WO2020158893A1 - 方向性電磁鋼板およびそれを用いた鉄心 - Google Patents
方向性電磁鋼板およびそれを用いた鉄心 Download PDFInfo
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Definitions
- the present invention relates to a grain-oriented electrical steel sheet suitable as an iron core material for a transformer.
- Oriented electrical steel sheet is a soft magnetic material used as an iron core material for transformers, and has a crystal structure in which the ⁇ 001> orientation, which is the easy axis of iron magnetization, is highly aligned with the rolling direction of the steel sheet.
- Such a texture is a secondary grain that preferentially grows large grains of ⁇ 110 ⁇ 001> orientation, which is called Goss orientation, during the purification annealing during the manufacturing process of grain-oriented electrical steel sheet. It is formed through a phenomenon called recrystallization.
- this formation method it is used as a general technique to secondarily recrystallize grains having a Goss orientation during purification annealing using precipitates called inhibitors.
- a method using AlN and MnS described in Patent Document 1 and a method using MnS and MnSe described in Patent Document 2 are disclosed and put to practical use industrially.
- the method using these inhibitors is a method that is useful for stably developing secondary recrystallized grains, but in order to finely disperse the inhibitor in the steel, slab heating is performed at a high temperature of 1300°C or higher, It was necessary to dissolve the inhibitor component once.
- Patent Document 3 and the like disclose a technique for developing Goss-oriented crystal grains by secondary recrystallization in a material containing no inhibitor component. By removing impurities such as inhibitor components as much as possible, this technique reveals the grain boundary misorientation angle dependence of the grain boundary energy of the crystal grain boundaries during primary recrystallization, making Goss orientation possible without the use of inhibitors.
- This is a technique for secondary recrystallizing grains having a grain, and the effect is called a texture inhibition effect. Since this method does not require fine dispersion of the inhibitor in the steel, it does not require high-temperature slab heating, which was indispensable until then, and is a method that offers great advantages in terms of cost and maintenance.
- the grain-oriented electrical steel sheet is mainly used as an iron core of a transformer, and therefore is required to have excellent magnetization characteristics, and particularly to have low iron loss.
- it is important to make secondary recrystallized grains in the steel sheet highly aligned 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 highly aligned in the ⁇ 110 ⁇ 001> orientation
- Goth orientation secondary recrystallized grains in the steel sheet highly aligned in the ⁇ 110 ⁇ 001> orientation
- a technique for introducing non-uniformity into the surface of a steel sheet by a physical method to subdivide the width of magnetic domains to reduce iron loss that is, a magnetic domain subdivision technique has been developed.
- Patent Document 4 proposes a technique for reducing iron loss of a steel sheet by irradiating a final product sheet with a laser and introducing a high dislocation density region into a surface layer of the steel sheet to narrow a magnetic domain width.
- Patent Document 5 proposes a technique for controlling the magnetic domain width by irradiation with an electron beam.
- Japanese Patent Publication No. 40-15644 Japanese Patent Publication No. 51-13469 JP 2000-129356 A Japanese Examined Patent Publication No. 57-2252 Japanese Patent Publication No. 6-72266 Japanese Patent Publication No. 62-56923 Japanese Patent Laid-Open No. 10-17931 Japanese Patent No. 4106815
- the magnetic domain subdivision technology described above has a very high iron loss reduction effect and is often applied to the highest grade grain oriented electrical steel sheets with low iron loss.
- equipment introduction cost and running cost increase, so iron loss reduction methods that do not use these technologies are necessary from the viewpoint of cost reduction. It is said that.
- the present invention meets the above-mentioned demands, and an object of the present invention is to propose a grain-oriented electrical steel sheet capable of reducing iron loss without using a domain refinement technique.
- the inventors have generated a fine crystal grain in a fixed ratio in the final product plate, thereby making it possible to obtain the iron loss characteristics without applying the magnetic domain refinement treatment. It has been found that an excellent grain-oriented electrical steel sheet can be obtained.
- an annealing separator mainly composed of MgO was applied, and a secondary recrystallization annealing was performed in which the annealing was maintained at 1250°C for 10 hours in a hydrogen atmosphere, which also doubled as a purification annealing.
- the iron loss W 17/50 (iron loss when excited to 1.7 T at 50 Hz) of the sample cut from the product plate thus obtained was measured by the method described in JIS C 2550-1:2011.
- the sample was immersed in a 10% hydrochloric acid aqueous solution at 80°C for 180 seconds to remove the coating on the front and back surfaces so that secondary recrystallized grains could be confirmed. I asked.
- the area of the sample investigated to obtain this particle size distribution was 336 cm 2 (for 4 Epstein samples). Based on the obtained data, the result of investigation on the relationship between the iron loss and the number of crystal grains having a grain size of more than 2.0 mm and less than 5.0 mm (per 1 cm 2 ) is shown in FIG.
- the first point is that in the steel slab A containing Sb, the iron loss is good when the number of crystal grains having a grain size of more than 2.0 mm and less than 5.0 mm is 0.2 to 5 grains/cm 2 .
- the second point is that in the steel slab B that does not contain Sb, the number of crystal grains with a grain size of more than 2.0 mm and less than 5.0 mm is very small, less than 0.2 grains/cm 2 , and reduction of iron loss cannot be expected. is there.
- the base iron component of the product plate obtained in Experiment 1 is mass%, and the slab A-started one has Si: 3.33%, Mn: 0.15%, Sb: 0.08%, balance Fe and unavoidable impurities.
- the slab B-started material had Si: 3.27%, Mn: 0.15%, balance Fe and inevitable impurities. That is, in the product plate, due to decarburization and purification, C, Al, N, and S were almost absent, but the content of other components was the same as the content in the slab.
- the crystal orientation of the crystal grains having a grain size of more than 2.0 mm and less than 5.0 mm was investigated in detail by the EBSD (electron backscatter diffraction) method.
- EBSD electron backscatter diffraction
- the orientation was considerably different from the Goss orientation, which is the main orientation of the coarse secondary recrystallized grains with a grain size of 5.0 mm or more.
