iron loss WT 17/50 divided by the sample iron loss W 17/50 (WT 17/50 /W 17/50 ).
  • the relationship between the building factor F17 and the Ti content in the steel sheet with forsterite film is illustrated in FIG. 4 .
  • the results illustrated in FIG. 4 indicate that when the Ti content in the steel sheet with forsterite film is less than 0.0050%, the building factor F17 is high even when the sheet belongs to group A.
  • the inventors found that the building factor is low and good when the Ti content in the steel sheet with forsterite film is from 0.0050% to 0.0200%. This essentially means that it is good for a certain amount of Ti to be present in the forsterite film.
  • the yoke and legs of the transformer have a certain width, and therefore the magnetic path differs in distance between the inside and the outside, like a track in athletics. Therefore, during excitation, the magnetic flux tends to be biased toward the inner side where the magnetic path is short. Even when the entire steel sheet is excited to 1.7 T, the magnetic flux density on the inner side exceeds that. Therefore, it may be that the more favorable the high magnetic field properties, the better the transformer properties such as the building factor. When Co is solute in iron, it is expected that the saturation magnetic flux density of the iron increases and high magnetic field properties improve, and this may be why the building factor improved. However, through Experiments 1 and 2, there were two cases where the building factor was not good, even when Co was added.
  • the first case was when the ratio of the hysteresis loss Wh 17 to the iron loss W 17/50 when excited at 1.7 T, that is, R17, and the ratio of the hysteresis loss Wh 19 to the iron loss W 19/50 when excited at 1.9 T, that is, R19, did not satisfy the relationship 0.30 ⁇ R17 ⁇ R19. Detailed investigation revealed that R17 was less than 0.30 in the majority of cases. Hysteresis loss is highly correlated with B 8 and the same B 8 is not expected to vary significantly, and therefore the above is considered a case of extremely large eddy current loss.
  • the second case was when the Ti content in the steel sheet with forsterite film was less than 0.0050 mass % or more than 0.0200 mass %.
  • the presence of a certain amount of Ti in the forsterite film may improve film properties.
  • an increase in film tension may refine the magnetic domain and decrease eddy current losses.
  • the eddy current loss ratio is lowered, contrary to the case of R17 and R19 above, and therefore the building factor may be decreased.
  • JP 2021-509149 A A production technique for a grain-oriented electrical steel sheet containing Co is described in JP 2021-509149 A.
  • the literature mentions a technique to improve the magnetic properties of the electrical steel sheet itself, which is completely different from the present disclosure, which decreases the building factor by combination with a technology to include Ti in the forsterite film.
  • a grain-oriented electrical steel sheet comprising a base steel sheet containing Si: 1.50 mass % to 8.00 mass %, Mn: 0.02 mass % to 1.00 mass %, and Co: 0.005 mass % to 0.050 mass %, and a base film mainly composed of forsterite, formed on the surface of the base steel sheet, wherein
  • the base steel sheet further contains one or more selected from the group consisting of Sn: 0.500 mass % or less, Cr: 0.500 mass % or less, Cu: 0.50 mass % or less, Ni: 0.50 mass % or less, Bi: 0.500 mass % or less, P: 0.500 mass % or less, Sb: 0.500 mass % or less, Mo: 0.500 mass % or less, B: 25.0 mass ppm or less, Nb: 0.020 mass % or less, V: 0.020 mass % or less, As: 0.0200 mass % or less, Zn: 0.020 mass % or less, Pb: 0.0100 mass % or less, W: 0.0100 mass % or less, Ga: 0.0050 mass % or less, and Ge: 0.0050 mass % or less.
  • a grain-oriented electrical steel sheet having magnetic properties that can sufficiently decrease the building factor can be provided.
  • FIG. 1 is a graph illustrating a relationship between Co content of base steel sheets and building factor F17, with respect to Experiment 1;
  • FIG. 2 is a graph illustrating the relationship between Co content of base steel sheets and building factor F17 (where only group A is extracted), with respect to Experiment 1;
  • FIG. 3 is a graph illustrating a relationship between Ti content of steel sheets with forsterite film and belonging to group A or group B, with respect to Experiment 2;
  • FIG. 4 is a graph illustrating a relationship between Ti content of steel sheets with forsterite film and building factor F17, with respect to Experiment 2.
