WO2012017654A1 - 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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- WO2012017654A1 WO2012017654A1 PCT/JP2011/004409 JP2011004409W WO2012017654A1 WO 2012017654 A1 WO2012017654 A1 WO 2012017654A1 JP 2011004409 W JP2011004409 W JP 2011004409W WO 2012017654 A1 WO2012017654 A1 WO 2012017654A1
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- steel sheet
- electron beam
- irradiation
- annealing
- grain
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- 229910001224 Grain-oriented electrical steel Inorganic materials 0.000 title claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 title claims description 19
- 238000010894 electron beam technology Methods 0.000 claims abstract description 62
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 44
- 239000010959 steel Substances 0.000 claims abstract description 44
- 238000005096 rolling process Methods 0.000 claims abstract description 36
- 229910052839 forsterite Inorganic materials 0.000 claims abstract description 30
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000011248 coating agent Substances 0.000 claims abstract description 27
- 238000000576 coating method Methods 0.000 claims abstract description 27
- 230000005381 magnetic domain Effects 0.000 claims abstract description 27
- 238000000137 annealing Methods 0.000 claims description 67
- 238000001816 cooling Methods 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 18
- 238000004804 winding Methods 0.000 claims description 14
- 238000005097 cold rolling Methods 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 9
- 238000013467 fragmentation Methods 0.000 claims description 8
- 238000006062 fragmentation reaction Methods 0.000 claims description 8
- 238000005261 decarburization Methods 0.000 claims description 5
- 229910000976 Electrical steel Inorganic materials 0.000 claims description 4
- 230000001747 exhibiting effect Effects 0.000 abstract 1
- 230000011218 segmentation Effects 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 73
- 229910052742 iron Inorganic materials 0.000 description 35
- 230000035882 stress Effects 0.000 description 29
- 230000006872 improvement Effects 0.000 description 16
- 230000000694 effects Effects 0.000 description 12
- 238000009826 distribution Methods 0.000 description 11
- 238000001953 recrystallisation Methods 0.000 description 10
- 239000000047 product Substances 0.000 description 9
- 230000001603 reducing effect Effects 0.000 description 8
- 230000001133 acceleration Effects 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 230000006866 deterioration Effects 0.000 description 6
- 238000013461 design Methods 0.000 description 5
- 238000005098 hot rolling Methods 0.000 description 5
- 239000003112 inhibitor Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 229910052711 selenium Inorganic materials 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- 230000001678 irradiating effect Effects 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 229910052717 sulfur Inorganic materials 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 230000004907 flux Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 229910052787 antimony Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000008119 colloidal silica Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000009749 continuous casting Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- GVALZJMUIHGIMD-UHFFFAOYSA-H magnesium phosphate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GVALZJMUIHGIMD-UHFFFAOYSA-H 0.000 description 2
- 239000004137 magnesium phosphate Substances 0.000 description 2
- 229960002261 magnesium phosphate Drugs 0.000 description 2
- 229910000157 magnesium phosphate Inorganic materials 0.000 description 2
- 235000010994 magnesium phosphates Nutrition 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 238000005554 pickling Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 229910052718 tin Inorganic materials 0.000 description 2
- 229910004283 SiO 4 Inorganic materials 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000005524 ceramic coating Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000004033 diameter control Methods 0.000 description 1
- 230000005281 excited state Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000002040 relaxant effect Effects 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
Images
Classifications
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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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
- C21D8/1244—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest
- C21D8/1272—Final recrystallisation annealing
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- 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
- C21D8/1288—Application of a tension-inducing coating
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/008—Ferrous alloys, e.g. steel alloys containing tin
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B3/00—Rolling materials of special alloys so far as the composition of the alloy requires or permits special rolling methods or sequences ; Rolling of aluminium, copper, zinc or other non-ferrous metals
- B21B3/02—Rolling special iron alloys, e.g. stainless steel
-
- 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 suitable as an iron core material such as a transformer and a method for manufacturing the same.
- the grain-oriented electrical steel sheet is mainly used as an iron core of a transformer and is required to have excellent magnetization characteristics, particularly low iron loss.
- it is important to highly align secondary recrystallized grains in the steel sheet in the (110) [001] orientation (so-called Goth orientation) and to reduce impurities in the product steel sheet.