- the misorientation angle between the fine grain orientation and the Goss orientation was about 25° on average.
- the iron loss is good when Sb is contained in the components of the product plate and the number of fine particles having a particle size of more than 2.0 mm and less than 5.0 mm is 0.2 to 5 particles/cm 2.
- the inventors think as follows. In the first place, the magnitude of the iron loss of the grain-oriented electrical steel sheet is greatly influenced by the magnetic domain structure in the secondary recrystallized grains. Most of the secondary recrystallized grains of the grain-oriented electrical steel sheet are composed of 180° magnetic domains, which are almost parallel to the rolling direction. The width of the magnetic domain has a great influence on the iron loss characteristic, and the narrower the width, the more the iron loss can be reduced.
- a magnetic domain subdivision processing method for imparting mechanical linear grooves to a steel sheet.
- This method utilizes the magnetic characteristics that the magnetostatic energy in the cross section of the groove increases when the groove is formed, so that the increase in the energy is solved by narrowing the magnetic domain width.
- the magnetic domains are discontinuous at the grain boundaries between the fine grains and the coarse secondary recrystallized grains. May be.
- a magnetic pole may be generated and the magnetostatic energy may increase, and it is presumed that the magnetic domains are subdivided for the same reason as above. We believe that this may be the mechanism of iron loss reduction due to the fine particles.
- the iron loss reducing action may also be due to the large misorientation angle between the fine grains and the coarse secondary recrystallized grains. That is, it is expected that as the average of the azimuth difference angles deviates from the range of low tilt angle (azimuth difference angle less than 15°) in which the azimuth difference is judged to be small, the iron loss reducing effect becomes greater. Therefore, the average of the misorientation angle between the crystal orientation and the Goss orientation of the fine particles having a grain size of more than 2.0 mm and less than 5.0 mm is preferably 15° or more, more preferably 20° or more, and 25 More preferably, it is at least °.
- Steel slab A contains Sb, which is known as a segregating element.
- Sb which is known as a segregating element.
- This Sb by suppressing the grain boundary migration by segregating to the grain boundaries of the primary recrystallized grains in the initial stage of the secondary recrystallization, the primary recrystallized grains are suppressed from growing to the secondary recrystallized grains, As a result, it is estimated that fine particles were generated.
- segregation elements such as Sb are not contained in the steel, so grain boundary migration is not suppressed at the initial stage of secondary recrystallization, and fine secondary particles do not occur Is suspected to have occurred.
- Patent Document 6 and Patent Document 7 As a technique for reducing iron loss using fine particles, there are methods disclosed in Patent Document 6 and Patent Document 7, for example.
- these documents only disclose that fine particles having a particle size of 2 mm or less have a magnetic domain refining effect, and only disclose a method of controlling the fine particles, for fine particles having a particle size of more than 2 mm. Is not mentioned. Therefore, it is presumed that the iron loss reduction technology disclosed in those documents and the technology of the present invention are essentially different in technical idea, and that the grain size of crystal grains to be used and the control method thereof are also different.
- Experiment 2 The steel slab A used in Experiment 1 was subjected to slab heating for uniform heating at 1200° C. for 60 minutes and then hot-rolled to a thickness of 2.4 mm. Then, after hot-rolled sheet annealing was performed at 1000° C. for 30 seconds in a dry nitrogen atmosphere, the sheet was finished to a thickness of 0.23 mm by cold rolling. Then, in a dry nitrogen atmosphere, the temperature was raised to 700° C. at a heating rate of 750° C./s and immediately cooled to room temperature at an average of 70° C./s without soaking.
- the iron loss W 17/50 (iron loss when excited to 1.7 T at 50 Hz) of the sample cut from the product plate thus obtained was measured by the method described in JIS C 2550-1:2011. Further, the sample was immersed in a 10% aqueous hydrochloric acid solution at 80° C. for 180 seconds to remove the coating on the front and back surfaces to expose the secondary recrystallized grains.
- the grain thickness of the grain-oriented electrical steel sheet is generally about 0.2 to 0.5 mm, and grains having a grain size larger than that thickness are basically considered to penetrate in the thickness direction. That is, in the grain-oriented electrical steel sheet of the present invention, all coarse secondary recrystallized grains with a grain size of 5 mm or more that can be observed on the front and back surfaces of the steel sheet from which the coating has been removed should be regarded as "grains penetrating in the sheet thickness direction". You can The “area exposed on the steel sheet surface side” of one coarse secondary recrystallized grain means that the secondary recrystallized grain is exposed on the steel sheet when the crystal grain is observed on the surface side of the steel sheet.
- the area or its projection surface is shown as a solid line graphic.
- the "area exposed on the back surface side" of the secondary recrystallized grains is, similarly to the front surface side, observed when the crystal grains are observed on the back surface side of the steel sheet, of a portion surrounded by grain boundaries. Area.
- the area or its projection surface (orthographic projection of the area) is shown as a broken-line graphic.
- a region where their projection planes match means that the area exposed on the steel plate front surface side of the target secondary recrystallized grain and the area exposed on the steel plate back surface side are parallel to the plate surface (rolling surface). When projected as orthographic projections on one plane, these orthographic projections are overlapping (matching) portions. In FIG. 2, the area is indicated by a hatched portion.
- the area ratios of the areas where the projection surfaces coincide with the exposed areas of the coarse secondary recrystallized grains are The area of the crystal grains exposed on the front surface side of the steel sheet and the area exposed on the back surface side of the steel sheet are the area ratios in which the steel sheet overlaps in the vertical direction (plate thickness direction) of rolling.
- the area ratio is calculated by the mathematical formula shown in FIG. The closer the area ratio is to 100%, the closer the grain boundaries of the secondary recrystallized grains are to being perpendicular to the rolled surface of the steel sheet.
- This area ratio showed a higher value as the secondary recrystallization annealing temperature was higher.
