WO2013046716A1 - 方向性電磁鋼板およびその製造方法 - Google Patents
方向性電磁鋼板およびその製造方法 Download PDFInfo
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- WO2013046716A1 WO2013046716A1 PCT/JP2012/006244 JP2012006244W WO2013046716A1 WO 2013046716 A1 WO2013046716 A1 WO 2013046716A1 JP 2012006244 W JP2012006244 W JP 2012006244W WO 2013046716 A1 WO2013046716 A1 WO 2013046716A1
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
- C21D8/1277—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties involving a particular surface treatment
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/34—Methods of heating
- C21D1/38—Heating by cathodic discharges
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
- C21D8/1277—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties involving a particular surface treatment
- C21D8/1283—Application of a separating or insulating coating
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/001—Ferrous alloys, e.g. steel alloys containing N
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/002—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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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/08—Ferrous alloys, e.g. steel alloys containing nickel
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/60—Ferrous alloys, e.g. steel alloys containing lead, selenium, tellurium, or antimony, or more than 0.04% by weight of sulfur
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- 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
- C23C30/00—Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process
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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
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/16—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of sheets
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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
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/16—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of sheets
- H01F1/18—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of sheets with insulating coating
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D2201/00—Treatment for obtaining particular effects
- C21D2201/05—Grain orientation
Definitions
- the present invention relates to a grain-oriented electrical steel sheet that is suitable for use in applications such as transformer iron cores and has excellent iron loss characteristics and no deterioration in corrosion resistance, and a method for producing the same.
- Patent Document 1 a manufacturing method of the grain-oriented electrical steel sheet having a magnetic flux density B 8 of greater than 1.97T It is shown.
- the film tension is applied after cooling to room temperature by forming a film on a steel sheet expanded at high temperature using the difference in thermal expansion between the film and the base iron.
- the technology to increase the tendency is saturated.
- Patent Document 2 since the strain to be applied is in the vicinity of the elastic region and the tension is applied only to the surface layer of the ground iron, the effect of reducing iron loss is obtained. There is a problem of being small.
- Patent Document 3 discloses a method for producing an electrical steel sheet having an iron loss with W 17/50 being less than 0.8 W / kg by electron beam irradiation.
- Patent Document 4 discloses a method for reducing iron loss by applying laser irradiation to an electromagnetic steel sheet.
- Patent Document 6 and Patent Document 7 there is a technique of reducing the laser power density by changing the beam shape and suppressing damage to the film due to irradiation.
- the laser is spread in the irradiation direction and the irradiation area is increased, if the irradiation speed is high, the heat in the vicinity of the irradiation part does not diffuse sufficiently and accumulates to increase the temperature. It will be damaged.
- an iron loss reduction effect for example, 15% or more
- the irradiated surface may be coated again to ensure corrosion resistance.
- re-coating after irradiation not only increases the cost of the product, but also increases the thickness of the sheet and reduces the space factor when the iron core is used.
- Patent Document 8 the irradiation beam is made into a sheet shape
- Patent Document 9 the number of apertures of the beam is set to one and the filament shape is made into a ribbon type.
- the methods for suppressing film damage due to irradiation are respectively shown.
- Patent Document 10 discloses a steel sheet that is free from damage to the coating by press-fitting the coating into the ground iron with an electron beam having a high acceleration voltage and a low current.
- the method of making the electron beam into a sheet type has problems that the output inside the sheet-shaped irradiation surface becomes non-uniform and it takes time to adjust the optical system.
- film damage due to irradiation appears when the filament is ribbon-shaped or the aperture is made one stage.
- the method disclosed in Patent Document 10 not only requires strain relief annealing after electron beam irradiation, but is also not sufficient in reducing iron loss.
- the present invention has been developed in view of the above-described present situation, and provides a grain-oriented electrical steel sheet suitable for use in applications such as a transformer core and having low iron loss and no deterioration in corrosion resistance, and a method for producing the same. With the goal.
- the iron loss after the electron beam irradiation is the irradiation energy per unit area (for example, when the electron beam is irradiated in the form of dots, the total of the irradiation energy given by the irradiation points included in a certain area is the area of the area. It was found that it strongly depends on what is divided by.
- Z is the ⁇ 0.35 power of the irradiation frequency (kHz).
- the irradiation energy of the electron beam is in the range of 1.0 Z to 3.5 ZJ per unit area: 1 cm 2 .