- Goth orientation secondary recrystallized grains in the steel sheet in the (110) [001] orientation
- impurities in the product steel sheet Furthermore, there is a limit in controlling the crystal orientation and reducing impurities in terms of the manufacturing cost. Therefore, a technique for reducing the iron loss by introducing non-uniformity to the surface of the steel sheet by a physical method and subdividing the width of the magnetic domain, that is, a magnetic domain subdivision technique has been developed.
- Patent Document 1 proposes a technique for reducing the iron loss of a steel sheet by irradiating the final product plate with a laser, introducing a high dislocation density region into the steel sheet surface layer, and narrowing the magnetic domain width.
- Patent Document 2 proposes a technique for controlling the magnetic domain width by electron beam irradiation.
- the noise of the actual transformer may increase. Further, the iron loss characteristics are required to be further improved.
- the present invention has been developed in view of the above-mentioned present situation.
- a grain-oriented electrical steel sheet capable of obtaining excellent low noise characteristics and low iron loss characteristics, together with its advantageous manufacturing method.
- the purpose is to provide.
- the tension of the forsterite film (coating mainly composed of Mg 2 SiO 4 ) is increased, and the irradiation surface of the electron beam that is further irradiated in a spot shape
- the iron loss was found to be improved by appropriately controlling the relationship between the diameter of the thermal strain introduction region and the irradiation pitch of the electron beam.
- the present invention has been developed based on the above findings.
- the gist configuration of the present invention is as follows. 1.
- the diameter A and the irradiation pitch B of the thermal strain introduction region on the electron beam irradiation surface are as follows: 0.5 ⁇ B / A ⁇ 5.0 (1) Oriented electrical steel sheet that satisfies this relationship.
- decarburization annealing is performed, and then the steel sheet surface is coated with an annealing separator mainly composed of MgO, and then the final finish annealing is performed.
- a tension coating after the finish annealing or after the tension coating, a method for producing a grain-oriented electrical steel sheet that performs magnetic domain fragmentation treatment by electron beam irradiation, (i) the basis weight of the annealing separator is 10.0 g / m 2 or more, (ii) The coil winding tension after application of the annealing separator is in the range of 30 to 150 N / mm 2 .
- the slab for grain-oriented electrical steel sheet is hot-rolled and then subjected to hot-rolled sheet annealing as necessary, and then subjected to one or more cold rollings or two or more cold rollings sandwiching intermediate annealing, and finally 3.
- (a), (b) is a figure which shows what is not point-like irradiation in irradiation of an electron beam. It is a figure which shows typically the concept of the spot diameter of a thermal strain introduction area
- the present invention in the grain-oriented electrical steel sheet that has been subjected to magnetic domain fragmentation treatment by electron beam irradiation, the tension of the forsterite film is increased, and the electron beam diameter and the region of thermal strain introduction on the surface of the steel sheet that has been subjected to spot irradiation with the electron beam It is important to properly control the relationship between the diameter and the irradiation pitch of the electron beam.
- the electron beam diameter hereinafter also simply referred to as the beam diameter
- the beam diameter means the irradiation diameter of the electron beam.
- the point-like irradiation of the electron beam means that regions having the same size as the two beam diameters (referred to as beam spots in the figure) do not overlap as shown in FIGS. 1 (a) and 1 (b). .
- the “diameter of the thermal strain introduction region (hereinafter also referred to as spot diameter)” means the diameter of the thermal strain introduction region directly by the electron beam as shown in FIG. It is also determined by the width of the generated magnetic domain discontinuity region.
- spot diameter means the diameter of the thermal strain introduction region directly by the electron beam as shown in FIG. It is also determined by the width of the generated magnetic domain discontinuity region.
- FIG. 3 shows the deterioration margin of hysteresis loss due to thermal strain introduced into the steel sheet by electron beam irradiation. It can be seen that when the film tension is strong (with good film tension), the iron loss deterioration margin does not change until the irradiation pitch of the electron beam in the direction intersecting the rolling direction reaches a certain value. On the other hand, when the film tension is weak, the iron loss deterioration margin increases as the irradiation pitch in the direction intersecting the rolling direction increases.
- the irradiation pitch is the distance between the centers of the beam spots.
- FIG. 4 shows an improvement margin for eddy current loss due to thermal distortion introduced into the steel sheet by electron beam irradiation.
- the eddy current loss showed a tendency that the improvement margin increased up to a certain irradiation pitch and the improvement margin decreased thereafter, regardless of the tension difference of the forsterite film.
- Fig. 5 shows the cost for improving the total iron loss.