  • Si is an element necessary for increasing the specific resistance of steel and decreasing iron loss. Further, Si is an element necessary for forming forsterite film in the steel sheet according to the present disclosure. However, Si content of less than 1.50% is ineffective, and the Si content exceeding 8.00% degrades steel workability and makes rolling difficult. Accordingly, the Si content is limited to 1.50% to 8.00%.
  • the Si content is preferably 2.50% or more.
  • the Si content is preferably 4.50% or less.
  • Mn is an element necessary for good hot workability. However, Mn content of less than 0.02% is ineffective, and the Mn content exceeding 1.00% decreases product sheet magnetic flux density. The Mn content is therefore from 0.02% to 1.00%. The Mn content is preferably 0.04% or more. The Mn content is preferably 0.20% or less.
  • Co content be in the range from 0.005% to 0.050%.
  • the Co content is preferably 0.006% or more.
  • the Co content is more preferably 0.008% or more.
  • the Co content is preferably 0.020% or less.
  • the Co content is more preferably 0.015% or less.
  • the base steel sheet of the grain-oriented electrical steel sheet may contain C (for example, 0.020% to 0.100%), may contain Al (for example, 0.002% to 0.040%), and may contain N (for example, 0.002% to 0.015%). Further, the base steel sheet may optionally contain S (for example, 0.020% or less) and/or Se (for example, 0.040% or less). In addition to the above components, the base steel sheet of the grain-oriented electrical steel sheet may contain the components (elements) described below as required.
  • the base steel sheet may contain one or more selected from the group consisting of Sn: (more than 0%) 0.500% or less, Cr: (more than 0%) 0.500% or less, Cu: (more than 0%) 0.50% or less, Ni: (more than 0%) 0.50% or less, Bi: (more than 0%) 0.500% or less, P: (more than 0%) 0.500% or less, Sb (more than 0%) 0.500% or less, Mo: (more than 0%) 0.500% or less, B: (more than 0 ppm) 25.0 ppm or less, Nb: (more than 0%) 0.020% or less, V: (more than 0%) 0.020% or less, As: (more than 0%) 0.0200% or less, Zn: (more than 0%) 0.020% or less, Pb: (more than 0%) 0.0100% or less, W: (more than 0%) 0.0100% or less, Ga: (more than 0%) 0.500% or less, Cr:
  • each of the above elements may be contained in the base steel sheet in a range up to the upper limit described above to further improve magnetic properties.
  • the amount of each element added (content) exceeds the above upper limit, the development of secondary recrystallized grains may be suppressed and magnetic properties may deteriorate.
  • each element is preferably contained in the following range.
  • Sn 0.005% or more, Cr: 0.005% or more, Cu: 0.01% or more, Ni: 0.01% or more, Bi: 0.005% or more, P: 0.005% or more, Sb: 0.005% or more, Mo: 0.005% or more, B: 0.1 ppm or more, Nb: 0.001% or more, V: 0.001% or more, As: 0.0010% or more, Zn: 0.001% or more, Pb: 0.0001% or more, W: 0.0010% or more, Ga: 0.0001% or more, and Ge: 0.0001% or more.
  • the balance other than the components (elements) mentioned above is Fe and inevitable impurity.
  • the chemical composition described above is the chemical composition in the base steel sheet, that is, without considering the base film, which is mainly composed of forsterite.
  • Ti content in the steel sheet with the base film mainly composed of forsterite that is, the Ti content in the base steel sheet and the base film as a whole, is limited to 0.0050% to 0.0200% for the reasons mentioned above.
  • the Ti content in the base steel sheet and the base film as a whole is preferably 0.0060% or more.
  • the Ti content is preferably 0.0150% or less.
  • the term “mainly composed” with respect to the base film refers to the component having the greatest mass among the components of the base film.
  • the Ti content in the base steel sheet is preferably 0.0030% or less.
  • the Ti content in the base steel sheet is 0.0030% or less, significant degradation of iron loss due to the formation of Ti precipitates in steel can be suppressed.