- the irradiation energy of the electron beam is set to a range of 105 ZJ or less per unit length: 1 m.
- the present invention is based on the above-described knowledge, and the gist configuration is as follows.
- Thickness t (mm) grain-oriented electrical steel sheet that has been subjected to electron beam irradiation, and rusted on the surface of the steel sheet after a wet test for 48 hours in an atmosphere of temperature: 50 ° C and humidity: 98%
- the iron loss W 17/50 after the electron beam irradiation is reduced by ( ⁇ 500 t 2 +200 t ⁇ 6.5)% or more compared to the iron loss W 17/50 before the electron beam irradiation, and (5t 2 ⁇ 2t + 1.065)
- the irradiation energy per unit area of the electron beam: 1 cm 2 is 1.0 Z to 3.5 ZJ
- the irradiation length of the electron beam unit irradiation is 1 m. 105ZJ or less
- the electron beam irradiation not only significantly improves the iron loss of the grain-oriented electrical steel sheet, but also can suppress the destruction of the coating film on the irradiated portion, thereby effectively reducing the corrosion resistance. Can be prevented.
- the coating re-coating process after electron beam irradiation can be omitted, not only the cost of the product is reduced, but the thickness of the coating does not increase. Improvement is possible.
- the component composition of the slab for grain-oriented electrical steel sheet may be a component composition that causes secondary recrystallization.
- an inhibitor for example, when using an AlN-based inhibitor, Al and N, and when using an MnS / MnSe-based inhibitor, an appropriate amount of Mn and Se and / or S should be contained. Good. Of course, both inhibitors may be used in combination.
- the preferred contents of Al, N, S and Se are Al: 0.01 to 0.065 mass%, N: 0.005 to 0.012 mass%, S: 0.005 to 0.03 mass%, and Se: 0.005 to 0.03 mass%, respectively. .
- the present invention can also be applied to grain-oriented electrical steel sheets in which the contents of Al, N, S, and Se are limited and no inhibitor is used.
- the amounts of Al, N, S and Se are preferably suppressed to Al: 100 mass ppm or less, N: 50 mass ppm or less, S: 50 mass ppm or less, and Se: 50 mass ppm or less, respectively.
- C 0.08 mass% or less C is added to improve the hot-rolled sheet structure, but in order to reduce C to 50 mass ppm or less where magnetic aging does not occur during the manufacturing process, 0.08 mass% or less It is preferable to do.
- the lower limit since a secondary recrystallization is possible even for a material not containing C, it is not particularly necessary to provide it.
- Si 2.0-8.0% by mass
- Si is an element effective for increasing the electrical resistance of steel and improving iron loss.
- the content is preferably set to 2.0% by mass or more.
- the Si content is preferably in the range of 2.0 to 8.0% by mass.
- Mn 0.005 to 1.0 mass%
- Mn is an element necessary for improving the hot workability. However, if the content is less than 0.005% by mass, the effect of addition is poor, whereas if it exceeds 1.0% by mass, the magnetic flux density of the product plate decreases.
- the Mn content is preferably in the range of 0.005 to 1.0 mass%.
- Ni 0.03-1.50 mass%
- Sn 0.01-1.50 mass%
- Sb 0.005-1.50 mass%
- Cu 0.03-3.0 mass%
- P 0.03-0.50 mass%
- Mo 0.005-0.10 mass%
- Cr At least one Ni selected from 0.03 to 1.50% by mass is an element useful for improving the magnetic properties by improving the hot rolled sheet structure.
- the content is less than 0.03% by mass, the effect of improving the magnetic properties is small.
- the amount of Ni is preferably in the range of 0.03 to 1.50% by mass.
- Sn, Sb, Cu, P, Mo and Cr are elements useful for improving the magnetic properties, respectively, but if any of them is less than the lower limit of each component described above, the effect of improving the magnetic properties is small, If the upper limit amount of each component described above is exceeded, the development of secondary recrystallized grains is hindered.
- the balance other than the above components is inevitable impurities and Fe mixed in the manufacturing process.
- the slab having the above-described component composition is heated and subjected to hot rolling according to a conventional method, but may be immediately hot rolled after casting without being heated.
- hot rolling may be performed, or the hot rolling may be omitted and the process may proceed as it is.
- hot-rolled sheet annealing is performed as necessary.
- the hot rolled sheet annealing temperature is preferably in the range of 800 to 1100 ° C.