- the forsterite film has a high tension and when the irradiation pitch in the direction intersecting the rolling direction is increased and spot irradiation is performed, there is a range where the iron loss improvement allowance is particularly large. I understand.
- the electron beam irradiation conditions are as follows: acceleration voltage: 40 kV, beam current: 1.5 mA, beam scanning speed: 5 m / s, beam diameter: 0.2 mm, irradiation pitch in the direction intersecting with the rolling direction: 0.25 mm Irradiation interval: 7.5 mm.
- the tension of the forsterite film was 2.0 MPa or more in both the rolling direction and the direction perpendicular to the rolling direction (hereinafter referred to as the rolling perpendicular direction).
- tensile_strength of a forsterite film if it is in the range which does not plastically deform a steel plate. Preferably it is 200 MPa or less.
- the ratio of the spot diameter A to the irradiation pitch B in the thermal strain introduction region on the beam irradiation surface is expressed by the following formula (1). It is necessary to satisfy the relationship. 0.5 ⁇ B / A ⁇ 5.0 (1)
- the forsterite film tension is improved and the electron beam diameter and the irradiation pitch are appropriately controlled.
- the irradiation conditions other than the electron beam diameter and the irradiation pitch are adjusted, and the ratio of the spot diameter A and the irradiation pitch B in the thermal strain introduction region on the beam irradiation surface is controlled within the range of the above formula (1). It was supposed to be.
- the film tension measuring method in the present invention is as follows.
- a sample of 280 mm in the rolling direction x 30 mm in the direction perpendicular to the rolling direction and 280 mm in the direction perpendicular to the rolling direction and 30 mm in the rolling direction is measured when measuring the tension in the direction perpendicular to the rolling direction. Cut out and peel off the tension coating on both sides with alkaline solution.
- the forsterite film on one side is removed with a hydrochloric acid solution, and the amount of warpage obtained by measuring the amount of warpage of the steel sheet before and after the removal is converted into tension by the following conversion formula (3).
- the tension obtained by this method is the tension applied to the surface from which the forsterite film has not been removed.
- the tension on one side of the steel sheet is obtained by the above-described method, and the tension on the opposite side is obtained by a similar method using a sample in another place of the same product. Then, an average value is derived, and the average value is taken as the tension applied to the sample.
- the difference in the tensile stress distribution applied to other than the irradiated portion is caused by the difference in the compressive stress distribution, and the eddy current loss improvement margin is improved.
- the reduction in eddy current loss improvement at a certain irradiation pitch or more is considered to be a result of an increase in the region where the compressive stress is low due to the change in the compressive stress distribution described above.
- this stress non-uniformity is also the reason why the ratio of the spot diameter A and the irradiation pitch B in the thermal strain introduction region on the beam irradiation surface must be set as described above by adjusting the irradiation conditions other than the irradiation pitch and the beam diameter. It is thought to maintain. This is because when the irradiation conditions other than the irradiation pitch and the beam diameter are inappropriate, the stress non-uniformity generated by the irradiation pitch and beam diameter control is easily eliminated.
- One of the points of the production method in the present invention is to increase the tension of the forsterite film applied to the steel plate.
- I Make the application amount of annealing separator 10.0g / m 2 or more, II Control coil winding tension after application of annealing separator to 30-150 N / mm 2 III It is important to control the average cooling rate up to 700 °C in the cooling process during final finish annealing to 50 °C / h or less.
- the annealing separator releases moisture, CO 2 and the like during annealing, the volume of the region where the annealing separator is applied is smaller than that at the time of application. That is, the decrease in volume means that voids are generated in the application region, and therefore, the amount of the annealing separator applied will affect the stress relaxation in the coil. Accordingly, in the present invention, if the basis weight of the annealing separator is small, the voids are insufficient, so the application amount of the annealing separator is limited to 10.0 g / m 2 or more.
- the amount of the annealing separator applied is not particularly limited as long as there is no inconvenience in the production process (coil winding deviation or the like during final finish annealing). If inconvenience such as the above-mentioned winding deviation occurs, it is preferably 50 g / m 2 or less.
- the cooling rate at the time of final finish annealing is reduced, the temperature distribution in the steel sheet is reduced, so the stress in the coil is relaxed. From the viewpoint of stress relaxation, the slower the cooling rate, the better. However, it is not preferable from the viewpoint of production efficiency, and is preferably 5 ° C./h or more.
