WO2020149330A1 - 方向性電磁鋼板の製造方法 - Google Patents
方向性電磁鋼板の製造方法 Download PDFInfo
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- WO2020149330A1 WO2020149330A1 PCT/JP2020/001161 JP2020001161W WO2020149330A1 WO 2020149330 A1 WO2020149330 A1 WO 2020149330A1 JP 2020001161 W JP2020001161 W JP 2020001161W WO 2020149330 A1 WO2020149330 A1 WO 2020149330A1
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Definitions
- the present invention relates to a method for manufacturing a grain-oriented electrical steel sheet having excellent coating adhesion.
- the present invention relates to a method for producing a grain-oriented electrical steel sheet which does not have a forsterite coating and is excellent in coating adhesion of an insulating coating.
- the present application claims priority based on Japanese Patent Application No. 2019-005059 filed in Japan on January 16, 2019, the contents of which are incorporated herein by reference.
- Oriented electrical steel sheet is a soft magnetic material and is mainly used as an iron core material for transformers. Therefore, magnetic properties such as high magnetization and low iron loss are required.
- the magnetization characteristic is the magnetic flux density induced when the iron core is excited. The higher the magnetic flux density is, the smaller the iron core can be made, which is advantageous in terms of the device configuration of the transformer and also in terms of the manufacturing cost of the transformer.
- Iron loss is the power loss consumed as heat energy when the iron core is excited by an alternating magnetic field. From the viewpoint of energy saving, iron loss is required to be as low as possible. The degree of iron loss is affected by magnetic susceptibility, plate thickness, film tension, amount of impurities, electrical resistivity, crystal grain size, magnetic domain size and the like. Although various technologies have been developed for magnetic steel sheets, research and development for reducing iron loss are being continued in order to improve energy efficiency.
- a forsterite film 2 mainly composed of Mg 2 SiO 4 (forsterite) is formed on a base material steel sheet 1, and the forsterite film 2 is formed on the forsterite film 2.
- the insulating film 3 is formed.
- the forsterite film and the insulating film have the functions of electrically insulating the surface of the base material steel sheet and applying tension to the base material steel sheet to reduce iron loss.
- the forsterite coating contains trace amounts of impurities and additives contained in the base steel sheet and the annealing separator, and their reaction products.
- the insulation film In order for the insulation film to exhibit insulation properties and the required tension, it must not be peeled off from the electrical steel sheet. Therefore, the insulating film is required to have high film adhesion. However, it is not easy to simultaneously increase both the tension applied to the base steel sheet and the film adhesion. Even now, research and development that enhances both of these are ongoing.
- Oriented electrical steel sheets are usually manufactured by the following procedure.
- a silicon steel slab containing 2.0 to 7.0 mass% of Si is hot-rolled, the hot-rolled steel sheet is annealed if necessary, and then the annealed steel sheet is once or intermediately annealed.
- Cold rolling is performed twice or more to sandwich the steel sheet to the final thickness.
- decarburization annealing is performed on the steel sheet having the final thickness in a wet hydrogen atmosphere to promote decarburization, promote primary recrystallization, and form an oxide layer on the surface of the steel sheet.
- An annealing separator having MgO (magnesia) as a main component is applied to a steel sheet having an oxide layer and dried, and after drying, the steel sheet is wound into a coil shape.
- the coil-shaped steel sheet is subjected to finish annealing to promote secondary recrystallization, and the crystal orientation of the crystal grains is integrated in the Goss orientation.
- MgO in the annealing separator is reacted with SiO 2 (silica) in the oxide layer to form an inorganic forsterite film mainly composed of Mg 2 SiO 4 on the surface of the base steel plate.
- the steel sheet with the forsterite coating is subjected to purification annealing to remove impurities in the base steel sheet by diffusing outward. Further, after flattening annealing is performed on the steel sheet, for example, a solution containing phosphate and colloidal silica as a main component is applied to the surface of the steel sheet having a forsterite film and baked to form an insulating film. At this time, tension due to the difference in coefficient of thermal expansion is applied between the crystalline base material steel sheet and the substantially amorphous insulating film. Therefore, the insulating film is sometimes called a tension film.
- the interface between the forsterite film mainly composed of Mg 2 SiO 4 (“2” in FIG. 1) and the steel plate (“1” in FIG. 1) usually has uneven unevenness (see FIG. 1). ).
- the uneven interface slightly reduces the iron loss reducing effect due to the tension. If this interface is smoothed, iron loss is reduced, and thus far, the following developments have been carried out.
- Patent Document 1 discloses a manufacturing method in which the forsterite film is removed by means such as pickling, and the surface of the steel sheet is smoothed by chemical polishing or electrolytic polishing. However, in the manufacturing method of Patent Document 1, it may be difficult for the insulating coating to adhere to the surface of the base steel sheet.
- an intermediate layer 4 (or a base film) may be formed between the base steel plate and the insulating film.
- the undercoating film formed by applying an aqueous solution of phosphate or alkali metal silicate disclosed in Patent Document 2 is also effective in film adhesion.
- Patent Document 3 discloses a method in which a steel sheet is annealed in a specific atmosphere to form an externally oxidized silica layer as an intermediate layer on the surface of the steel sheet before forming an insulating film. ing.
- Patent Documents 4 to 6 in the case where an insulating film containing an acidic organic resin that does not substantially contain chromium as a main component is formed on a steel plate, a phosphorus compound layer (FePO 4 , Fe 3) is provided between the steel plate and the insulating film.
- (PO 4) 2, FeHPO 4 , Fe (H 2 PO 4) 2, Zn 2 Fe (PO 4) 2, Zn 3 (PO 4) 2, and a layer consisting of a hydrate, or, Mg There is disclosed a technique of increasing the appearance and adhesion of an insulating film by forming a layer composed of Ca or Al phosphate and having a thickness of 10 to 200 nm).
- a stress-strained portion or groove extending in a direction intersecting with the rolling direction is formed at a predetermined interval along the rolling direction to obtain 180°.
- a magnetic domain control method is known in which the width of the magnetic domain is narrowed (180° magnetic domain is subdivided).
- the 180° magnetic domain subdivision effect of the reflux magnetic domain generated in the strained portion (strained region) is utilized.
- a typical method is to use shock waves or rapid heating by laser beam irradiation. In this method, the surface shape of the irradiated portion is hardly changed, and the stress-strained portion is formed on the base steel sheet.