- the hot-rolled sheet annealing temperature is less than 800 ° C, the band structure in hot rolling remains, making it difficult to achieve a sized primary recrystallization structure and inhibiting the development of secondary recrystallization.
- recrystallization annealing is performed and an annealing separator is applied. After applying the annealing separator, a final finish annealing is performed for the purpose of secondary recrystallization and forsterite film formation.
- an insulating coating is applied to the steel sheet surface before or after planarization annealing.
- this insulating coating means a coating (hereinafter referred to as tension coating) that can apply tension to a steel sheet in order to reduce iron loss.
- tension coating any known tension coating used for grain-oriented electrical steel sheets can be equally applied to the present invention, but those composed of colloidal silica and phosphate are particularly preferable.
- inorganic coatings containing silica, ceramic coatings by physical vapor deposition, chemical vapor deposition, and the like are also included.
- the above-described grain-oriented electrical steel sheet after tension coating is subjected to magnetic domain fragmentation treatment by irradiating the surface of the steel sheet with an electron beam under the following conditions.
- a reduction effect can be sufficiently exhibited, and damage to the film can be suppressed.
- an electron beam irradiation method will be described.
- Accelerating voltage 40-300kV
- a higher acceleration voltage is better.
- Electron beams generated by high acceleration voltages tend to penetrate materials, especially those composed of light elements. In general, forsterite coatings and tension coatings are composed of light elements. Therefore, if the acceleration voltage is high, the electron beam is easily transmitted and the coating is not easily damaged. Further, it is preferable that the voltage exceeds 40 kV because the irradiation beam current required for obtaining the same output is small and the beam diameter can be reduced. However, if it exceeds 300 kV, the irradiation beam current becomes excessively low, which may make it difficult to make minute adjustments.
- Irradiation diameter 350 ⁇ m or less If the irradiation diameter is larger than 350 ⁇ m, the heat-affected zone is enlarged and the iron loss (hysteresis loss) may be deteriorated.
- the measurement was defined by the half width of a current (or voltage) curve obtained by a known slit method.
- the lower limit of the irradiation diameter is not limited, but if it is excessively small, the beam energy density becomes excessively high and film damage due to irradiation is likely to be generated. Therefore, it is preferably about 100 ⁇ m or more.
- the electron beam irradiation pattern is not limited to a straight line but is irradiated from the width end of the steel sheet to the other width end while having a regular pattern such as a waveform. be able to. Further, a plurality of electron guns may be used to divide the irradiation area with one unit. Irradiation with respect to the width direction of the steel sheet is performed using a deflection coil, and is repeated with an irradiation time of s 1 at regular intervals: d (mm) along the irradiation position. In the present invention, this irradiation point is called a dot.
- the predetermined interval d is within a predetermined range.
- This interval d is referred to as dot pitch in the present invention.
- the reciprocal of s 1 can be regarded as the irradiation frequency.
- the irradiation from the width end to the width end is repeated at a certain interval in the direction intersecting the rolling direction of the irradiated material. This interval is hereinafter referred to as a line interval.
- the irradiation direction is preferably set to an angle of about ⁇ 30 degrees with respect to the direction perpendicular to the rolling direction of the steel sheet.
- Irradiation time per dot (reciprocal of irradiation frequency) s 1 : 0.003 to 0.1 ms (3 to 100 ⁇ s) If the irradiation time s 1 is shorter than 0.003 ms, there is a possibility that the iron loss cannot be improved because sufficient heat influence cannot be exerted on the ground iron. On the other hand, if it is longer than 0.1 ms, the irradiated heat diffuses into the steel during the irradiation time. For this reason, even if the irradiation energy per dot represented by V ⁇ I ⁇ s 1 is constant, the maximum temperature reached by the irradiated portion tends to be low, and there is a possibility that the iron loss is deteriorated. Therefore, the irradiation time s 1 is preferably in the range of 0.003 to 0.1 ms. V is an acceleration voltage and I is a beam current.
- the dot pitch in the present invention is preferably in the range of 0.01 to 0.5 mm.
- Line spacing 1-15mm If the line spacing is narrower than 1 mm, the heat-affected zone is expanded and the iron loss (hysteresis loss) may be deteriorated. On the other hand, when the width is larger than 15 mm, the magnetic domain is not sufficiently subdivided and the iron loss tends not to be improved. Accordingly, the line spacing in the present invention is preferably in the range of 1 to 15 mm.