- the total area of the samples investigated to obtain this area ratio was 336 cm 2 (for 4 Epstein samples). The result of examining the relationship between the area ratio and the iron loss is shown in FIG. As is clear from FIG. 3, the higher the area ratio, the lower the iron loss and the better.
- the grain boundaries are made vertical by prolonging the holding time of the secondary recrystallization annealing.
- increase the holding temperature of the secondary recrystallization annealing it is estimated that the same phenomenon will occur. That is, it is presumed that the grain boundary becomes perpendicular to the plate surface (rolling surface) due to the increase in the holding temperature, the area ratio is increased, and the iron loss is improved. According to this estimation, it is considered that the iron loss decreases as the grain boundary becomes closer to vertical. The reason for this is not clear, but it is presumed that, as the grain boundaries are more vertical, the magnetic domains in the grains are less disturbed, the domain walls move smoothly when the steel sheet is exemplified, and the iron loss is reduced.
- the above-mentioned area ratio at which the iron loss was good was 95% or more, but in order to achieve such an area ratio, the holding temperature of the secondary recrystallization annealing was set to an extremely high temperature of 1260°C or more. It was effective to do.
- the generation of the fine grains is, in addition to the utilization of the segregation element, if necessary, after cold rolling and before decarburization annealing, heat up to 700° C. at a high temperature rising rate and immediately quench without soaking.
- This is the first technology that could be realized by adopting a method different from the conventional one, such as adding steps and increasing the annealing temperature of the secondary recrystallization annealing to an extremely high temperature.
- one of the objects of the present invention is to reduce the cost increase due to the magnetic domain refining treatment, so that the product plate is not subjected to the magnetic domain refining treatment.
- the present invention has been completed based on the above findings. That is, the gist of the present invention is as follows. 1.
- the composition of the components is mass% and contains Si: 1.5 to 8.0% and Mn: 0.02 to 1.0%, and Sn: 0.010 to 0.400%, Sb: 0.010 to 0.400%, Mo: 0.010 to 0.200% and P: 0.010.
- the crystal grains are composed of coarse secondary recrystallized grains having a grain size of 5.0 mm or more, fine grains of more than 2.0 mm and less than 5.0 mm, and fine grains of 2.0 mm or less, and a plate among the coarse secondary recrystallized grains.
- the ratio is 95% or more, and has a structure containing fine particles having a particle size of more than 2.0 mm and less than 5.0 mm at a frequency of 0.2 to 5 particles/cm 2 .
- a grain-oriented electrical steel sheet characterized in that the steel sheet is not subjected to magnetic domain subdivision processing.
- composition of the components is% by mass, and further selected from Cr: 0.01 to 0.50%, Cu: 0.01 to 0.50%, Ni: 0.01 to 0.50%, Bi: 0.005 to 0.50% and Nb: 0.001 to 0.01%.
- the present invention it is possible to obtain a grain-oriented electrical steel sheet having excellent iron loss characteristics without applying a magnetic domain refining treatment by generating a certain proportion of fine crystal grains having a specific grain size in the final product plate.
- Si 1.5-8.0%
- Si is an element necessary for increasing the specific resistance of steel and improving iron loss, but if it is less than 1.5%, its effect of addition is poor, while if it exceeds 8.0%, the workability of steel deteriorates. Since rolling becomes difficult, the Si content is limited to 1.5 to 8.0%. It is preferably 2.5 to 4.5%.
- Mn 0.02-1.0%
- Mn is an element necessary for improving the hot workability, but if it is less than 0.02%, the effect is poor, while if it exceeds 1.0%, the magnetic flux density of the product plate decreases, so the Mn content is 0.02%. Up to 1.0% It is preferably 0.04 to 0.20%.
- At least one of the segregating elements Sn, Sb, Mo, and P is respectively Sn: 0.010 to 0.400%, Sb: 0.010 to 0.400%, Mo: 0.010 to 0.200%, P: 0.010 to 0.200% must be contained.
- Sn 0.020 to 0.100%
- Sb 0.020 to 0.100%
- Mo 0.020 to 0.070%
- P 0.012 to 0.100%.
- the balance other than the above elements is Fe and inevitable impurities.
- unavoidable impurities include C, Al, N, S, and Se, which are significantly reduced by purification and decarburization.
- the level of unavoidable impurities is not particularly limited, but it is preferable that C is less than 30 ppm, N is less than 20 ppm, and Al, S and Se are each less than 10 ppm.
- the crystal grains of the product plate are composed of coarse secondary recrystallized grains having a grain size of 5.0 mm or more, fine grains of more than 2.0 mm and less than 5.0 mm, and fine grains of 2.0 mm or less.
- the coarse secondary recrystallized grains are exposed in the areas where their projection planes match, out of the areas exposed on the front and back sides of the steel sheet, respectively.
- the area ratio to each area is 95% or more and that the fine particles having a particle size of more than 2.0 mm and less than 5.0 mm are included at a frequency of 0.2 to 5 particles/cm 2 .
- the grain size of crystal grains was calculated by extracting grain boundaries by image analysis and elliptic approximation by the ellipse approximation method, and taking the average of the major axis and the minor axis as the grain size of each crystal grain.
- molten steel having a predetermined composition adjustment may be produced as a slab by a conventional ingot making method or a continuous casting method, or a thin cast piece having a thickness of 100 mm or less may be produced by a direct casting method. ..
- the components (Si, Mn, segregation element, optional component elements) that are preferably added are preferably added at the molten steel stage because it is difficult to add them in the intermediate steps.
- the respective contents of Si, Mn, the segregation element, and the optional component element in the slab thus manufactured are retained in the component composition of the product plate.
- the content of unavoidable impurities C, Al, N, S, Se, etc. in the slab is not particularly limited, but in order to achieve the above-mentioned unavoidable impurity level in the product plate, for example, C: 0.10% or less, Al : 500 ppm or less, N: 100 ppm or less, S and Se: 200 ppm or less each.
- the slab Prior to hot rolling, the slab is heated in the usual way.