- the relaxation of the stress in the coil is performed only by controlling the cooling rate, the cooling rate cannot be set to 5 ° C./h or more, but in the present invention, the application amount of the annealing separator and the control of the winding tension are controlled. Therefore, the cooling rate is allowed up to 50 ° C / h.
- the second point is that the electron beam diameter should be 0.5 mm or less and irradiate in a spot shape. If the electron beam diameter is too large, the penetration of the electron beam in the plate thickness direction becomes small, and an optimal stress distribution cannot be obtained. Therefore, it is necessary to increase the amount of energy penetrating in the plate thickness direction by irradiating electrons in the narrowest possible region with an electron beam diameter of 0.5 mm or less. More preferably, it is 0.3 mm or less. Further, the ratio of the electron beam diameter A ′ and the irradiation pitch B in the direction crossing the rolling direction is expressed by the following equation (2). 1.0 ⁇ B / A ′ ⁇ 7.0 (2) It is necessary to control within the range.
- the ratio of the spot diameter A to the irradiation pitch B is expressed by the following formula (1) 0.5 ⁇ B / A ⁇ 5.0 (1) It is necessary to control within the range. This is because an optimal stress distribution cannot be obtained if a beam current value or scanning speed that does not satisfy this relationship is set.
- 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.
- C 0.08 mass% or less
- the burden of reducing C to 50 massppm or less where no magnetic aging occurs during the manufacturing process increases. Therefore, the content is preferably 0.08% by mass or less.
- 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, and its content of 2.0% by mass or more is particularly effective for reducing iron loss. On the other hand, when it is 8.0% by mass or less, particularly excellent workability and magnetic flux density can be obtained. Accordingly, 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 advantageous for improving the hot workability, but if the content is less than 0.005% by mass, the effect of addition is poor. On the other hand, if it is 1.0 mass% or less, the magnetic flux density of a product board will become especially favorable. Therefore, the Mn content is preferably in the range of 0.005 to 1.0% by 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 mass% is an element useful for further improving the hot rolled sheet structure and further improving the magnetic properties.
- the content is less than 0.03% by mass, the effect of improving the magnetic properties is small.
- the content is 1.5% by mass or less, the stability of secondary recrystallization is increased, and the magnetic properties are further improved. Therefore, the Ni content is preferably in the range of 0.03 to 1.5% by mass.
- Sn, Sb, Cu, P, Mo, and Cr are elements that are useful for further improving the magnetic properties, but if any of them is less than the lower limit of each component, the effect of improving the magnetic properties is small.
- the amount is not more than the upper limit amount of each component described above, the development of secondary recrystallized grains is the best. For this reason, it is preferable to make it contain in said range, respectively.
- 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 main purpose of hot-rolled sheet annealing is to eliminate the band structure generated by hot rolling and to make the primary recrystallized structure sized, thereby further developing the goth structure and improving the magnetic properties in the secondary recrystallization annealing. That is.
- 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 recrystallized structure and obtaining the desired secondary recrystallization improvement. I can't.
- the hot-rolled sheet annealing temperature exceeds 1100 ° C., the grain size after the hot-rolled sheet annealing becomes too coarse, and it becomes difficult to realize a sized primary recrystallized structure.
- decarburization annealing (also used for recrystallization annealing) is performed, and an annealing separator is applied. .
- a final finish annealing is performed for the purpose of secondary recrystallization and forsterite film formation.
- the annealing separator is preferably composed mainly of MgO in order to form forsterite.
- MgO as a main component means that it may contain a known annealing separator component or property improving component other than MgO as long as it does not inhibit the formation of the forsterite film that is the object of the present invention. To do.
- 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) capable of imparting tension to a steel sheet in order to reduce iron loss.
- the tension coating include silica-containing inorganic coating, physical vapor deposition, and ceramic coating by chemical vapor deposition.
- the directional electrical steel sheet after the final finish annealing or after the tension coating described above is subjected to magnetic domain refinement by irradiating the surface of the steel sheet with an electron beam at any time.
- the depth of plastic strain applied to the steel sheet is preferably about 10 to 40 ⁇ m.
- the irradiation direction of the electron beam needs to be performed in a direction crossing the rolling direction, and this irradiation direction is preferably performed in a direction of about 45 to 90 degrees with respect to the rolling direction.
- a method of manufacturing a grain-oriented electrical steel sheet that performs a magnetic domain subdivision process using a conventionally known electron beam can be applied except for the steps and manufacturing conditions described above.
- an annealing separator mainly composed of MgO was applied.