- Processing chamber pressure 3 Pa or less If the pressure in the processing chamber is higher than 3 Pa, electrons generated from the electron gun are scattered and the energy of the electrons that have a thermal effect on the ground iron is reduced. The iron loss may not improve. There is no particular lower limit, and the lower the processing chamber pressure, the better. In the present invention, it is needless to say that the convergence current is adjusted in advance so that the beam in the width direction becomes uniform when irradiating with deflection in the width direction. For example, there is no problem even if the dynamic focus function (see Patent Document 11) is applied.
- Irradiation energy per unit irradiation length (1 m) of electron beam 105 ZJ or less
- Z is a value represented by s 1 0.35 or ⁇ 0.35 to the irradiation frequency (kHz).
- kHz irradiation frequency
- the appropriate condition is a certain value (105ZJ / m) or less.
- the lower limit is not particularly limited as long as the magnetic domain fragmentation effect can be obtained, but is preferably about 60 ZJ / m.
- Z in the present invention is derived based on experiments conducted by the inventors themselves. Specifically, ten 0.23 mm thick materials with a tension coating prepared under the same conditions as those in Examples described later were prepared, and electron beam irradiation was performed at the frequencies shown in Table 1. Subsequently, the minimum irradiation energy was obtained when at least one sample in which the number of rust generation after the wet test after exposure to a wet environment of temperature: 50 ° C. and humidity: 98% for 48 hours appeared to be zero appeared. The results are also shown in Table 1. Here, the result of the maximum irradiation energy is graphed and shown in FIG. As shown in the figure, the upper limit (105Z J / m) is derived by performing curve fitting by the least square method.
- the energy per unit length is the region when the length of the electron beam irradiated linearly or curvedly from the width end of the steel sheet to the other width end is L (m). Is the value obtained by dividing the total energy irradiated to L by L.
- FIG. 2 shows the effect of irradiation energy per unit length on corrosion resistance after irradiation with an electron beam at a frequency of 100 kHz.
- Electron beam irradiation conditions were as follows: acceleration voltage: 60kV, dot pitch: 0.35mm, line spacing: 5mm, shape 5cm x 10cm, plate thickness: 0.23mm, temperature: 50 ° C-humidity: 98% wet
- acceleration voltage 60kV
- dot pitch 0.35mm
- line spacing 5mm
- shape 5cm x 10cm plate thickness: 0.23mm
- temperature 50 ° C-humidity: 98% wet
- the amount of rust generated on the surface irradiated with the electron beam was visually measured and evaluated as the number of points generated per unit area. As a result, it was confirmed that the amount of rust generated can be suppressed by reducing the irradiation energy per unit length.
- the data width in the vertical axis direction is the maximum value and the minimum value in the measurement with N: 10.
- Irradiation energy per unit area (1cm 2 ) of irradiated material 1.0Z to 3.5ZJ
- Z Is useful Table 2 summarizes the minimum and maximum irradiation energy at which the iron loss reduction rate is 13% or more (iron loss reduction amount is 0.13 W / kg or more).
- the irradiation energy of the electron beam for optimizing the iron loss is Z to 3.5 Z per unit area: 1 cm 2 .
- the iron loss reduction rate ⁇ W (%) at the iron loss W 17/50 is 13% which is higher than 12% described in Patent Document 7 (in the steel plate used in this experiment, In order to achieve a loss reduction amount of 0.13 W / kg or more), an irradiation energy range per unit area was set, and the proportionality coefficient was determined as being proportional to Z.
- the samples used to determine the results of Table 2 the magnetic flux density B 8 before irradiation was 1.90 ⁇ 1.92 T.
- FIG. 3 shows the relationship between the amount of change in iron loss W 17/50 due to electron beam irradiation at a frequency of 100 kHz (iron loss after irradiation ⁇ iron loss before irradiation) and irradiation energy per unit area. From the figure, it can be confirmed that the iron loss is reduced when the irradiation energy of the electron beam is 1.0 Z to 3.5 Z (0.2 to 0.7) J / cm 2 .
- the amount of change in the iron loss W 17/50 is determined by an energy adjustment method such as an irradiation line interval, a dot pitch, and a beam current as shown in FIG.
- the irradiation energy per unit area can be arranged.
- the irradiation at this time is performed within the above-mentioned electron beam generation conditions.
- the irradiation energy per unit area as used in the field of this invention is the area of the sample used for a magnetic measurement, and is the value which remove
- the iron loss reduction rate ⁇ W (%) specified in this experiment is 13%, which is higher than 12% described in Patent Document 7 as described above when the plate thickness is 0.23 mm. That is all.