- high temperature annealing for solid solution of the inhibitor is not required, so it is preferable to set the slab heating temperature to a low temperature of less than 1300°C for cost reduction, more preferably 1250°C. It is as follows.
- the slab heating temperature is preferably 1300°C or higher because the inhibitor forms a solid solution.
- the steel slab heated to the slab heating temperature is hot-rolled into a hot-rolled steel sheet.
- the conditions for the hot rolling are not particularly limited, and the hot rolling can be performed under any conditions.
- the hot rolled sheet annealing temperature is preferably about 950 to 1150°C. If it is less than that, the unrecrystallized portion remains, and if it is more than that, the grain size after annealing becomes too coarse, and the subsequent primary recrystallization texture becomes unsuitable. It is preferably 1000°C or higher and 1100°C or lower.
- the cold-rolled sheet of final thickness is made by one cold rolling or two or more cold rolling steps with intermediate annealing.
- the annealing temperature of the intermediate annealing is preferably in the range of 900 to 1200°C. If it is less than 900°C, the recrystallized grains after the intermediate annealing become finer, and further, the Goss nuclei in the primary recrystallized structure are reduced and the magnetic properties of the product sheet are deteriorated. On the other hand, when the temperature exceeds 1200° C., the crystal grains become too coarse and it becomes difficult to obtain a primary recrystallized structure of grain size, as in the case of hot-rolled sheet annealing.
- the cold rolled sheet with the final thickness is then subjected to decarburization annealing and primary recrystallization annealing.
- the annealing temperature is preferably in the range of 800 to 900° C.
- the annealing atmosphere is preferably the wet atmosphere, from the viewpoint of promptly promoting the decarburizing reaction.
- the primary recrystallization annealing and the decarburization annealing may be performed separately.
- a steel sheet that has been subjected to decarburization annealing and primary recrystallization annealing is subjected to a secondary recrystallization annealing that also serves as a purification annealing after applying an annealing separator mainly composed of MgO, thereby developing a secondary recrystallization structure and It is possible to form a forsterite coating.
- the secondary recrystallization annealing is preferably performed at 800° C. or higher in order to develop the secondary recrystallization.
- the grain boundary of the coarse secondary recrystallized grain is perpendicular to the plate surface, of the area exposed respectively on the steel plate front surface side and the back surface side of the secondary recrystallized grain penetrating in the plate thickness direction.
- the holding temperature is preferably 1250° C. or higher in order to increase the area ratio of the areas where the projection planes coincide with each exposed area of the coarse secondary recrystallized grains to 95% or higher. More preferably, it is 1260°C or higher.
- the manufacturing method is not limited, but it is preferable to perform the secondary recrystallization annealing that also serves as the purification annealing at a holding temperature higher than usual.
- a coating that can apply tension to the steel sheet to reduce iron loss is preferable. It is preferable to use a method of applying a tension coating via a binder, a method of vapor-depositing an inorganic substance on the surface layer of a steel sheet to form a coating by a physical vapor deposition method or a chemical vapor deposition method, because it has excellent coating adhesion and a remarkable iron loss reducing effect.
- the grain-oriented electrical steel sheet of the present invention can be suitably obtained by the above production method, but is not limited to the one obtained by the above production method as long as it has the characteristics specified by the present invention.
- the grain-oriented electrical steel sheet of the present invention is characterized in that the steel sheet is not subjected to magnetic domain subdivision processing.
- “the magnetic domain is not subdivided into the steel sheet” means that the nonuniformity (strain) is introduced into the surface of the steel sheet by a physical method to subdivide the width of the magnetic domain. Means not been done.
- Specific examples of such treatment include heat-resistant strain introduction such as linear or dot-shaped groove formation, and non-heat-resistant strain introduction by irradiation with laser beam, electron beam, plasma flame, ultraviolet ray, or the like. However, it is not limited to these.
- the grain-oriented electrical steel sheet of the present invention is not subjected to the magnetic domain subdivision processing, the non-heat resistant strain is not removed by the strain relief annealing during the manufacture of the wound core, and the heat resistant magnetic domain subdivision is also performed. It is also possible to avoid a decrease in magnetic flux density due to. Therefore, it is useful as a material for wound cores manufactured through strain relief annealing.
- a sample with an overall area of 336 cm 2 (for 4 Epstein samples) cut out from the product plate was immersed in a 10% hydrochloric acid aqueous solution at 80°C for 180 seconds to remove the coating on the front and back surfaces to expose the secondary recrystallized grains. ..
- An image of the sample in which the secondary recrystallized grains were exposed was captured with a scanner at an image quality of 300 dpi, and grain boundaries were detected by image analysis software (“Photoshop CS6” made by Adobe) to create an image of only grain boundaries. This image was created on both the front and back sides of the sample.
- the image on the front side and the image on the back side can be distinguished by changing the color (for example, red on the front side and blue on the back side), and only the image on the back side is flipped horizontally or vertically to be a mirror image, and then both The images were overlaid.
- the orthographic projection of the grain boundary on the front surface side and the orthographic projection of the grain boundary on the back surface side were copied on one plane parallel to the plate surface (rolling surface).
- the part surrounded by the grain boundary on the front surface side and the part surrounded by the grain boundary on the back surface side are on the same plane as shown in FIG.
- the overlapping (matching) part was specified as the "region where the projection planes match", and the area (cm 2 ) was calculated.
- the area is divided by the average value of the area on the front surface side of the secondary recrystallized grain and the area of the portion surrounded by the grain boundaries on the back surface side to obtain the area ratio (%) of the region where the projection planes coincide. It was calculated.
- the area of each grain is calculated from the image of only the grain boundary acquired using the image analysis software, and the grain size is calculated by using the area as the circle equivalent diameter to obtain a coarse grain size of 5.0 mm or more.
- the proportions of recrystallized grains, fine grains having a grain size of more than 2.0 mm and less than 5.0 mm, and fine grains having a grain size of 2.0 mm or less were obtained.
- the number of fine particles having a particle size of more than 2.0 mm and less than 5.0 mm per 1 cm 2 was counted.