- the method of forming the groove utilizes the demagnetizing effect of the magnetic poles generated on the side wall of the groove. That is, the magnetic domain control is classified into a strain imparting type and a groove forming type.
- Patent Document 7 after removing the oxide on the surface of the finish-annealed steel plate to form a smooth surface, a film is formed on the surface, and the magnetic domains are subdivided by laser beam, electron beam, or plasma flame irradiation. Is disclosed.
- Japanese Patent Laid-Open Publication No. 49-096920 Japanese Patent Laid-Open No. 05-279747 Japanese Unexamined Patent Publication No. 06-184762 Japanese Patent Laid-Open No. 2001-220683 Japanese Patent Laid-Open No. 2003-193251 Japanese Patent Laid-Open No. 2003-193252 Japanese Patent Laid-Open No. 11-012755
- the forsterite coating as shown in FIG.
- the present inventors have studied various magnetic domain controls, and as a result of increasing the energy density of the laser beam or electron beam with which the grain-oriented electrical steel sheet is irradiated, magnetic domains are preferable. Focused on being subdivided.
- the method for manufacturing the grain-oriented electrical steel sheet according to this embodiment is not limited to the following method.
- the following manufacturing method is one example for manufacturing the grain-oriented electrical steel sheet according to the present embodiment.
- the grain-oriented electrical steel sheet according to the present embodiment is a base material steel sheet in which generation of a forsterite film is suppressed during finish annealing or the forsterite film is removed after finish annealing, as a starting material, with respect to this base material steel sheet, It suffices to form the intermediate layer, form the insulating film, and form the strained region to manufacture.
- an annealing separator containing alumina as a main component can be used instead of magnesia.
- An annealing separator containing alumina as a main component is applied to the surface of a steel sheet having an oxide layer and dried, and after drying, the steel sheet is wound into a coil. Then, the coiled steel sheet is subjected to finish annealing (secondary recrystallization).
- finish annealing secondary recrystallization
- the annealing separator containing alumina as a main component is used, even if finish annealing is performed, formation of a film of an inorganic mineral substance such as forsterite on the surface of the steel sheet is suppressed.
- the surface of the steel sheet is preferably finished by chemical polishing or electrolytic polishing to be smooth.
- the rolling direction of the base steel sheet is a rolling direction in hot rolling or cold rolling when the base steel sheet is manufactured by the manufacturing method described below.
- the rolling direction may be referred to as a steel sheet passing direction, a conveying direction, or the like.
- the rolling direction is the longitudinal direction of the base steel sheet.
- the rolling direction can also be specified using an apparatus for observing the magnetic domain structure or an apparatus for measuring the crystal orientation such as the X-ray Laue method.
- the region excluding the base metal steel plate specified above there is a region where the P content is 5 atom% or more and the O content is 30 atom% or more, excluding the measurement noise, and corresponding to this region If the line segment (thickness) on the scanning line of the line analysis is 300 nm or more, this region is determined to be an insulating film.
- the total content of Fe, Cr, P and O is 70 atomic% or more and the Si content is less than 10 atomic% excluding measurement noise.
- the area is determined to be a deposit.
- M 2 P 2 O 7 may exist in the conventional insulating film, this M 2 P 2 O 7 (M is at least one of Fe and Cr, or both) is subjected to electron diffraction.
- the crystal structure can be specified and discriminated from the pattern.
- the area in the map is divided into an area where the CI value is equal to or more than the critical value and an area where the CI value is less than the critical value. Then, one of the regions is set as a strained region (irradiated region), and the other region is set as a region other than the strained region (unirradiated region). Thereby, the distorted area can be specified.
- the region 5 may be composed only precipitate M 2 P 4 O 13, or may be a region including the precipitates and other precipitate M 2 P 4 O 13. Further, the region 6 may be composed only of the amorphous phosphorus oxide deposits, or may be a region containing the amorphous phosphorus oxide deposits and other deposits.
- the total length of the observation visual field in the direction orthogonal to the sheet thickness direction is L.
- L d the length of the observation visual field in the direction orthogonal to the sheet thickness direction
- ⁇ L d the line segment ratio X of the void region in which the voids exist.
- the line segment ratio X is more preferably 20% or less.
- the length of the overlapped portion is subtracted from the length L d of the overlapped void to obtain the void length.
- the length of the two voids 8 that overlap when viewed along the plate thickness direction is L 4 obtained by subtracting the overlapping length.
- the line segment ratio X is more preferably 10% or less from the viewpoint of improving the adhesiveness of the insulating film.
- the lower limit of the line segment ratio X is not particularly limited and may be 0%.
- the binarization of the image for image analysis may be performed by manually coloring the voids in the tissue photograph based on the above-described void discrimination result and binarizing the image.
- the line segment ratio of the void is measured at three locations in the direction perpendicular to the rolling direction and the plate thickness direction of the base material steel plate at intervals of 50 mm or more for the same strain region, Let X be the arithmetic mean value of the line segment ratios.
- the ratio of M 2 P 4 O 13 in the insulating film in the central portion is 10% or more in area ratio in a cross-sectional view of a plane parallel to the rolling direction and the sheet thickness direction. % Or less is more preferable.
- the area ratio is preferably 20% or more, more preferably 30% or more.
- the area ratio is preferably 50% or less, more preferably 40% or less.
- the precipitates should be specified by the above-mentioned method, and then the precipitates of M 2 P 4 O 13 should be specified by analyzing the electron beam diffraction pattern.
- the area ratio of M 2 P 4 O 13 in the central insulating film is the total cross sectional area of M 2 P 4 O 13 in the same cross section with respect to the total cross sectional area of the central insulating film including precipitates and voids. Is the ratio of.
- These cross-sectional areas may be calculated by image analysis or may be calculated from cross-sectional photographs.
- the area ratio of the amorphous phosphorous oxide region in the central insulating film is 1% or more and 60% or less in a sectional view of a plane parallel to the rolling direction and the sheet thickness direction. More preferably.
- the area ratio of the amorphous phosphorous oxide region is 1% or more, local stress in the insulating film is relieved. Further, when the area ratio of the amorphous phosphorous oxide region is 60% or less, the effect of not lowering the tension of the insulating film can be obtained.