- the iron loss reduction rate is affected by the plate thickness: t (mm), but in FIG.
- the material used in this experiment has a pre-irradiation iron loss of 0.86 to 0.88 W / kg, so as to the absolute value of the reduction amount, a reduction of 13% corresponds to a reduction of 0.11 W / kg.
- the iron loss reduction amount is aligned in the above-mentioned narrow range, but in reality, the direction before the electron beam irradiation
- the iron loss of the electrical steel sheet is high-grade and is about 1.0 W / kg (when the thickness is 0.23 mm).
- the (-500t 2 + 200t-6.5) when performing% iron loss reducing iron loss of the present invention will become (5t 2 -2t + 1.065) W / kg in W 17/50 Therefore, the iron loss achieved in the present invention is limited to a range that is equal to or less than this value.
- those iron loss before irradiation is lower than 1.0 W / kg, if the iron loss after the electron beam irradiation (-500t 2 + 200t-6.5) % reduction, the iron loss (5t 2 -2t + 1.065) W Of course, it will be lower than / kg.
- the determination of film breakage is performed by performing a wet test, which is one of the corrosion resistance tests as described above, and quantifying the amount of rust that appears along the irradiated area. Specifically, whether or not rust occurs on the steel sheet surface, especially the heat-affected zone of the electron beam, after the specimen after electron beam irradiation is exposed to an environment of temperature: 50 ° C and humidity: 98% for 48 hours. judge. Whether or not rust has occurred is determined by the presence or absence of visual discoloration, and the amount is evaluated by the number of points generated per unit area. However, when the rust is more prominent and the rust at one place covers a wide area, the rust generation area ratio should be evaluated.
- a method for manufacturing a grain-oriented electrical steel sheet that is subjected to a magnetic domain refinement process using a conventionally known electron beam can be applied except for the steps and manufacturing conditions described above.
- Iron loss is 0.54 to 0.55 W / kg (plate thickness: 0.20 mm), 0.56 to 0.58 W / kg (plate thickness: 0.23 mm), 0.62 to 0.63 W / kg (plate) Thickness: 0.27 mm) and 0.72 to 0.73 W / kg (plate thickness: 0.30 mm).
- magnetic domain fragmentation treatment was performed to irradiate an electron beam under each irradiation condition shown in Table 4 (in the range of 0.001 to 0.08 ms in terms of s 1 ), and iron loss and temperature: 50 ° C.-humidity: 98% wetness
- Table 5 shows the measurement results.
- the iron loss reduction rate can be reduced by setting the electron beam irradiation conditions to 105 ZJ / m or less per unit length and 1.0 Z to 3.5 ZJ / cm 2 per unit area according to the present invention.
- a low iron loss grain oriented electrical steel sheet having ⁇ W of ( ⁇ 500 t 2 +200 t ⁇ 6.5)% or more and iron loss W 17/50 of (5t 2 ⁇ 2t + 1.065) W / kg or less was obtained. Furthermore, since rust did not occur after the wet test, it can be seen that the corrosion resistance was not deteriorated by the electron beam irradiation.