- Example 1 A steel slab containing C: 0.015%, Si: 3.72%, Mn: 0.05%, Al: 0.020%, N: 0.0070% and Sn: 0.15% with the balance Fe and unavoidable impurities produced by continuous casting. Then, after performing slab heating for soaking at 1300° C. for 45 minutes, hot rolling was applied to finish the product to a thickness of 2.6 mm. Then, after hot-rolled sheet annealing was performed at 950° C. for 60 seconds in a dry nitrogen atmosphere, cold rolling was performed to a sheet thickness of 0.23 mm. Then, it was heated to 700° C.
- the iron loss W 17/50 (iron loss when excited to 1.7 T at 50 Hz) of the sample cut out from the product plate thus obtained was measured by the method described in JIS C 2550-1:2011.
- the obtained sample was immersed in a 10% hydrochloric acid aqueous solution at 80°C for 180 seconds to remove the coating on the front and back surfaces so that secondary recrystallized grains could be confirmed.
- a particle size distribution was obtained. Furthermore, among the coarse secondary recrystallized grains with a grain size of 5 mm or more, for the grains penetrating in the plate thickness direction, among the exposed areas on the steel plate front surface side and back surface side, respectively, their projection planes match.
- Table 1 The obtained results are also shown in Table 1.
- Table 1 the underline indicates that it is outside the scope of the present invention.
- the average value of the misorientation angle between the crystal orientation and the Goss orientation of the fine grains having a grain size of more than 2.0 mm and less than 5.0 mm measured on the product sheet of the present invention example was 33.5°. As is clear from the table, it is found that good iron loss characteristics are obtained under the conditions within the range of the present invention.
- Example 2 A steel slab containing the components shown in Table 2 and the balance Fe and unavoidable impurities is manufactured by continuous casting.
- sol.Al is contained in an amount of 150 ppm or more
- slab heating for uniform heating at 1320°C for 50 minutes is performed.
- slab heating was performed soaking at 1230° C. for 50 minutes, and then hot rolling was performed to a thickness of 2.0 mm.
- the sheet was finished by cold rolling to have a sheet thickness of 0.20 mm. Then, it was heated to 720° C.
- the iron loss W 17/50 (iron loss when excited to 1.7 T at 50 Hz) and magnetic flux density B 8 (magnetic flux density when excited with a magnetizing force of 800 A/m) of the sample cut out from the product plate thus obtained It was measured by the method described in JIS C 2550-1:2011.
- the obtained sample was immersed in a 10% hydrochloric acid aqueous solution at 80°C for 180 seconds to remove the coating on the front and back surfaces so that the secondary recrystallized grains could be confirmed. A particle size distribution was obtained.
- the projection planes of the exposed areas on the steel plate front side and back surface side are the same.
- the area ratio of the area to be exposed to each area where the coarse secondary recrystallized grains were exposed was calculated under each condition. The results are shown in Table 3.