- the area ratio of the amorphous phosphorus oxide region is more preferably 5% or more, and the area ratio of the amorphous phosphorus oxide region is more preferably 40% or less.
- the area ratio of the amorphous phosphorous oxide region in the central insulating film can be measured by the same method as the area ratio of M 2 P 4 O 13 in the central insulating film.
- the composition of the base steel sheet is not particularly limited.
- the grain-oriented electrical steel sheet is manufactured through various processes, there are preferable component compositions of the raw steel billet (slab) and the base material steel sheet for manufacturing the grain-oriented electrical steel sheet according to the present embodiment.
- the composition of these components will be described below.
- % relating to the composition of the raw steel billet and the base steel sheet means mass% with respect to the total mass of the raw steel billet or the base steel sheet.
- the base steel sheet of the grain-oriented electrical steel sheet according to the present embodiment contains, for example, Si: 0.8 to 7.0%, C: 0.005% or less, N: 0.005% or less, S and Se. Is limited to 0.005% or less and acid-soluble Al: 0.005% or less, with the balance being Fe and impurities.
- Si 0.8% or more and 7.0% or less Si (silicon) increases the electrical resistance of the grain-oriented electrical steel sheet and reduces iron loss.
- the lower limit of the Si content is preferably 0.8% or more, and more preferably 2.0% or more.
- the preferable upper limit of the Si content is 7.0% or less.
- C 0.005% or less C (carbon) forms a compound in the base steel sheet and deteriorates iron loss, so the smaller the amount, the better.
- the C content is preferably limited to 0.005% or less.
- the preferable upper limit of the C content is 0.004% or less, and more preferably 0.003% or less. Since the lower the C, the more preferable, the lower limit includes 0%. However, if C is attempted to be reduced to less than 0.0001%, the manufacturing cost increases significantly. Therefore, 0.0001% is a practical lower limit in manufacturing. is there.
- N 0.005% or less N (nitrogen) forms a compound in the base steel sheet and deteriorates the iron loss, so the smaller the amount, the better.
- the N content is preferably limited to 0.005% or less.
- the preferable upper limit of the N content is 0.004% or less, and more preferably 0.003% or less. Since the smaller N is, the more preferable, the lower limit may be 0%.
- Total amount of S and Se 0.005% or less S (sulfur) and Se (selenium) form a compound in the base steel sheet and deteriorate iron loss, so the smaller the amount, the better. It is preferable to limit one or both of S and Se to 0.005% or less.
- the total amount of S and Se is preferably 0.004% or less, more preferably 0.003% or less. The lower the content of S or Se, the better. Therefore, the lower limits may be 0%.
- Acid-soluble Al 0.005% or less Acid-soluble Al (acid-soluble aluminum) forms a compound in the base steel sheet and deteriorates iron loss, so the smaller the amount, the better.
- the acid-soluble Al content is preferably 0.005% or less.
- the acid-soluble Al content is preferably 0.004% or less, more preferably 0.003% or less. The lower the amount of acid-soluble Al, the better, so the lower limit may be 0%.
- the balance of the composition of the base steel sheet described above consists of Fe and impurities.
- impurities refer to those that are mixed in from the ore as raw material, scrap, or the manufacturing environment when steel is industrially manufactured.
- the content of the above-mentioned selective element may be, for example, as follows.
- the lower limit of the selection element is not particularly limited, and the lower limit may be 0%. Even if these selective elements are contained as impurities, the effect of the grain-oriented electrical steel sheet according to the present embodiment is not impaired.
- Mn 0% or more and 1.00% or less
- Bi 0% or more and 0.010% or less
- B 0% or more and 0.008% or less
- Ti 0% or more and 0.015% or less
- Nb 0% or more and 0.20% or less
- V 0% or more and 0.15% or less
- Sn 0% or more and 0.30% or less
- Sb 0% or more and 0.30% or less
- Cr 0% or more and 0.30% or less
- Cu 0% or more and 0.40% or less
- P 0% or more and 0.50% or less
- Ni 0% or more and 1.00% or less
- Mo 0% or more and 0.10% or less.
- the chemical composition of the base steel sheet described above may be measured by a general analysis method.
- the steel composition may be measured using ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry).
- C and S may be measured by the combustion-infrared absorption method
- N may be measured by the inert gas melting-thermal conductivity method
- O may be measured by the inert gas melting-non-dispersion infrared absorption method.
- the base material steel sheet of the grain-oriented electrical steel sheet according to the present embodiment preferably has a crystal grain texture developed in the ⁇ 110 ⁇ 001> orientation.
- the ⁇ 110 ⁇ 001> orientation means a crystal orientation (Goss orientation) in which ⁇ 110 ⁇ planes are aligned parallel to the steel sheet surface and ⁇ 100> axes are aligned in the rolling direction.
- the magnetic properties are preferably improved by controlling the crystal orientation of the base steel sheet to the Goss orientation.
- the texture of the base steel sheet may be measured by a general analysis method. For example, it may be measured by an X-ray diffraction method (Laue method).
- Each layer of the grain-oriented electrical steel sheet according to this embodiment is observed and measured as follows.
- the base material steel sheet, the intermediate layer, and the insulating film are specified as follows based on the observation result of the COMPO image and the quantitative analysis result of SEM-EDS. That is, it is a region in which the Fe content is 80 atomic% or more and the O content is less than 30 atomic% excluding measurement noise, and the line segment (thickness) on the scanning line of the line analysis corresponding to this area is 300 nm. If the above is the case, this region is determined to be the base material steel plate, and the region excluding this base material steel plate is determined to be the intermediate layer and insulating film.
- the region excluding the base metal steel plate specified above there is a region where the P content is 5 atom% or more and the O content is 30 atom% or more, excluding the measurement noise, and corresponding to this region If the line segment (thickness) on the scanning line of the line analysis is 300 nm or more, this region is determined to be an insulating film.
- the region that is the above-mentioned insulating film do not include the precipitates and inclusions contained in the film as a judgment target, and select the region that satisfies the above quantitative analysis results as the matrix phase. It is determined that For example, if it is confirmed from the COMPO image or the line analysis result that precipitates or inclusions are present on the scanning line of the line analysis, this region is not taken into consideration and the determination is made based on the quantitative analysis result as the matrix.
- the precipitates and inclusions can be distinguished from the parent phase by the contrast in the COMPO image, and can be distinguished from the parent phase by the abundance of the constituent elements in the quantitative analysis result.