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Abstract
Description
ここに、磁束密度は、電磁鋼板の結晶方位をGoss方位へ集積させることにより向上させることができ、例えば特許文献1には、1.97Tを超える磁束密度B8を有する方向性電磁鋼板の製造方法が示されている。
例えば、特許文献3には、電子ビーム照射によってW17/50が0.8W/kgを下回る鉄損を有する電磁鋼板の製造方法が示されている。また、特許文献4には、電磁鋼板にレーザ照射を施すことによって、鉄損を低減する方法が示されている。
(1) 電子ビームの照射エネルギを、単位面積:1cm2当たり、1.0Z~3.5ZJの範囲とする。
(2) 電子ビームの照射エネルギを、単位長さ:1m当たり105ZJ以下の範囲とする。
1.電子ビーム照射が施され、被膜を有する板厚:t(mm)の方向性電磁鋼板であって、温度:50℃、湿度:98%の雰囲気中48時間保持する湿潤試験後に、鋼板表面に錆が発生せず、電子ビーム照射後の鉄損W17/50が、電子ビーム照射前の鉄損W17/50に比べて(-500t2+200t-6.5)%以上低減し、かつ(5t2-2t+1.065)W/kg以下であることを特徴とする方向性電磁鋼板。
はじめに、本発明に従う方向性電磁鋼板の製造条件に関して説明する。
本発明において、方向性電磁鋼板用スラブの成分組成は、二次再結晶が生じる成分組成であればよい。また、インヒビターを利用する場合、例えばAlN系インヒビターを利用する場合であればAlおよびNを、またMnS・MnSe系インヒビターを利用する場合であればMnとSeおよび/またはSを適量含有させればよい。勿論、両インヒビターを併用してもよい。この場合におけるAl、N、SおよびSeの好適含有量はそれぞれ、Al:0.01~0.065質量%、N:0.005~0.012質量%、S:0.005~0.03質量%、Se:0.005~0.03質量%である。
この場合には、Al、N、SおよびSe量はそれぞれ、Al:100質量ppm以下、N:50質量ppm以下、S:50質量ppm以下、Se:50質量ppm以下に抑制することが好ましい。
C:0.08質量%以下
Cは、熱延板組織の改善のために添加をするが、製造工程中に磁気時効の起こらない50質量ppm以下までCを低減するためには、0.08質量%以下とすることが好ましい。なお、下限に関しては、Cを含まない素材でも二次再結晶が可能であるので特に設ける必要はない。
Siは、鋼の電気抵抗を高め、鉄損を改善するのに有効な元素であるが、十分な鉄損低減効果を達成するためには、含有量を2.0質量%以上とすることが好ましい。一方、8.0質量%を超えると加工性が著しく低下し、また磁束密度も低下するため、Si量は2.0~8.0質量%の範囲とすることが好ましい。
Mnは、熱間加工性を良好にする上で必要な元素であるが、含有量が0.005質量%未満ではその添加効果に乏しく、一方1.0質量%を超えると製品板の磁束密度が低下するため、Mn量は0.005~1.0質量%の範囲とすることが好ましい。
Ni:0.03~1.50質量%、Sn:0.01~1.50質量%、Sb:0.005~1.50質量%、Cu:0.03~3.0質量%、P:0.03~0.50質量%、Mo:0.005~0.10質量%およびCr:0.03~1.50質量%のうちから選んだ少なくとも1種
Niは、熱延板組織を改善して磁気特性を向上させるために有用な元素である。しかしながら、含有量が0.03質量%未満では磁気特性の向上効果が小さく、一方1.50質量%を超えると二次再結晶が不安定になり磁気特性が劣化する。そのため、Ni量は0.03~1.50質量%の範囲とするのが好ましい。
なお、上記成分以外の残部は、製造工程において混入する不可避的不純物およびFeである。
さらに、必要に応じて熱延板焼鈍を施す。この時、ゴス組織を製品板において高度に発達させるためには、熱延板焼鈍温度として800~1100℃の範囲が好適である。熱延板焼鈍温度が800℃未満であると、熱間圧延でのバンド組織が残留し、整粒した一次再結晶組織を実現することが困難になり、二次再結晶の発達が阻害される。一方、熱延板焼鈍温度が1100℃を超えると、熱延板焼鈍後の粒径が粗大化しすぎるために、整粒した一次再結晶組織の実現が極めて困難となる。
まず、電子ビームの発生条件について説明する。
加速電圧:40~300kV
加速電圧は、高いほうがよい。高い加速電圧によって生成された電子ビームは、物質、特に軽元素から構成されるものを透過する傾向がある。一般にフォルステライト被膜や張力コーティングは軽元素から構成されるため、加速電圧が高ければ電子ビームを透過しやすくなり、被膜が損傷されにくくなる。また、40kVを超えて高いほど、同一出力を得るために必要な照射ビーム電流が少なく、ビーム径を絞ることができるため好ましい。しかしながら、300kVを超えると照射ビーム電流が過度に低くなるため、その微小な調整が困難となるおそれが生じる。