- the coating amount of the annealing separator and the winding tension after application of the annealing separator were changed.
- final finish annealing for the purpose of secondary recrystallization and purification was performed at 1180 ° C. for 60 hours. In this final finish annealing, the average cooling rate in the cooling process in the temperature range of 700 ° C. or higher was changed. Then, a tension coating consisting of 50% colloidal silica and magnesium phosphate was applied.
- acceleration voltage 50kV
- beam current 2.0mA
- beam scanning speed 15m / sec
- beam diameter 0.18mm
- irradiation interval in rolling direction 6.0mm
- irradiation pitch in direction intersecting rolling direction 0.5mm rolling direction
- Angle of crossing A magnetic domain fragmentation treatment was applied to irradiate an electron beam in a spot shape under an irradiation condition of 80 degrees to obtain a product, and the iron loss and film tension were measured.
- each product was subjected to oblique shearing, a three-phase transformer of 750 kVA was assembled, and iron loss and noise were measured in a state excited at 50 Hz and 1.7 T.
- the design value of noise in this transformer is 62dB.
- the measurement results of the iron loss and noise described above are also shown in Table 2.
- an annealing separator mainly composed of MgO was applied.
- the coating amount of the annealing separator was 12 g / m 2 and the winding tension was 60 N / mm 2 .
- final finish annealing for the purpose of secondary recrystallization and purification was performed at 1180 ° C. for 60 hours.
- the average cooling rate up to 700 ° C. was set to 15 ° C./h.
- a tension coating consisting of 50% colloidal silica and magnesium phosphate was applied.
- the magnetic domain was subdivided with an electron beam and a laser to obtain a product, and the iron loss and film tension were measured.
- the beam diameter, the irradiation pitch in the direction intersecting the rolling direction, the beam current value, and the scanning speed were changed as shown in Table 3.
- Other conditions are as follows.
- Electron beam acceleration voltage: 150 kV
- Laser Wavelength: 0.53 ⁇ m pulse laser, beam scanning speed: 300mm / sec, laser output: 15W, irradiation interval in rolling direction: 5mm
- each product was sheared at an oblique angle