- this region is the intermediate layer.
- This intermediate layer has a Si content of 20 atom% or more on average and an O content of 30 atom on average as the average of the whole (for example, the arithmetic average of atom% of each element measured at each measurement point on the scanning line). % Or more should be satisfied.
- the quantitative analysis result of the intermediate layer is a quantitative analysis result of the mother phase, which does not include the analytical results of precipitates and inclusions contained in the intermediate layer.
- the total content of Fe, Cr, P and O is 70 atomic% or more and the Si content is less than 10 atomic% excluding measurement noise.
- the area is determined to be a deposit.
- the crystal structure can be specified from the electron diffraction pattern as described above.
- M 2 P 2 O 7 may exist in the conventional insulating film, this M 2 P 2 O 7 (M is at least one of Fe and Cr, or both) is subjected to electron diffraction.
- the crystal structure can be specified and discriminated from the pattern.
- the above-mentioned COMPO image observation and SEM-EDS quantitative analysis are performed to identify each layer and measure the thickness at five or more locations while changing the observation visual field.
- the arithmetic mean value is obtained from the values excluding the maximum and minimum values, and this average value is taken as the thickness of each layer.
- the average value is obtained by measuring the thickness at a position where it can be determined that the oxide film is an external oxidation region and not an internal oxidation region while observing the morphology of the structure. In the strain region, the average thickness of the intermediate layer and the average thickness of the insulating film can be calculated by the same method.
- the corresponding layer is observed in detail by TEM. Then, the layer is identified and the thickness is measured by TEM.
- a test piece including a layer to be observed in detail using a TEM is cut by FIB (Focused Ion Beam) processing so that the cutting direction is parallel to the plate thickness direction (specifically, cutting is performed).
- FIB Flucused Ion Beam
- each layer is specified and the thickness of each layer is measured.
- the method of identifying each layer and the method of measuring the thickness of each layer using TEM may be performed according to the method using SEM described above.
- the area where the Fe content is 80 atomic% or more excluding the measurement noise and the O content is less than 30 atomic% is determined to be the base material steel sheet, and the area excluding the base material steel sheet is set to the intermediate Judge as a layer and insulating film.
- the areas where the P content is 5 atomic% or more and the O content is 30 atomic% or more are determined to be insulating films, excluding measurement noise.
- the precipitates and inclusions contained in the insulating film are not included in the judgment, and the area that satisfies the above quantitative analysis results as the matrix phase is isolated.
- the intermediate layer may have an average Si content of 20 atom% or more and an O content of 30 atom% or more on average as a whole of the intermediate layer.
- the above-mentioned quantitative analysis result of the intermediate layer does not include the analysis result of precipitates and inclusions contained in the intermediate layer, and is the quantitative analysis result of the mother phase.
- the total content of Fe, Cr, P and O is 70 atomic% or more and the Si content is less than 10 atomic% excluding measurement noise.
- the area is determined to be a deposit.
- the crystal structure of the precipitate can be specified from the electron diffraction pattern.
- the observation/measurement with the above-mentioned TEM was carried out at 5 or more places with different observation fields of view, and the arithmetic mean value was calculated from the values excluding the maximum and minimum values among the measurement results obtained at 5 or more places in total. , This average value is adopted as the average thickness of the corresponding layer. In the strain region, the average thickness of the intermediate layer and the average thickness of the insulating film can be calculated by the same method.
- the contents of Fe, P, Si, OCr, etc. contained in the base material steel sheet, the intermediate layer, and the insulating coating are determined by determining the base material steel sheet, the intermediate layer, and the insulating coating to obtain the thickness thereof. Is the criterion of judgment.
- a bending adhesion test can be performed and evaluated. Specifically, a flat plate-shaped test piece of 80 mm ⁇ 80 mm is wound around a round bar having a diameter of 20 mm and then flattened. Then, measure the area of the insulating coating that has not peeled from this electromagnetic steel sheet, and define the value obtained by dividing the area that has not peeled by the area of the steel sheet as the coating residual area ratio (%) to determine the coating adhesion of the insulating coating. Evaluate. For example, it may be calculated by placing a transparent film with a 1 mm grid scale on a test piece and measuring the area of the insulating film that has not peeled off.
- the iron loss (W 17/50 ) of the grain- oriented electrical steel sheet is measured under the conditions of an AC frequency of 50 Hertz and an induced magnetic flux density of 1.7 Tesla.
- Example 1 The raw material billets having the component compositions shown in Table 1 were soaked at 1150° C. for 60 minutes and then subjected to hot rolling to obtain hot rolled steel sheets having a thickness of 2.3 mm. Next, this hot rolled steel sheet was held at 1120° C. for 200 seconds, immediately cooled, held at 900° C. for 120 seconds, and then rapidly cooled to perform hot rolled sheet annealing. The hot rolled annealed sheet after the hot rolled sheet annealing was pickled and then subjected to cold rolling to obtain a cold rolled steel sheet having a final sheet thickness of 0.23 mm.
- This cold-rolled steel sheet (hereinafter referred to as “steel sheet”) was subjected to decarburization annealing at 850° C. for 180 seconds in an atmosphere of hydrogen:nitrogen of 75%:25%.
- the decarburization-annealed steel sheet was subjected to nitriding annealing at 750° C. for 30 seconds in a mixed atmosphere of hydrogen, nitrogen, and ammonia to adjust the nitrogen content of the steel sheet to 230 ppm.
- the annealing separator containing alumina as a main component is applied to the steel sheet after nitriding annealing, and then the steel sheet is heated to 1200° C. at a temperature rising rate of 10° C./hour in a mixed atmosphere of hydrogen and nitrogen for finish annealing. gave. Then, in a hydrogen atmosphere, the steel sheet was subjected to purification annealing in which the steel sheet was kept at 1200° C. for 20 hours. Then, the steel sheet was naturally cooled to produce a base material steel sheet having a smooth surface.
- an intermediate layer was formed under the conditions shown in Table 2.
- a solution containing phosphate and colloidal silica as a main component was applied on the surface of the base material steel sheet on which the intermediate layer was formed under the conditions shown in Table 2, and an insulating film was formed under the conditions shown in Table 2.
- the "temperature of the central portion of the strain region” means the temperature of the central portion of the strain region in the rolling direction of the base steel sheet and the extending direction of the strain region.