- the area of the sample investigated to obtain these particle size distribution and area ratio was 336 cm 2 (for 4 Epstein samples).
- Table 3 also shows the results of examining the base iron component of the product plate using the sample from which the coating on the front and back surfaces was removed.
- the underline indicates that it is outside the scope of the present invention.
- the average value of the misorientation angle between the crystal orientation and the Goss orientation of the fine particles having a grain size of more than 2.0 mm and less than 5.0 mm measured on the product sheet of the present invention example was 26.9°.
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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、鋼板の表面に対して物理的な手法で不均一性を導入して、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、特許文献5には、電子ビームの照射により磁区幅を制御する技術が提案されている。
さて、発明者らは、上記の目的を達成すべく鋭意検討を重ねた結果、最終製品板に細かい結晶粒を一定割合で発生させることにより、磁区細分化処理を適用しなくても鉄損特性に優れた方向性電磁鋼板が得られることを見出した。
<実験1>
質量%で、C:0.030%、Si:3.33%、Mn:0.15%、Al:0.0026%、N:0.0025%、S:0.0014%およびSb:0.08%を含み、残部はFeおよび不可避的不純物からなる鋼スラブAと、C:0.031%、Si:3.27%、Mn:0.15%、Al:0.0020%、N:0.0021%およびS:0.0013%を含み、Sbは含有せず、残部はFeおよび不可避的不純物からなる鋼スラブBとを、連続鋳造にて製造し、1200℃で30分均熱するスラブ加熱を施した後、熱間圧延により2.2mmの厚さに仕上げた。ついで、乾燥窒素雰囲気下で1080℃、30秒の熱延板焼鈍を施した後、冷間圧延により0.23mmの板厚に仕上げた。さらに、乾燥窒素雰囲気下で昇温速度を20℃/sから1500℃/sまで種々変更して700℃まで加熱し、均熱せず直ちに平均100℃/sで室温まで冷却した。続いて50%H2-50%N2、露点50℃の湿潤雰囲気下で、850℃で150秒の脱炭焼鈍を兼ねた一次再結晶焼鈍を施した。さらに、MgOを主体とする焼鈍分離剤を塗布し、水素雰囲気下で1250℃で10時間保定する純化焼鈍を兼ねた二次再結晶焼鈍を行った。
得られたデータをもとに、鉄損と粒径2.0mm超5.0mm未満の結晶粒の個数(1cm2当たり)との関係について調査した結果を、図1に示す。
1点目は、Sbを含有する鋼スラブAでは、粒径2.0mm超5.0mm未満の結晶粒の個数が0.2~5個/cm2の時に鉄損が良好なことである。
2点目は、Sbを含有しない鋼スラブBでは、粒径2.0mm超5.0mm未満の結晶粒の個数が非常に少なく0.2個/cm2未満であり、また鉄損の低減も望めないことである。
そもそも、方向性電磁鋼板の鉄損の大小は、二次再結晶粒内の磁区構造に大きく影響される。方向性電磁鋼板の二次再結晶粒は、そのほとんどが180°磁区と呼ばれる圧延方向にほぼ平行な磁区で構成されている。そして、その磁区の幅が鉄損特性に大きく影響し、幅が狭いほど鉄損が低減できる。例えば、鋼板に機械的な線状溝を付与する磁区細分化処理法がある。その方法は、溝を形成すると、溝断面の静磁エネルギーが増大するため、そのエネルギーの増大を、磁区幅を狭くすることで解消しようとする磁気特性を利用したものである。
上述するように、前記細粒は、粗大な二次再結晶粒との間で大きな方位差角を有するため、前記細粒と粗大な二次再結晶粒との粒界では磁区が不連続になる場合がある。この場合、磁極が発生し静磁エネルギーが増大する可能性があり、上記と同じ理由により磁区が細分化されることが推測される。これが前記細粒による鉄損低減のメカニズムであろうと考えている。
鋼スラブAはSbを含有し、これは偏析元素として知られている。このSbが、二次再結晶初期の段階で一次再結晶粒の粒界に偏析して粒界移動を抑制することで、一次再結晶粒が二次再結晶粒まで成長することを抑制し、その結果、細粒が発生したと推定される。一方、鋼スラブBではSbのような偏析元素が鋼中に含まれないため、二次再結晶初期で粒界移動が抑制されず、細粒は発生せずに粗大な二次再結晶粒のみが生じたと推測される。
よって、それら文献開示の低鉄損化技術と本発明の技術とは、技術的思想が本質的に異なり、利用する結晶粒の粒径およびその制御方法も異なるものと推測される。
上記実験1では、一般的な方向性電磁鋼板の製造方法とは異なり、冷間圧延後であって脱炭焼鈍前に、乾燥窒素雰囲気下で昇温速度を実験的に種々変更して700℃まで加熱し、均熱せず直ちに平均100℃/sで室温まで冷却する工程を追加している。この工程が二次再結晶時の細粒発生に寄与したと考えている。
実験1で使用した鋼スラブAを、1200℃で60分均熱するスラブ加熱を施した後、熱間圧延により2.4mmの厚さに仕上げた。その後、乾燥窒素雰囲気下で1000℃、30秒の熱延板焼鈍を施した後、冷間圧延により0.23mmの板厚に仕上げた。ついで、乾燥窒素雰囲気下で昇温速度:750℃/sで700℃まで加熱し、均熱せず直ちに平均70℃/sで室温まで冷却した。続いて55%H2-45%N2、露点55℃の湿潤雰囲気下で850℃、120秒の脱炭を兼ねた一次再結晶焼鈍を施した。さらに、MgOを主体とする焼鈍分離剤を塗布し、水素雰囲気下で1100℃から1300℃までの種々の温度に保定する純化を兼ねた二次再結晶焼鈍を行った。このとき、保定温度までの昇温速度は平均で20℃/hとした。
方向性電磁鋼板の製品板の板厚は、一般に0.2~0.5mm程度であり、その板厚より粒径が大きい粒は、基本的に板厚方向に貫通しているとみなされる。つまり、本発明の方向性電磁鋼板において、被膜を除去した鋼板の表裏面で観察できる粒径5mm以上の粗大な二次再結晶粒は全て「板厚方向に貫通している粒」とみなすことができる。
ある1個の粗大な二次再結晶粒の「鋼板表面側で露出する面積」とは、当該結晶粒を鋼板の表面側で観察した場合に、当該二次再結晶粒が露出して鋼板上で二次元(すなわち、平面)的に占める面積であり、より具体的には、鋼板表面上で観察される粒界で囲まれた部分の面積である。図2では、当該面積またはその投影面(当該面積の正射影)を実線の図形として示す。