  • the Ti content in the steel sheet with the base film is 0.0050% or more. This is because, as mentioned above, a certain amount of Ti in the forsterite film may improve film properties and decrease eddy current loss, but when the Ti content is less than 0.0050%, the effect is estimated to be poor.
  • the hysteresis loss can be calculated by multiplying the energy loss of the iron core in one cycle of the hysteresis loop by 50, which is the excitation frequency.
  • the following describes a method of producing the grain-oriented electrical steel sheet according to the present disclosure.
  • the method of production may use a typical method for producing an electrical steel sheet.
  • molten steel prepared to have defined components may be made into a slab by typical ingot casting or continuous casting, or made into a thin slab or thinner cast steel having a thickness of 100 mm or less by direct casting.
  • Molten steel may be produced by either a blast furnace or an electric furnace steelmaking process.
  • the various components that may be contained in the base steel sheet are difficult to add during the process, and therefore adding them at the molten steel stage is preferred.
  • the slab may be heated and hot rolled by a typical method or hot rolled directly after casting without heating.
  • a chemical composition containing a small amount of inhibitor components does not require high-temperature annealing for dissolving the inhibitor, and therefore a low temperature of 1300° C. or less is effective for cost-reduction purposes.
  • the temperature is preferably 1250° C. or less.
  • hot-rolled sheet annealing may be carried out as required.
  • the temperature of hot-rolled sheet annealing is preferably about 950° C. to 1150° C. When the temperature is 950° C. or more, residual un-recrystallized portions can be sufficiently suppressed, and when the temperature is 1150° C. or less, excessive coarsening of grain size after annealing can be suppressed and the subsequent primary recrystallized texture can be made more favorable.
  • the temperature of hot-rolled sheet annealing is preferably 1000° C. or more.
  • the temperature of hot-rolled sheet annealing is preferably 1100° C. or less.
  • the steel sheet after the hot rolling or hot-rolled sheet annealing is subjected to cold rolling once, or twice or more with intermediate annealing carried out therebetween, to obtain a cold-rolled sheet having a final sheet thickness.
  • the annealing temperature for intermediate annealing is preferably in a range from 900° C. to 1200° C.
  • the temperature is 900° C. or more, the recrystallized grain becoming too fine after intermediate annealing can be well suppressed, and further, a decrease in magnetic properties of the product sheet due to a decrease in Goss nuclei in the primary recrystallized texture can be well suppressed.
  • the temperature is 1200° C. or less, as with hot-rolled sheet annealing, excessive coarsening of crystal grains can be suppressed and the primary recrystallized texture of the uniformly-sized grains can be made better.
  • the cold-rolled sheet having a final sheet thickness is then subjected to primary recrystallization annealing that also serves as decarburization annealing.
  • the annealing temperature for this primary recrystallization annealing is, when accompanied by decarburization annealing and from the viewpoint of allowing the decarburization reaction to proceed rapidly, preferably in a range from 800° C. to 900° C., and the atmosphere is preferably a wet atmosphere.
  • an annealing separator mainly composed of MgO is applied, followed by purification annealing to develop a secondary recrystallized texture and form a forsterite film.
  • mainly composed of MgO means that MgO content is 75 mass % or more.
  • Ti may be made to be present in the forsterite film in other ways.
  • secondary recrystallization annealing (purification annealing) is carried out.
  • This purification annealing is preferably carried out at 800° C. or more for the development of secondary recrystallization, and from the purification point of view, the temperature is preferably raised to a holding temperature of 1100° C. or more.
  • the holding temperature is more preferably 1180° C. or more.
  • the hold time is preferably at least 3 h and at most 15 h.
  • water washing, brushing, or pickling is preferably carried out to remove adhered annealing separator.
  • an N 2 atmosphere up to a first intermediate temperature for example, a temperature selected from the range from 600° C. to 800° C.
  • a mixed N 2 and H 2 atmosphere from the first intermediate temperature to a second intermediate temperature for example, a temperature selected from the range from 1050° C. to 1150° C.