- a grain-oriented electrical steel sheet having no forsterite coating and having a strain region formed in the base steel sheet good adhesion of the insulating coating can be secured, and a good iron loss reduction effect can be obtained.
- a method for manufacturing a grain-oriented electrical steel sheet can be provided. Therefore, the industrial availability is high.
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Abstract
Description
本願は、2019年1月16日に日本に出願された特願2019-005059号に基づき優先権を主張し、その内容をここに援用する。
(3)上記(1)または(2)に記載の方向性電磁鋼板の製造方法において、歪領域形成工程では、電子ビームの照射条件が、加速電圧:50kV以上350kV以下、ビーム電流:0.3mA以上50mA以下、ビーム照射径:10μm以上500μm以下、照射間隔:3mm以上20mm以下、スキャン速度:5m/秒以上80m/秒以下、であってもよい。
(4)上記(1)から(3)のいずれか一つに記載の方向性電磁鋼板の製造方法において、母材鋼板上に中間層を形成する中間層形成工程をさらに備え、中間層形成工程では、焼鈍温度:500℃以上1500℃以下、保持時間:10秒以上600秒以下、露点:-20℃以上5℃以下、に調整された焼鈍条件で母材鋼板に熱処理を施して中間層を形成してもよい。
(5)上記(1)から(4)のいずれか一つに記載の方向性電磁鋼板の製造方法において、中間層が形成された母材鋼板に、絶縁皮膜を形成する絶縁皮膜形成工程をさらに備え、絶縁皮膜形成工程では、絶縁皮膜形成用溶液を塗布量2g/m2~10g/m2で母材鋼板の表面に塗布し、絶縁皮膜形成用溶液が塗布された母材鋼板を3秒~300秒放置し、絶縁皮膜形成用溶液が塗布された母材鋼板を、水素および窒素を含有しかつ酸化度PH2O/PH2が0.001以上0.3以下に調整された雰囲気ガス中で、昇温速度5℃/秒以上30℃秒以下で加熱し、加熱された母材鋼板を、水素および窒素を含有しかつ酸化度PH2O/PH2が0.001以上0.3以下に調整された雰囲気ガス中で、300℃以上950℃以下の温度範囲で、10秒以上300秒以下で均熱し、均熱された母材鋼板を、水素および窒素を含有しかつ酸化度PH2O/PH2が0.001以上0.05以下に制御された雰囲気ガス中で、冷却速度5℃/秒以上50℃秒以下で、500℃まで冷却してもよい。
また、本発明者らは、上記のような特定の照射条件を満たさない場合、磁区の幅を狭く制御できたとしても、絶縁皮膜中に空隙が発生し、絶縁皮膜の密着性が劣化することも見出した。
また、以下の実施形態において、「~」を用いて表される数値限定範囲は、「~」の前後に記載される数値を下限値及び上限値として含む範囲を意味する。「超」または「未満」と示す数値は、その値が数値範囲に含まれない。
以下に、本発明に係る方向性電磁鋼板の製造方法について説明する。なお、本実施形態に係る方向性電磁鋼板の製造方法は、下記の方法に限定されない。下記の製造方法は、本実施形態に係る方向性電磁鋼板を製造するための一つの例である。
本実施形態に係る方向性電磁鋼板は、仕上げ焼鈍時にフォルステライト皮膜の生成が抑制された又は仕上げ焼鈍後にフォルステライト皮膜が除去された母材鋼板を出発材料として、この母材鋼板に対して、中間層を形成し、絶縁皮膜を形成し、歪領域を形成して製造すればよい。
本実施形態に係る方向性電磁鋼板の製造方法の歪領域形成工程では、圧延方向および歪領域の伸びる方向における歪領域の中央部の温度が800℃以上2000℃以下に加熱される。
(a)仕上げ焼鈍で生成したフォルステライト等の無機鉱物質の皮膜を、酸洗、研削等の手段で除去した母材鋼板を焼鈍し、又は、
(b)仕上げ焼鈍で上記無機鉱物質の皮膜の生成を抑制した母材鋼板を焼鈍し、
(c)熱酸化焼鈍、すなわち露点を制御した雰囲気下での焼鈍によって、母材鋼板の表面上に中間層を形成し、
(d)この中間層上に、燐酸塩とコロイド状シリカを主体とする絶縁皮膜形成用溶液を塗布して焼付ける。
上記の製造方法によって、母材鋼板と前記母材鋼板上に接して配された中間層と、中間層上に接して配されかつ最表面となる絶縁皮膜とを有する方向性電磁鋼板を製造することができる。
Siを0.8~7.0質量%含有する珪素鋼片を、好ましくはSiを2.0~7.0質量%含有する珪素鋼片を、熱間圧延し、熱間圧延後の鋼板に必要に応じて焼鈍を施し、その後、焼鈍後の鋼板に1回又は中間焼鈍を挟む2回以上の冷間圧延を施して、最終板厚の鋼板に仕上げる。次いで、最終板厚の鋼板に、脱炭焼鈍を施すことで、脱炭に加え、一次再結晶を進行させるとともに、鋼板表面に酸化層を形成する。
次いで、母材鋼板の表面に、絶縁皮膜形成用溶液を塗布量2g/m2~10g/m2で塗布し、絶縁皮膜形成用溶液が塗布された母材鋼板を3秒~300秒放置する。
この条件で均熱された母材鋼板を、水素および窒素を含有しかつ酸化度PH2O/PH2が0.001以上0.05以下に制御された雰囲気ガス中で、冷却速度5℃/秒以上50℃秒以下で、500℃まで冷却する。
加熱~冷却における雰囲気の酸化度が上記で示した下限値未満であると、中間層が薄くなってしまう場合がある。また、上記で示した上限値を超えると中間層が厚くなってしまう場合がある。
また、冷却時の冷却速度が5℃/秒未満であると生産性が低下してしまう場合がある。また、冷却速度が50℃/秒超であると絶縁皮膜中に多くの空隙が発生してしまう場合がある。