当該二次再結晶粒の「裏面側で露出する面積」とは、表面側と同様にして、当該結晶粒を鋼板の裏面側で観察した場合に観察される、粒界で囲まれた部分の面積である。図2では、当該面積またはその投影面(当該面積の正射影)を破線の図形として示す。
「それらの投影面が一致する領域」とは、対象の二次再結晶粒の鋼板表面側で露出する面積と鋼板裏面側で露出する面積とを、板面(圧延面)に対して平行な一平面上にそれぞれ正射影として投影した場合に、それら正射影が重なり合う(一致する)部分である。図2では、当該領域を斜線部分で示す。
従って、「その鋼板表面側および裏面側でそれぞれ露出する面積のうち、それらの投影面が一致する領域の、該粗大な二次再結晶粒が露出した各面積に対する面積率」は、該二次結晶粒の鋼板表面側で露出する面積と鋼板裏面側で露出する面積とが、鋼板の圧延垂直方向(板厚方向)に重なり合う面積率である。その面積率は、図2に示す数式で算出される。この面積率が100%に近いほど、二次再結晶粒の粒界が鋼板圧延面に対し垂直に近いことを意味する。
図3から明らかなように、前記面積率が高いほど、鉄損が低く良好であることがわかる。
特許文献8によると、方向性電磁鋼板の製品板の打ち抜き性に関する記載があり、二次再結晶の粒界を板面に対して垂直方向に近づけることで、粒界をせん断する機会が減り、打ち抜き性を改善できると指摘されている。この場合は、二次再結晶焼鈍の保定時間を長時間化することで、粒界を垂直にさせているが、本実験2の様に、二次再結晶焼鈍の保定温度を高温化することでも同様の現象が起こると推定される。すなわち、保定温度高温化により、粒界が板面(圧延面)に対して垂直となり、上記面積率が増大して、鉄損が向上したと推定される。この推定によれば、粒界が垂直に近くなるほど、鉄損が低下すると考えられる。この理由は定かではないが、おそらくは、垂直な粒界ほど、粒内の磁区に乱れが少なく、鋼板が例示された際の磁壁の移動がスムーズとなり、鉄損が低減したと推定している。
上記実験2では、鉄損が良好となる上記面積率は95%以上であったが、そのような面積率を達成するには、二次再結晶焼鈍の保定温度を1260℃以上と極めて高温にすることが有効であった。
ただし、本発明では、製品板の鋼組織において細粒が発生していることが重要であり、その手段を規定するものではない。一例では、偏析元素を大量に含有すると、冷間圧延後であって脱炭焼鈍前に、速い昇温速度で700℃まで加熱し、均熱せずに直ちに急冷する工程を採用しなくても、細粒が増加して、本発明範囲内に入る製品板が得られる場合がある。
また、本発明の目的の一つは、磁区細分化処理によるコストアップを低減することであるため、製品板に磁区細分化処理を施すことはない。
すなわち、本発明の要旨構成は次のとおりである。
1.成分組成は、質量%で、Si:1.5~8.0%およびMn:0.02~1.0%を含有し、かつSn:0.010~0.400%、Sb:0.010~0.400%、Mo:0.010~0.200%およびP:0.010~0.200%のうちから選んだ少なくとも一種を含有し、残部はFeおよび不可避的不純物からなり、
結晶粒が、粒径として5.0mm以上の粗大な二次再結晶粒と2.0mm超5.0mm未満の細粒と2.0mm以下の微細粒とからなり、該粗大な二次再結晶粒のうち板厚方向に貫通している粒について、その鋼板表面側および裏面側でそれぞれ露出する面積のうち、それらの投影面が一致する領域の、該粗大な二次再結晶粒が露出した各面積に対する面積率が95%以上であり、かつ該粒径2.0mm超5.0mm未満の細粒を0.2~5個/cm2の頻度で含む組織を有し、
鋼板に対する磁区細分化処理が施されていないことを特徴とする、方向性電磁鋼板。
4.前記1から3のいずれかに記載の方向性電磁鋼板を用いて作製された巻鉄心。
また、本発明によれば、偏析元素をさらに含有させ、かつ二次再結晶焼鈍の昇温速度と保定時間を適正化することで、高周波鉄損の低減と打ち抜き性の向上を両立させることができる。
Si:1.5~8.0%
Siは、鋼の比抵抗を高め、鉄損を改善させるために必要な元素であるが、1.5%未満であるとその添加効果に乏しく、一方8.0%を超えると鋼の加工性が劣化し、圧延が困難となることから、Si量は1.5~8.0%に限定される。好ましくは、2.5~4.5%である。
Mnは、熱間加工性を良好にするために必要な元素であるが、0.02%未満であると効果に乏しく、一方1.0%を超えると製品板の磁束密度が低下するので、Mn量は0.02~1.0%とする。好ましくは、0.04~0.20%である。
すなわち、磁気特性を向上させる目的で、Cr:0.01~0.50%、Cu:0.01~0.50%、Ni:0.01~0.50%、Bi:0.005~0.50%、Nb:0.001~0.01%のうちから選んだ一種を単独または複合して添加することができる。それぞれ添加量が下限量より少ない場合には磁気特性向上効果がなく、一方上限量を超えると二次再結晶粒の発達が抑制され磁気特性が劣化する。
本発明の方向性電磁鋼板の製造方法は、一般的な電磁鋼板を製造する方法を利用できる。すなわち、所定の成分調整がなされた溶鋼を、通常の造塊法もしくは連続鋳造法でスラブを製造してもよいし、100mm以下の厚さの薄鋳片を直接鋳造法で製造してもよい。上述の、添加が好ましい成分(Si、Mn、偏析元素、任意成分元素)は、途中工程で加えることは困難であることから、溶鋼段階で添加することが好ましい。そのように製造されたスラブにおけるSi、Mn、偏析元素、および任意成分元素の各含有量は、製品板の成分組成でも保持される。
なお、スラブにおける不可避不純物C、Al、N、S、Se等の各含有量は、特に限定されないが、製品板で上述の不可避不純物レベルを達成するためには、例えばC:0.10%以下、Al:500ppm以下、N:100ppm以下、SおよびSe:各200ppm以下とすることが好ましい。
当該細粒の発生を確保する観点から、当該工程において、昇温速度は100~3000℃/sの範囲とすることが好ましく、冷却速度は5~200℃/sの範囲とすることが好ましい。
そして、本発明の方向性電磁鋼板は、磁区細分化処理を施していないため、巻鉄心製造時の歪取焼鈍により非耐熱型の歪が除去されることがなく、また耐熱型の磁区細分化による磁束密度の低下を回避することもできる。そのため、歪取焼鈍を経て製造される巻鉄心の材料として有用である。
以下、各測定方法を具体的に説明する。
製品板から切り取った全体面積336cm2(エプスタインサンプル4枚分)のサンプルを80℃の10%塩酸水溶液に180秒浸漬して、表裏面の被膜を除去して二次再結晶粒を露出させた。
二次再結晶粒が露出したサンプルの画像をスキャナーで300dpiの画質にて取り込み、画像解析ソフト(Adobe社製「Photoshop CS6」)で粒界を検出して、粒界のみの画像を作成した。この画像作成は、サンプルの表裏両面について行った。表面側の画像と裏面側の画像は色を変えて識別可能にし(例えば、表面側は赤色、裏面側は青色)、裏面側の画像のみを左右または上下を反転させて鏡像としてから、両方の画像を重ね合わせた。このようにして、表面側の粒界の正射影と裏面側の粒界の正射影とを、板面(圧延面)に対して平行な一平面上に写した。サンプルに含まれる粒径5.0mm以上の二次再結晶粒全てについて、表面側の粒界で囲まれた部分と裏面側の粒界で囲まれた部分とが図2のように同一平面上で重なり合う(一致する)部分を「投影面が一致する領域」として特定し、その面積(cm2)を算出した。当該面積を、該二次再結晶粒の表面側で面積と裏面側の粒界で囲まれた部分の面積との平均値で除して、投影面が一致する領域の面積率(%)を算出した。