照射径が350μmを超えて太いと、熱影響域が拡大し、鉄損(ヒステリシス損)が劣化するおそれがあるので、350μm以下とすることが好ましい。測定は、公知のスリット法で得られる電流(あるいは電圧)曲線の半値幅で規定した。なお、照射径の下限に限定はないが、過度に小さいと、ビームエネルギ密度が過度に高くなり、照射による被膜損傷が生成しやすくなるため、100μm程度以上とするのが好ましい。
本発明では、電子ビームの照射パタンは、直線に限らず、波形などのように規則的なパタンを有しながら鋼板の幅端部から、もう一方の幅端部へ照射させることができる。また、電子銃を複数台使用して、1台での照射域を分割しても良い。
鋼板の幅方向に対する照射は、偏向コイルを用いて行い、照射位置に沿って、一定間隔:d(mm)毎に、照射時間をs1として、繰り返す。本発明では、この照射点をドットと言う。またその際、一定間隔:d(mm)を、所定の範囲とすることが好ましい。この間隔:dを、本発明ではドットピッチと言う。なお、本発明においては、電子ビームが間隔:dを移動する時間が極めて短いので、s1の逆数を照射周波数とみなすことができる。
さらに、上記の幅端から幅端へ向かう照射を、被照射材の圧延方向と交わる向きに一定の間隔をおいて繰り返すが、この間隔を、以下線間隔と呼ぶ。また、照射方向は、鋼板の圧延方向に直角な方向に対し、±30度程度の角度とするのが好ましい。
照射時間s1が0.003msより短いと、地鉄に十分な熱影響をおよぼすことができずに鉄損が改善しないおそれがある。一方、0.1msより長いと、照射時間中に、照射した熱が鋼中などに拡散してしまう。そのため、V×I×s1で表される1ドット当たりの照射エネルギが一定であっても、照射部の最高到達温度が低くなる傾向になるので、鉄損が劣化してしまうおそれが生じる。従って、照射時間s1は0.003~0.1msの範囲が好ましい。なお、Vは加速電圧、Iはビーム電流である。
ドットピッチが0.5mmより広いと、地鉄に熱影響がおよばない部分が生じて、十分に磁区が細分化されず、鉄損が改善しないおそれがある。一方、0.01mmより狭いと照射速度が過度に低下し、照射効率が落ちる。従って、本発明におけるドットピッチは、0.01~0.5mmの範囲とするのが好ましい。
線間隔が1mmより狭いと、熱影響域が拡大し、鉄損(ヒステリシス損)が劣化するおそれがある。一方、15mmより広いと、十分に磁区細分化されず、鉄損が改善しない傾向にある。従って、本発明における線間隔は、1~15mmの範囲とするのが好ましい。
加工室の圧力が3Paより高いと、電子銃から発生した電子が散乱され、地鉄に熱影響を与える電子のエネルギが減少するため、十分に磁区細分化が成されず、鉄損が改善しないおそれがある。なお、下限に特に定めはなく加工室の圧力は低いほど良い。
なお、本発明では、収束電流に関し、幅方向に偏向して照射する際、幅方向のビームが均一になるように、事前に収束電流を調整することは言うまでもない。例えば、ダイナミックフォーカス機能(特許文献11参照)を適用してもなんら問題はない。
本発明において、Zは、s1 0.35または照射周波数(kHz)の-0.35乗で表される値である。一般に、鋼板の幅方向における単位長さ当たりの照射エネルギが高いほど、磁区細分化が進み渦電流損が下がるが、過度にエネルギを照射した場合には、ヒステリシス損が増大するだけでなく、ビーム照射部が過度に高温化し、被膜が損傷する。そのため、以下に説明するように、ある値(105ZJ/m)以下が適正条件となる。なお、下限は、磁区細分化効果が得られれば、特に制限はないが、60ZJ/m程度が好ましい。
具体的には、後述する実施例と同様の条件で作製した張力コーティング付きの0.23mm厚材を10枚準備し、表1に示す周波数で電子ビーム照射を行った。ついで、温度:50℃-湿度:98%の湿潤環境に48h暴露した後の湿潤試験後の錆発生点数が目視確認で0になる試料が1枚でも現れたときの最小照射エネルギを求めた。その結果を、表1に併記する。
ここで、この最大照射エネルギの結果をグラフ化し、図1に示す。同図に示したように、最小二乗法によりカーブフィッティングを行うことで、上記上限値(105Z J/m)を導出したのである。
その結果、単位長さ当たりの照射エネルギを低減することによって、錆の発生量を抑制できることが確認できた。なお、図中、縦軸方向のデータ幅は、N:10とした測定における最大値と最小値である。ここに、単位長さ当たりの照射エネルギを105Z=21J/m以下とすることによって、錆の発生が効果的に抑制されていることが分かる。