したがって、圧延方向における歪領域の中央部及び歪領域の伸びる方向における歪領域の中央部の双方に該当する領域が800℃以上2000℃以下に加熱される。
ここで、圧延方向および歪領域の伸びる方向における歪領域の中央部の温度を800℃以上2000℃以下に加熱するために、歪領域形成工程では、加速電圧:50kV以上350kV以下、ビーム電流:0.3mA以上50mA以下、ビーム照射径:10μm以上500μm以下、照射間隔:3mm以上20mm以下、スキャン速度:5m/秒以上80m/秒以下の条件で、電子ビームが照射されることが好ましい。電子ビームは、高加速電圧化による皮膜損傷の抑制効果や、高速でビーム制御ができるなどの特徴があるため、電子ビームを用いることが好ましい。
歪領域形成工程では、圧延方向および歪領域の伸びる方向における歪領域の中央部の温度が800℃以上1500℃以下に加熱されてもよい。
電子ビームの加速電圧は高い方が好ましい。電子ビームの加速電圧が高いほど、電子ビームの物質透過性が高まり、電子ビームが絶縁皮膜を透過しやすくなる。そのため、絶縁皮膜の損傷が抑制される。また、加速電圧が高いとビーム径を小さくしやすいという利点がある。以上の効果を得るために、加速電圧を50kV以上とすることが好ましい。なお、加速電圧は70kV以上とすることが好ましく、100kV以上とすることがより好ましい。
一方、設備コスト抑制の観点から、加速電圧は350kV以下とすることが好ましい。なお、加速電圧は300kV以下とすることが好ましく、250kV以下とすることがより好ましい。
ビーム電流は、ビーム径縮小の観点からは小さい方が好ましい。ビーム電流が大きすぎるとビームを収束させることが困難となる可能性があるため、ビーム電流を50mA以下とすることが好ましい。なお、ビーム電流は30mA以下とすることがより好ましい。ビーム電流が小さすぎると、十分な磁区細分化効果を得るために必要な歪を形成することができない可能性があるため、ビーム電流を0.3mA以上とすることが好ましい。なお、ビーム電流は0.5mA以上とすることがより好ましく、1mA以上とすることがさらに好ましい。
ビームの走査方向と直交する方向におけるビーム照射径は、小さいほど単板鉄損の向上に有利である。電子ビームの走査方向と直交する方向におけるビーム照射径を500μm以下とすることが好ましい。ここで、本実施形態では、ビーム照射径を、スリット法(幅0.03mmのスリットを使用)によって測定したビームプロファイルの半値幅と定義する。なお、走査方向と直交する方向におけるビーム照射径は、400μm以下とすることが好ましく、300μm以下とすることがより好ましい。
走査方向と直交する方向におけるビーム照射径の下限は特に限定されないが、10μm以上とすることが好ましい。電子ビームの走査方向と直交する方向におけるビーム照射径が10μm以上であれば、1つの電子ビーム源によって広い範囲に対し照射を行うことが可能である。なお、走査方向と直交する方向におけるビーム照射径は、30μm以上とすることが好ましく、100μm以上とすることがより好ましい。
また、照射間隔が3mm以上20mm以下であることにより、磁区細分化による渦電流損の低減とヒステリシス損の増加抑制とのバランスによる鉄損低減という効果が得られる。照射間隔とは、母材鋼板の圧延方向に沿った、電子ビームを照射する距離であり、圧延方向における歪領域の間隔である。
さらに、スキャン速度が5m/秒以上80m/秒以下であることにより、磁区細分化効果と生産性向上とが両立できる。
ビームのスキャン速度は5m/秒以上とすることが好ましい。ここで、スキャン速度とは、各歪領域を形成する際の電子ビームの照射開始地点から照射終了地点までの距離を当該地点間のスキャンに要した時間で除することで得られるスキャン速度、すなわち平均スキャン速度である。例えば、電子ビームの照射開始地点及び照射終了地点が鋼板の幅方向の両端部となる場合、スキャン速度は、鋼板の幅端部から、もう一方の幅端部へビームを走査しながら照射する間の、平均スキャン速度(鋼板の幅端部間の距離を当該幅端部間の走査に要した時間で除した速度)となる。スキャン速度が5m/秒より小さいと、処理時間が長くなり、生産性が低下する可能性がある。走査速度は、45m/秒以上とすることがより好ましい。
本実施形態に係る方向性電磁鋼板は、母材鋼板と、母材鋼板上に接して配された中間層と、中間層上に接して配された絶縁皮膜とを有する。
本実施形態に係る方向性電磁鋼板は、母材鋼板の表面に圧延方向と交差する方向に延びる歪領域を有し、圧延方向および板厚方向と平行な面の断面視で、歪領域上の絶縁皮膜中にM2P4O13が存在する。Mは、Fe又はCrの少なくとも一方、あるいは双方を意味する。
ここで、フォルステライト皮膜のない方向性電磁鋼板とは、フォルステライト皮膜を製造後に除去して製造した方向性電磁鋼板、又は、フォルステライト皮膜の生成を抑制して製造した方向性電磁鋼板である。
本実施形態において、圧延方向と交差する方向とは、圧延方向に対して母材鋼板の表面に平行かつ直角な方向(以下、単に「圧延方向に対して直角な方向」とも称する)から母材鋼板の表面に平行に時計回り方向または反時計回り方向に45°以内の傾きの範囲にある方向を意味する。歪領域は母材鋼板の表面に形成されるため、歪領域は、母材鋼板の表面上の圧延方向および板厚方向に対して直角な方向から、母材鋼板の板面において45°以内の傾きの方向に延在する。
基材である母材鋼板は、母材鋼板の表面において結晶方位がゴス方位に制御された結晶粒集合組織を有する。母材鋼板の表面粗度は、特に制限されないが、母材鋼板に大きい張力を付与して鉄損の低減を図る点で、算術平均粗さ(Ra)で0.5μm以下が好ましく、0.3μm以下がより好ましい。なお、母材鋼板の算術平均粗さ(Ra)の下限は、特に制限されないが、0.1μm以下では鉄損改善効果が飽和してくるので下限を0.1μmとしてもよい。
中間層は、母材鋼板上に接して配され(すなわち、母材鋼板の表面に形成され)、母材鋼板と絶縁皮膜とを密着させる機能を有する。中間層は、母材鋼板の表面上に連続して広がっている。中間層が母材鋼板と絶縁皮膜との間に形成されることで、母材鋼板と絶縁皮膜との密着性が向上して、母材鋼板に応力が付与される。