上述のように画像解析ソフトを用いて取得した粒界のみの画像から、各粒の面積を算出し、それを円相当径として粒径を計算することによって、粒径5.0mm以上の粗大な二次再結晶粒、粒径2.0mm超5.0mm未満の細粒、粒径2.0mm以下の微細粒の割合を求めた。
上記の方法で計算した粒径を元に、1cm2あたりに存在する粒径2.0mm超5.0mm未満の細粒の個数をカウントした。
二次再結晶粒が露出したサンプルを20mm角に剪断し、得られた20mm角サンプル片に存在する粒径2.0mm超5.0mm未満の細粒全ての結晶方位を測定した。結晶方位は、SEMに付帯するElectron Back-Scattering Pattern(EBSP)装置を用いて電子線後方散乱回折像から測定した。測定された結晶方位とゴス方位との間の方位差角の平均を計算によって求めた。
C:0.015%、Si:3.72%、Mn:0.05%、Al:0.020%、N:0.0070%およびSn:0.15%を含み、残部はFeおよび不可避的不純物からなる鋼スラブを、連続鋳造にて製造し、1300℃で45分均熱するスラブ加熱を施した後、熱間圧延により2.6mmの厚さに仕上げた。その後、乾燥窒素雰囲気下で950℃、60秒の熱延板焼鈍を施した後、冷間圧延で0.23mmの板厚に仕上げた。ついで、乾燥窒素雰囲気下で表1に示す昇温速度で700℃まで加熱し、均熱せず直ちに平均80℃/sの冷却速度で室温まで冷却した。続いて60%H2-40%N2、露点60℃の湿潤雰囲気下で850℃、90秒の脱炭焼鈍を兼ねた一次再結晶焼鈍を施した。さらに、MgOを主体とする焼鈍分離剤を塗布し、水素雰囲気下で表1に示す温度で10時間保定する純化焼鈍を兼ねた二次再結晶焼鈍を行った。
また、本発明例の製品板について測定した粒径2.0mm超5.0mm未満の細粒の結晶方位とゴス方位との間の方位差角の平均値は、いずれも33.5°であった。
同表から明らかなように、本発明範囲内の条件で、良好な鉄損特性が得られていることがわかる。
表2に示す成分を含み、残部はFeおよび不可避的不純物からなる鋼スラブを、連続鋳造にて製造し、sol.Alを150ppm以上含む場合には1320℃で50分均熱するスラブ加熱を施した後、あるいはsol.Alが150ppm未満の場合には1230℃で50分均熱するスラブ加熱を施した後、熱間圧延により2.0mmの厚さに仕上げた。その後、乾燥窒素雰囲気下で1125℃、20秒の熱延板焼鈍を施した後、冷間圧延で0.20mmの板厚に仕上げた。ついで、乾燥窒素雰囲気下で昇温速度700℃/sで720℃まで加熱し、均熱せず直ちに平均120℃/sの冷却速度で室温まで冷却した。続いて45%H2-55%N2、露点48℃の湿潤雰囲気下で830℃、140秒の脱炭焼鈍を施した。さらに、MgOを主体とする焼鈍分離剤を塗布し、その後1275℃で10時間、水素雰囲気下で保定する純化焼鈍を兼ねた二次再結晶焼鈍を行った。二次再結晶焼鈍の昇温速度は20℃/hとした。
なお、表2中、下線は本発明の範囲外であることを示す。
また、この表裏面の被膜を除去したサンプルを用いて、製品板の地鉄成分を調べた結果を表3に併記する。表3中、下線は本発明の範囲外であることを示す。
また、本発明例の製品板について測定した粒径2.0mm超5.0mm未満の細粒の結晶方位とゴス方位との間の方位差角の平均値は、いずれも26.9°であった。
Claims (4)
- 成分組成は、質量%で、Si:1.5~8.0%およびMn:0.02~1.0%を含有し、かつSn:0.010~0.400%、Sb:0.010~0.400%、Mo:0.010~0.200%およびP:0.010~0.200%のうちから選んだ少なくとも一種を含有し、残部はFeおよび不可避的不純物からなり、
結晶粒が、粒径として5.0mm以上の粗大な二次再結晶粒と2.0mm超5.0mm未満の細粒と2.0mm以下の微細粒とからなり、該粗大な二次再結晶粒のうち板厚方向に貫通している粒について、その鋼板表面側および裏面側でそれぞれ露出する面積のうち、それらの投影面が一致する領域の、該粗大な二次再結晶粒が露出した各面積に対する面積率が95%以上であり、かつ該粒径2.0mm超5.0mm未満の細粒を0.2~5個/cm2の頻度で含む組織を有し、
鋼板に対する磁区細分化処理が施されていないことを特徴とする、方向性電磁鋼板。 - 前記粒径2.0mm超5.0mm未満の細粒の結晶方位とゴス方位との間の方位差角の平均が15°以上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。
- 前記成分組成が、質量%で、さらに、Cr:0.01~0.50%,Cu:0.01~0.50%、Ni:0.01~0.50%、Bi:0.005~0.50%およびNb:0.001~0.01%のうちから選んだ一種または二種以上を含有す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。
- 請求項1から3のいずれか1項に記載の方向性電磁鋼板を用いて作製された巻鉄心。
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- 2020-01-30 EP EP20748720.8A patent/EP3919636A4/en active Pending
- 2020-01-30 US US17/426,729 patent/US11959149B2/en active Active
- 2020-01-30 KR KR1020217023938A patent/KR102504894B1/ko active IP Right Grant
- 2020-01-30 CN CN202080011581.2A patent/CN113366125B/zh active Active
- 2020-01-30 JP JP2020531678A patent/JP6813134B2/ja active Active
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Also Published As
Publication number | Publication date |
---|---|
EP3919636A1 (en) | 2021-12-08 |
KR102504894B1 (ko) | 2023-02-28 |
JPWO2020158893A1 (ja) | 2021-02-18 |
JP6813134B2 (ja) | 2021-01-13 |
US20220098697A1 (en) | 2022-03-31 |
EP3919636A4 (en) | 2022-03-23 |
KR20210107833A (ko) | 2021-09-01 |
CN113366125A (zh) | 2021-09-07 |
CN113366125B (zh) | 2023-01-20 |
US11959149B2 (en) | 2024-04-16 |
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