照射の周波数が鉄損に与える影響を考えた場合、やはり、前述したように照射部の最高到達温度などに影響すると考えられるから、鉄損を適正化する照射エネルギを導出する際にも、Zは有用である。
表2に、鉄損低減率が13%以上(鉄損低減量が0.13W/kg以上)になる最小および最大の照射エネルギをまとめて記載する。その結果を考察すると、鉄損を適正化する電子ビームの照射エネルギは、単位面積:1cm2当たりZ~3.5Zであることが導出される。
以下、本発明に従う方向性電磁鋼板の特徴を説明する。
照射後の鉄損W17/50:(5t2-2t+1.065)W/kg以下
従来の技術でも、鉄損低減効果が弱い条件で電子ビームを照射すれば、被膜損傷が生じないことから、鉄損低減効果抜きに、本発明を議論することはできない。
前述したように、本実験の規定する鉄損低減率ΔW(%)は、板厚:0.23mmの場合、前述のように、特許文献7に記載される12%よりも高い値である13%以上とした。ここで、鉄損低減率は、板厚:t(mm)の影響を受けるが、非特許文献2のFig.4では、鉄損低減率はΔW=-500t2+200t-α(α:7.5~9)となっていることから、より高い鉄損低減率である(-500t2+200t-6.5)%以上を本発明で規定する鉄損低減率とした。本実験に用いた材料は、照射前鉄損が、0.86~0.88W/kgであるので、低減量の絶対値としては、13%の低減が0.11W/kgの低減に相当する。
この最終仕上げ焼鈍では、700℃以上の温度領域の冷却過程における平均冷却速度を変化させた。ついで、50%のコロイダルシリカとリン酸マグネシウムからなる張力コーティングを付与し、鉄損を測定した。鉄損は、渦電流損(1.7T、50Hz)が0.54~0.55W/kg(板厚:0.20mm)、0.56~0.58W/kg(板厚:0.23mm)、0.62~0.63W/kg(板厚:0.27mm)、0.72~0.73W/kg(板厚:0.30mm)であった。
その後、表4に示す各照射条件(s1に換算して0.001~0.08msの範囲)で電子ビームを照射する磁区細分化処理を施し、鉄損および温度:50℃-湿度:98%の湿潤環境に48h暴露した後の錆発生点数を目視で測定した。
測定結果を、表5に示す。
Claims (5)
- 電子ビーム照射が施され、被膜を有する板厚:t(mm)の方向性電磁鋼板であって、温度:50℃、湿度:98%の雰囲気中48時間保持する湿潤試験後に、鋼板表面に錆が発生せず、電子ビーム照射後の鉄損W17/50が、電子ビーム照射前の鉄損W17/50に比べて(-500t2+200t-6.5)%以上低減し、かつ(5t2-2t+1.065)W/kg以下であることを特徴とする方向性電磁鋼板。
- 前記被膜が、コロイダルシリカおよびリン酸塩からなる被膜と、その下地被膜であるフォルステライト被膜であることを特徴とする請求項1に記載の方向性電磁鋼板。
- 被膜を有する方向性電磁鋼板に対し、電子ビームを、圧延方向と交わる向きに照射するに当たり、該電子ビームの照射間隔:d(mm)毎の照射時間をs1(ms)とし、またZ=s1 0.35とした時、該電子ビーム照射条件につき、該電子ビームの単位面積:1cm2当たりの照射エネルギを1.0Z~3.5ZJとし、かつ電子ビームの単位照射長さ:1m当たりの照射エネルギを105ZJ以下とすることを特徴とする方向性電磁鋼板の製造方法。
- 前記照射間隔:d(mm)を0.01~0.5mmの範囲とし、かつ前記照射時間:s1(ms)を0.003~0.1msの範囲とすることを特徴とする請求項3に記載の方向性電磁鋼板の製造方法。
- 前記被膜を、コロイダルシリカおよびリン酸塩からなる被膜と、その下地被膜であるフォルステライト被膜とすることを特徴とする請求項3または4に記載の方向性電磁鋼板の製造方法。
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RU2569269C1 (ru) | 2015-11-20 |
WO2013046716A8 (ja) | 2014-04-10 |
US10011886B2 (en) | 2018-07-03 |
US20140234638A1 (en) | 2014-08-21 |
JP5594437B2 (ja) | 2014-09-24 |
KR101593346B1 (ko) | 2016-02-11 |
EP2762578A4 (en) | 2015-03-11 |
EP2762578A1 (en) | 2014-08-06 |
CN103827326A (zh) | 2014-05-28 |
KR20140061546A (ko) | 2014-05-21 |
EP2762578B1 (en) | 2017-03-22 |
CN103827326B (zh) | 2016-05-11 |
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