このような構成とすることで、歪領域においても絶縁皮膜の密着性を良好に保つことができる。
具体的には、次に説明する手法で、歪領域の中間層の平均厚さ、ならびに歪領域以外の中間層の平均厚さを測定することができる。
定量分析する元素は、Fe、Cr、P、Si、Oの5元素とする。以下に説明する「原子%」とは、原子%の絶対値ではなく、これらの5元素に対応するX線強度を基に計算した相対値である。
また、TEM-EDSで測定される上記相対値は、日本電子株式会社製の透過電子顕微鏡(JEM-2100F)および日本電子株式会社製のエネルギー分散型X線分析装置(JED-2300T)で線分析を行い、その結果を日本電子株式会社製のEDSデータ用ソフト(Analysis Station)に入力して計算した場合の具体的数値であるものとする。もちろん、SEM-EDS、TEM-EDSでの測定は以下に示す例に限られない。
絶縁皮膜は、燐酸塩とコロイド状シリカ(SiO2)を主体とする溶液を中間層の表面に塗布して焼付けて形成されるガラス質の絶縁皮膜である。あるいは、アルミナゾルとホウ酸とを主体とする溶液を塗布して焼付けて絶縁皮膜を形成してもよい。
この絶縁皮膜は、母材鋼板に高い面張力を付与することができる。絶縁皮膜は、例えば方向性電磁鋼板の最表面を構成する。
図3および図4を用いて、母材鋼板に形成された歪領域の説明をする。
図3は、圧延方向および板厚方向と平行な面の断面を示す模式的な図であり、母材鋼板1の表面に形成された歪領域Dを含む図である。図3に示すように、母材鋼板1上に接して中間層4が配され、中間層4上に接して絶縁皮膜3が配され、母材鋼板1の表面に歪領域Dが形成されている。なお、中間層4は他の層に比べて厚さが小さいため、図3においては、中間層4は線で表現されている。
なお、圧延方向において、歪領域の中心と歪領域の中央部の中心の位置が一致することがより好ましい。
図4に示す例では、歪領域Dの中央部Cの絶縁皮膜3中にM2P4O13の析出物が存在する。図4では、この析出物を領域5としている。また、図4の領域5の周辺では、非晶質燐酸化物の析出物を含む領域6が存在する。絶縁皮膜3において、領域5と領域6を除く領域は絶縁皮膜の母相7やボイド8を含む。
領域6は絶縁皮膜3の表面近傍に形成される場合もある。
この同定は、ICDD(International Centre for Diffraction Data)のPDF(Powder Diffraction File)を用いて行えばよい。具体的には、析出物がM2P4O13の場合、PDF:01-084-1956の回折パターンが現れ、析出物が従来の絶縁皮膜に存在するM2P2O7の場合、PDF:00-048-0598の回折パターンが現れる。また、析出物が非晶質燐酸化物の場合、回折パターンはハローパターンとなる。
このような構成とすることで、ボイドを起点とした絶縁皮膜の剥離が抑制され、絶縁皮膜の密着性が向上するという効果が得られる。
ここで、図5の例では、ボイド8の長さLdの合計ΣLdは、ΣLd=L1+L2+L3+L4である。図5に示すように、板厚方向にボイド8が重なる場合、重なるボイドの長さLdから重なった部分の長さを引いたものをボイドの長さとする。図5において、板厚方向に沿って見たときに重なる2つのボイド8の長さは、重なり合う長さを引いたL4とする。
なお、画像解析を行うための画像の二値化は、上記したボイドの判別結果に基づき、組織写真に対して手作業で空隙の色付けを行って画像を二値化してもよい。
このような構成とすることで、磁区細分化効果が安定して得られるという効果が得られる。
面積率は、好ましくは、20%以上であり、より好ましくは30%以上である。面積率は、好ましくは50%以下であり、より好ましくは40%以下である。このような構成とすることで、絶縁皮膜の密着性が向上するという効果が得られる。
非晶質燐酸化物領域の面積率が1%以上であることで、絶縁皮膜中の局所応力が緩和される。また、非晶質燐酸化物領域の面積率が60%以下であることで絶縁皮膜の張力を低下させないという効果が得られる。
非晶質燐酸化物領域の面積率は、より好ましくは5%以上であり、非晶質燐酸化物領域の面積率は、より好ましくは40%以下である。中央部の絶縁皮膜中の非晶質燐酸化物領域の面積率は、中央部の絶縁皮膜中のM2P4O13の面積率と同様の方法で測定することができる。
以下、素材鋼片および母材鋼板の成分組成に係る%は、素材鋼片または母材鋼板の総質量に対する質量%を意味する。
本実施形態に係る方向性電磁鋼板の母材鋼板は、例えば、Si:0.8~7.0%を含有し、C:0.005%以下、N:0.005%以下、SおよびSeの合計量:0.005%以下、ならびに酸可溶性Al:0.005%以下に制限し、残部がFeおよび不純物からなる。
Si(シリコン)は、方向性電磁鋼板の電気抵抗を高めて鉄損を低下させる。Si含有量の好ましい下限は0.8%以上であり、さらに好ましくは2.0%以上である。一方、Si含有量が7.0%を超えると、母材鋼板の飽和磁束密度が低下するため、鉄心の小型化が難くなる可能性がある。このため、Si含有量の好ましい上限は7.0%以下である。
C(炭素)は、母材鋼板中で化合物を形成し、鉄損を劣化させるため、少ないほど好ましい。C含有量は、0.005%以下に制限することが好ましい。C含有量の好ましい上限は0.004%以下であり、さらに好ましくは0.003%以下である。Cは少ないほど好ましいので、下限は0%を含むが、Cを0.0001%未満に低減しようとすると、製造コストが大幅に上昇するので、製造上、0.0001%が実質的な下限である。
N(窒素)は、母材鋼板中で化合物を形成し、鉄損を劣化させるため、少ないほど好ましい。N含有量は、0.005%以下に制限することが好ましい。N含有量の好ましい上限は0.004%以下であり、さらに好ましくは0.003%以下である。Nは少ないほど好ましいので、下限が0%であればよい。