  • an H 2 atmosphere from the second intermediate temperature to the holding temperature for example, a temperature selected from the range from 1050° C. to 1150° C.
  • flattening annealing is carried out for shape adjustment, which is effective for iron loss reduction.
  • applying an insulating coating to the steel sheet surface before or after the flattening annealing is effective for reducing iron loss.
  • the insulating coating a film that can impart tension to the steel sheet to reduce iron loss is preferable.
  • a method of tension film coating application through a binder, or coating by depositing an inorganic substance onto the steel sheet surface layer by physical vapor deposition or chemical vapor deposition is preferable, as these methods have excellent coating adhesion and a considerable iron loss reduction effect.
  • Steel slab B-C 0.072%, Si: 3.51%, Mn: 0.07%, Al: 0.0080%, N: 0.0047%, Co: 0.011%, Mo: 0.025%, Ti: 0.0025%, with the balance being Fe and inevitable impurity.
  • Each of the steel slabs A to D described above was produced by continuous casting, and after slab heating to soak at 1200° C. for 40 min, the slabs were hot rolled to a thickness of 2.2 mm. Hot-rolled sheet annealing was then carried out at 1000° C. for 60 s in an N 2 atmosphere. Next, cold rolling was carried out to a thickness of 0.23 mm, followed by decarburization annealing at 850° C. for 90 s in a wet atmosphere of 60% H 2 —40% N 2 with a dew point of 60° C.
  • an annealing separator consisting mainly of MgO (MgO: 97 mass %) was applied, and purification annealing was carried out by holding at 1100° C. for 25 h, then holding at 1200° C. for 10 h.
  • an N 2 atmosphere was used from room temperature to 700° C.
  • an atmosphere in which the mixing ratio of N 2 and H 2 was varied was used from 700° C. to 1100° C.
  • an H 2 atmosphere was used from 1100° C. (start of holding) to 1200° C. (end of holding).
  • an Ar atmosphere was used during cooling.
  • the Ti content (the total Ti content of the base steel sheet and the base film) of the obtained samples was measured according to the method specified in JIS G1223. The results are listed in Table 1.
  • a three-phase three-leg model transformer simulating a transformer was fabricated having an external shape of 500 mm square and a sheet width of 100 mm for each leg and each yoke, and model transformer iron loss WT 17/50 (transformer iron loss when excited at 50 Hz to 1.7 T) was measured.
  • the number of stacked sheets of each sample was 50, with two sheets stacked alternately.
  • the building factor F17 of the model transformer was then calculated as the model transformer iron loss WT 17/50 divided by the sample iron loss W 17/50 (WT 17/50 /W 17/50 ). The results are listed in Table 1.
  • an annealing separator consisting mainly of MgO (MgO: 88 mass %) was applied.
  • MgO MgO: 88 mass %
  • TiO 2 powder was put into warm water at 50° C. and stirred for 24 h, and 5 parts by mass of the resulting superhydrated TiO 2 was added to the MgO powder.
  • purification annealing was carried out by holding at 1200° C. for 10 h. At this time, the heating rate to 1200° C. was 15° C./h. Further, during the heating process, an N 2 atmosphere was used from room temperature to 700° C., an atmosphere in which the mixing ratio of N 2 and H 2 was varied was used from 700° C. to 1100° C., and an H 2 atmosphere was used from 1100° C. to 1200° C. Further, an H 2 atmosphere was used during the hold time, and an Ar atmosphere was used during cooling.
  • the Ti content (the total Ti content of the base steel sheet and the base film) of the obtained samples was measured according to the method specified in JIS G1223. The measurement results are listed in Table 3.
  • a three-phase three-leg model transformer simulating a transformer was fabricated having an external shape of 500 mm square and a sheet width of 100 mm for each leg and each yoke, and model transformer iron loss WT 17/50 (transformer iron loss when excited at 50 Hz to 1.7 T) was measured.
  • the number of stacked sheets of each sample was 50, with two sheets stacked alternately.
  • the building factor F17 of the model transformer was then calculated as the model transformer iron loss WT 17/50 divided by the sample iron loss W 17/50 (WT 17/50 /W 17/50 ). The results are listed in Table 3.

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