- a 500 kVA three-phase transformer was assembled, and iron loss and noise were measured in an excited state at 50 Hz and 1.7 T.
- the design value of noise in this transformer is 55dB.
- the measurement results of the iron loss and noise described above are also shown in Table 3.
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Abstract
Description
そのためには、鋼板中の二次再結晶粒を(110)[001]方位(いわゆる、ゴス方位)に高度に揃えることや製品鋼板中の不純物を低減することが重要である。さらに、結晶方位の制御や、不純物を低減することは、製造コストとの兼ね合い等で限界がある。そこで、鋼板の表面に対して物理的な手法で不均一性を導入し、磁区の幅を細分化して鉄損を低減する技術、すなわち磁区細分化技術が開発されている。
また、鉄損特性については、更なる改善が要求されている。
その結果、電子ビーム照射による磁区細分化処理済の方向性電磁鋼板において、フォルステライト被膜(Mg2SiO4を主体とする被膜)の張力をアップし、さらに点状に照射する電子ビームの照射面における熱歪み導入領域の直径と電子ビームの照射ピッチとの関係を適正に制御することで鉄損が改善することを見出した。
本発明は、上記した知見に基づき開発されたものである。
1.表面にフォルステライト被膜をそなえ、電子ビーム照射による磁区細分化処理済の方向性電磁鋼板であって、該フォルステライト被膜による鋼板への付与張力が、圧延方向および圧延方向と直角な方向ともに2.0MPa以上であり、かつ電子ビーム照射面における熱歪み導入領域の直径Aと照射ピッチBとが、次式(1)
0.5≦B/A≦5.0 ・・・(1)
の関係を満足する方向性電磁鋼板。
(i) 焼鈍分離剤の目付け量を10.0g/m2以上とする、
(ii) 焼鈍分離剤塗布後のコイル巻き取り張力を30~150N/mm2の範囲とする、
(iii) 最終仕上げ焼鈍工程の冷却過程における700℃までの平均冷却速度を50℃/h以下に制御する、
(iv) 電子ビーム径を0.5mm以下とし、かつ電子ビーム径A´と照射ピッチBとを、次式(2)
1.0≦B/A´≦7.0 ・・・(2)
の範囲に制御する、
(v) 電子ビーム径と照射ピッチ以外の照射条件を調整して、ビーム照射面における熱歪み導入領域の直径Aと照射ピッチBとを、次式(1)
0.5≦B/A≦5.0 ・・・(1)
の範囲に制御する方向性電磁鋼板の製造方法。
本発明では、電子ビーム照射による磁区細分化処理済の方向性電磁鋼板において、フォルステライト被膜の張力をアップすること、および電子ビーム径および電子ビームを点状照射した鋼板表面における熱歪み導入領域の直径と電子ビームの照射ピッチとの関係を適正に制御することが重要である。
なお、本発明における電子ビーム径(以下、単にビーム径ともいう)とは、電子ビームの照射直径を意味する。また、電子ビームの点状照射とは、図1(a)および(b)にそれぞれ示すように2つのビーム径と同じ大きさの領域(図中、ビームスポットという)が重ならないことを意味する。
また、「熱歪み導入領域の直径(以下、スポット径ともいう)」とは、図2に示すように、直接的には電子ビームによる熱歪み導入領域の直径を意味するが、熱歪み導入によって生じた磁区不連続部領域の幅によっても求められる。
ここに、電子ビームを照射した場合は、電子ビームのビーム径と同じ大きさの領域が加熱されるものの、鋼板に与えられた熱は拡散するので、一般的に、熱歪み導入領域のスポット径はビーム径よりも大きくなる。なお、本発明において、特に断らない場合、径は直径を意味する。
フォルステライト被膜の張力が種々に異なるサンプルに電子ビームを照射した。ここに、鉄損に及ぼす張力の影響を調査した。照射条件は、加速電圧:40kV、ビーム電流:1.5 mA、ビーム走査速度:5m/s、ビーム径:0.2mm、圧延方向と交差する方向の照射ピッチ:0.05, 0.10, 0.15, 0.25, 0.5, 1.0, 1.4, 3.0, 5.0および10.0mmならびに圧延方向の照射間隔:7.5mmで実施した。
この時、電子ビームの照射条件は、加速電圧:40kV、ビーム電流:1.5mA、ビーム走査速度:5m/s、ビーム径:0.2mm、圧延方向と交差する方向の照射ピッチ:0.25mm圧延方向の照射間隔:7.5mmとした。
図6に示したように、フォルステライト被膜の張力が圧延方向および圧延方向と直角な方向(以下、圧延直角方向という)ともに2.0MPa以上の場合に、鉄損が大きく改善されることが判明した。なお、フォルステライト被膜の張力については、鋼板が塑性変形しない範囲内であればとくに上限はない。好適には200MPa以下である。
0.5≦B/A≦5.0 ・・・(1)
製品(張力コーティング塗布材)より、圧延方向の張力を測定する場合は、圧延方向280mm×圧延直角方向30mm、圧延直角方向の張力を測定する場合は、圧延直角方向280mm×圧延方向30mmのサンプルを切り出し、両面の張力コーティングをアルカリ溶液で剥離する。ついで、片面のフォルステライト被膜を塩酸溶液で除去し、その除去前後の鋼板反り量を測定して得られた反り量を以下の換算式(3)にて張力換算する。この方法で求めた張力は、フォルステライト被膜を除去しなかった面に付与されている張力である。