S(硫黄)およびSe(セレン)は、母材鋼板中で化合物を形成し、鉄損を劣化させるため、少ないほど好ましい。SまたはSeの一方、または両方の合計を0.005%以下に制限することが好ましい。SおよびSeの合計量は、0.004%以下が好ましく、0.003%以下がさらに好ましい。SまたはSeの含有量は少ないほど好ましいので、下限がそれぞれ0%であればよい。
酸可溶性Al(酸可溶性アルミニウム)は、母材鋼板中で化合物を形成し、鉄損を劣化させるため、少ないほど好ましい。酸可溶性Alは、0.005%以下であることが好ましい。酸可溶性Alは、0.004%以下が好ましく、0.003%以下がさらに好ましい。酸可溶性Alは少ないほど好ましいので、下限が0%であればよい。
Mn:0%以上かつ1.00%以下、
Bi:0%以上かつ0.010%以下、
B:0%以上かつ0.008%以下、
Ti:0%以上かつ0.015%以下、
Nb:0%以上かつ0.20%以下、
V:0%以上かつ0.15%以下、
Sn:0%以上かつ0.30%以下、
Sb:0%以上かつ0.30%以下、
Cr:0%以上かつ0.30%以下、
Cu:0%以上かつ0.40%以下、
P:0%以上かつ0.50%以下、
Ni:0%以上かつ1.00%以下、および
Mo:0%以上かつ0.10%以下。
母材鋼板の集合組織は、一般的な分析方法によって測定すればよい。例えば、X線回折法(ラウエ法)により測定すればよい。ラウエ法とは、鋼板にX線ビームを垂直に照射して、透過または反射した回折斑点を解析する方法である。回折斑点を解析することによって、X線ビームを照射した場所の結晶方位を同定することができる。照射位置を変えて複数箇所で回折斑点の解析を行えば、各照射位置の結晶方位分布を測定することができる。ラウエ法は、粗大な結晶粒を有する金属組織の結晶方位を測定するのに適した手法である。
定量分析する元素は、Fe、Cr、P、Si、Oの5元素とする。以下に説明する「原子%」とは、原子%の絶対値ではなく、これらの5元素に対応するX線強度を基に計算した相対値である。以下では、上述した装置などを用いてこの相対値を計算した場合の具体的数値を示す。
なお、歪領域においても同様の手法で中間層の平均厚さ、および絶縁皮膜の平均厚さを算出することができる。
本発明は、本発明の要旨を逸脱せず、本発明の目的を達成する限りにおいて、種々の条件を採用し得るものである。
表1に示す成分組成の素材鋼片を1150℃で60分均熱してから熱間圧延に供し、2.3mm厚の熱延鋼板とした。次いで、この熱延鋼板を1120℃で200秒保持した後、直ちに冷却して、900℃で120秒保持し、その後に急冷する熱延板焼鈍を行った。熱延板焼鈍後の熱延焼鈍板を酸洗後、冷間圧延に供し、最終板厚0.23mmの冷延鋼板とした。
中間層が形成された母材鋼板の表面に、燐酸塩とコロイド状シリカを主体とする溶液を表2に示す条件で塗布し、表2に示す条件で絶縁皮膜を形成した。
表4からわかるように、本発明の製造方法で作製した方向性電磁鋼板は密着性が良好である。
表4からわかるように、本発明の製造方法で作製した方向性電磁鋼板は、鉄損が低減されている。
2 フォルステライト皮膜
3 絶縁皮膜
4 中間層
5 M2P4O13の析出物を含む領域
6 非晶質燐酸化物の析出物を含む領域
7 絶縁皮膜の母相
8 ボイド
Claims (5)
- 方向性電磁鋼板の製造方法であって、
母材鋼板と、前記母材鋼板上に接して配された中間層と、前記中間層上に接して配された絶縁皮膜とを有する方向性電磁鋼板に電子ビームを照射して、前記母材鋼板の表面に前記母材鋼板の圧延方向と交差する方向に延びる歪領域を形成する歪領域形成工程を備え、
前記歪領域形成工程では、前記母材鋼板の圧延方向および前記歪領域の伸びる方向における前記歪領域の中央部の温度が800℃以上2000℃以下に加熱される
ことを特徴とする方向性電磁鋼板の製造方法。 - 前記歪領域形成工程では、前記母材鋼板の圧延方向および前記歪領域の伸びる方向における前記歪領域の中央部の温度が800℃以上1500℃以下に加熱される
ことを特徴とする請求項1に記載の方向性電磁鋼板の製造方法。 - 前記歪領域形成工程では、電子ビームの照射条件が、
加速電圧:50kV以上350kV以下、
ビーム電流:0.3mA以上50mA以下、
ビーム照射径:10μm以上500μm以下、
照射間隔:3mm以上20mm以下、
スキャン速度:5m/秒以上80m/秒以下、
であることを特徴とする請求項1または2に記載の方向性電磁鋼板の製造方法。 - 前記母材鋼板上に前記中間層を形成する中間層形成工程をさらに備え、中間層形成工程では、
焼鈍温度:500℃以上1500℃以下、
保持時間:10秒以上600秒以下、
露点:-20℃以上5℃以下、
に調整された焼鈍条件で前記母材鋼板に熱処理を施して中間層を形成する
ことを特徴とする請求項1から3のいずれか一項に記載の方向性電磁鋼板の製造方法。 - 前記中間層が形成された前記母材鋼板に、前記絶縁皮膜を形成する絶縁皮膜形成工程をさらに備え、絶縁皮膜形成工程では、
絶縁皮膜形成用溶液を塗布量2g/m2~10g/m2で前記母材鋼板の表面に塗布し、
前記絶縁皮膜形成用溶液が塗布された母材鋼板を3秒~300秒放置し、
前記絶縁皮膜形成用溶液が塗布された母材鋼板を、水素および窒素を含有しかつ酸化度PH2O/PH2が0.001以上0.3以下に調整された雰囲気ガス中で、昇温速度5℃/秒以上30℃秒以下で加熱し、
加熱された前記母材鋼板を、水素および窒素を含有しかつ酸化度PH2O/PH2が0.001以上0.3以下に調整された雰囲気ガス中で、300℃以上950℃以下の温度範囲で、10秒以上300秒以下で均熱し、
均熱された前記母材鋼板を、水素および窒素を含有しかつ酸化度PH2O/PH2が0.001以上0.05以下に制御された雰囲気ガス中で、冷却速度5℃/秒以上50℃秒以下で、500℃まで冷却する
ことを特徴とする請求項1から4のいずれか一項に記載の方向性電磁鋼板の製造方法。
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