本発明では、張力がサンプル両面に付与されているので、上記した方法で鋼板の片面の張力を求め、さらに同じ製品の別の場所のサンプルを用いて、反対面の張力を同様の方法で求めて、平均値を導出し、その平均値をサンプルに付与されている張力とする。
(点状照射によって渦電流損の改善代が増加する理由)
鋼板への投入熱量が同じ場合、電子ビームの照射ピッチが狭いと、照射線上の領域に一定量の熱量が投入されて、均一な圧縮応力分布となる。一方、照射ピッチを広くして、局所部により多くの熱量を投入すると、局所的に大きな圧縮応力が付与されて、不均一な応力分布となる。本発明では、これらの圧縮応力分布の差によって、照射部以外へ付与される引張応力分布に差が生じ、渦電流損改善代が向上したものと考えている。
また、ある一定以上の照射ピッチで、渦電流損改善代が低下することも、上記した圧縮応力分布の変化により、圧縮応力が低い領域が増加した結果と考えている。
本発明では、フォルステライト被膜が鋼板に付与する応力によって、熱歪みにより発生する応力が緩和され、鋼板の履歴損劣化を抑制していると考えられる。
すなわち、熱歪が導入される照射部付近において、磁歪振動波形が歪み、騒音に高調波成分が重畳されることで騒音が増大するが、このような磁歪振動波形の歪みの低減に、フォルステライト被膜の張力をアップすることが極めて有効に作用していると考えられる。
本発明における製造方法のポイントの一つは、鋼板に付与したフォルステライト被膜の張力をアップさせることである。フォルステライト被膜の張力をアップさせる手段としては、
I 焼鈍分離剤の塗布量を10.0g/m2以上にする、
II 焼鈍分離剤塗布後のコイル巻き取り張力を30~150N/mm2に制御する、
III 最終仕上げ焼鈍時の冷却過程における700℃までの平均冷却速度を50℃/h以下に制御することが重要である。
従って、フォルステライト被膜へのダメージを抑制するためには、鋼板間に少しの空隙を与えて、鋼板に発生する応力を低減することおよび冷却速度を低減してコイル内の温度差を低減することが有効となる。
焼鈍分離剤は、焼鈍中に水分やCO2などを放出するため、焼鈍分離剤を塗布した領域は、塗布時より体積が減少する。すなわち、体積が減少するということは、塗布領域に空隙が生じることを意味しているので、焼鈍分離剤の塗布量の多少がコイル内の応力緩和に作用することとなる。
従って、本発明では、焼鈍分離剤の目付け量が少ないと空隙が不十分であることから、焼鈍分離剤の塗布量を10.0g/m2以上に限定する。なお、焼鈍分離剤の塗布量は、生産工程に不都合(最終仕上げ焼鈍時のコイルの巻きずれ等)のない限り、とくに上限はない。上記巻きずれなどの不都合が生じるようであれば、50g/m2以下とすることが好ましい。
このように、焼鈍分離剤の塗布量、巻き取り張力および冷却速度の制御を行い、コイル内の応力を緩和させることによって、圧延方向および圧延直角方向のフォルステライト被膜張力をアップさせることが可能になる。
1.0≦B/A´≦7.0 ・・・(2)
の範囲に制御することが必要である。
というのは、比(B/A´)が1.0未満では、照射ピッチが狭すぎて不均一な応力分布が発生しないからである。一方、比(B/A´)が7.0超の場合は、応力発生ポイントが離れすぎ、応力が低い領域が発生するため、磁区細分化効果が不十分になり鉄損改善効果が低下する。
0.5≦B/A≦5.0 ・・・(1)
の範囲に制御することが必要である。
というのは、この関係を満足しないビーム電流値や走査速度を設定した場合は、最適な応力分布が得られないからである。
というのは、レーザーと電子ビームとで鋼板内における熱の伝わり方が異なる。ここに、電子ビームの方が板厚方向への侵入が容易なので、鋼板に発生する応力分布がそれぞれ異なることが推定される。従って、レーザ照射による磁区細分化の過程においては、鋼板に発生する応力分布が鉄損を低減する領域を生じさせることがなかったためと考えている。
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、結晶粒の<100>方向への集積度が高いほど、磁区細分化による鉄損低減効果は大きくなるので、集積度の指標となる磁束密度B8が1.90T以上であることが好ましい。
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、0.08質量%を超えると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を低減する負担が増大するため、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り、含有量が2.0質量%以上でとくに鉄損低減効果が良好である。一方、8.0質量%以下の場合、とくに優れた加工性や磁束密度を得ることができる。従って、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有利な元素であるが、含有量が0.005質量%未満ではその添加効果に乏しい。一方1.0質量%以下とすると製品板の磁束密度がとくに良好となる。このため、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、熱延板組織をさらに改善して磁気特性を一層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1.5質量%以下ではとくに二次再結晶の安定性が増し、磁気特性がさらに改善される。そのため、Ni量は0.03~1.5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。
本発明において電子ビームの照射方向は、圧延方向と交差する方向に行う必要があるが、この照射方向は、圧延方向に45~90度程度の方向に対して行うことが好ましい。
表1に示す成分組成になる鋼スラブを連続鋳造にて製造し、1430℃に加熱後、熱間圧延により板厚:1.6mmの熱延板としたのち、1000℃で10秒の熱延板焼鈍を施した。ついで、冷間圧延により中間板厚:0.55mmとし、酸化度PH2O/PH2=0.37、温度:1100℃、時間:100秒の条件で中間焼鈍を実施した。その後、塩酸酸洗により表面のサブスケールを除去したのち、再度、冷間圧延を実施して、板厚:0.23mmの冷延板とした。
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た。
ついで、各製品を斜角せん断し、750kVAの三相トランスを組み立て、50Hz、1.7Tで励磁した状態での鉄損および騒音を測定した。本トランスにおける騒音の設計値は62dBである。
上記した鉄損および騒音の測定結果を表2に併記する。
これに対し、No.2,3,8,11は焼鈍分離剤の塗布量が本発明の範囲外、No.10,11,12は巻き取り張力が本発明の範囲外、No.7,12は冷却速度が本発明の範囲外となっており、鋼板に付与した張力が本発明を満足しておらず、そのいずれもが騒音の設計値を満足していない。
表1に示す成分組成になる鋼スラブを連続鋳造にて製造し、1430℃に加熱後、熱間圧延により板厚:1.6mmの熱延板としたのち、1000℃で10秒の熱延板焼鈍を施した。ついで、冷間圧延により中間板厚:0.55mmとし、酸化度PH2O/PH2=0.37、温度:1100℃、時間:100秒の条件で中間焼鈍を実施した。その後、塩酸酸洗により表面のサブスケールを除去したのち、再度、冷間圧延を実施して、板厚:0.23mmの冷延板とした。
a) 電子ビーム:加速電圧:150kV、圧延方向の照射間隔:5mm、圧延方向と交差する角度:90度
b) レーザ:波長:0.53μmのパルスレーザ、ビーム走査速度:300mm/秒、レーザ出力:15W、圧延方向の照射間隔:5mm
ついで、各製品を斜角せん断し、500kVAの三相トランスを組み立て、50Hz、1.7Tで励磁した状態での鉄損および騒音を測定した。本トランスにおける騒音の設計値は55dBである。
上記した鉄損および騒音の測定結果を表3に併記する。
これに対し、レーザーで磁区細分化を行ったNo.6,8,10の比較例、また電子ビームによる磁区細分化処理を施したものの、熱歪み導入領域のスポット径Aやビーム径A’、これらと照射ピッチBとの関係などが本発明の範囲外であるNo.2,4,5,9,12,13,14の比較例は、そのいずれもが鉄損性に劣っていた。
Claims (3)
- 表面にフォルステライト被膜をそなえ、電子ビーム照射による磁区細分化処理済の方向性電磁鋼板であって、該フォルステライト被膜による鋼板への付与張力が、圧延方向および圧延方向と直角な方向ともに2.0MPa以上であり、かつ電子ビーム照射面における熱歪み導入領域の直径Aと照射ピッチBとが、次式(1)
0.5≦B/A≦5.0 ・・・(1)
の関係を満足する方向性電磁鋼板。 - 方向性電磁鋼板用スラブを圧延して最終板厚に仕上げたのち、脱炭焼鈍を施し、ついで鋼板表面にMgOを主成分とする焼鈍分離剤を塗布してから、最終仕上げ焼鈍を行った後、張力コーティングを施し、該仕上げ焼鈍後または該張力コーティング後に、電子ビーム照射による磁区細分化処理を行う方向性電磁鋼板の製造方法であって、
(i) 焼鈍分離剤の目付け量を10.0g/m2以上とする、
(ii) 焼鈍分離剤塗布後のコイル巻き取り張力を30~150N/mm2の範囲とする、
(iii) 最終仕上げ焼鈍工程の冷却過程における700℃までの平均冷却速度を50℃/h以下に制御する、
(iv) 電子ビーム径を0.5mm以下とし、かつ電子ビーム径A´と照射ピッチBとを、次式(2)
1.0≦B/A´≦7.0 ・・・(2)
の範囲に制御する、
(v) 電子ビーム径と照射ピッチ以外の照射条件を調整して、ビーム照射面における熱歪み導入領域の直径Aと照射ピッチBとを、次式(1)
0.5≦B/A≦5.0 ・・・(1)
の範囲に制御する方向性電磁鋼板の製造方法。 - 方向性電磁鋼板用スラブを、熱間圧延し、ついで必要に応じて熱延板焼鈍を施したのち、1回の冷間圧延または中間焼鈍を挟む2回以上の冷間圧延を施して、最終板厚に仕上げる請求項2に記載の方向性電磁鋼板の製造方法。
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EP2602339A1 (en) | 2013-06-12 |
EP2602339B1 (en) | 2018-04-18 |
JP2012036445A (ja) | 2012-02-23 |
US9536658B2 (en) | 2017-01-03 |
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US20130143050A1 (en) | 2013-06-06 |
JP5593942B2 (ja) | 2014-09-24 |
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