WO2022210870A1 - 無方向性電磁鋼板 - Google Patents

無方向性電磁鋼板 Download PDF

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Publication number
WO2022210870A1
WO2022210870A1 PCT/JP2022/015948 JP2022015948W WO2022210870A1 WO 2022210870 A1 WO2022210870 A1 WO 2022210870A1 JP 2022015948 W JP2022015948 W JP 2022015948W WO 2022210870 A1 WO2022210870 A1 WO 2022210870A1
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steel sheet
annealing
crystal
oriented electrical
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PCT/JP2022/015948
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English (en)
French (fr)
Japanese (ja)
Inventor
岳顕 脇坂
義顕 名取
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Nippon Steel Corp
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Nippon Steel Corp
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Priority to CN202280025365.2A priority Critical patent/CN117120648A/zh
Priority to BR112023019184A priority patent/BR112023019184A2/pt
Priority to JP2023511478A priority patent/JP7755183B2/ja
Priority to EP22781080.1A priority patent/EP4317474A4/en
Priority to US18/284,032 priority patent/US20240153684A1/en
Priority to KR1020237032623A priority patent/KR20230150986A/ko
Publication of WO2022210870A1 publication Critical patent/WO2022210870A1/ja
Anticipated expiration legal-status Critical
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Definitions

  • the present invention relates to a non-oriented electrical steel sheet.
  • This application claims priority based on Japanese Patent Application No. 2021-061752 filed in Japan on March 31, 2021 and Japanese Patent Application No. 2021-099597 filed in Japan on June 15, 2021. , the contents of which are hereby incorporated by reference.
  • Patent Document 1 describes that in a method of punching a non-oriented electrical steel sheet to produce a motor core, the roundness of the cutting edge of a punching die is controlled according to the elongation rate of the non-oriented electrical steel sheet. ing.
  • the non-oriented electrical steel sheet used for the stator core of the motor is subjected to core annealing to reduce iron loss after the stator core is punched out with a die.
  • core annealing To reduce iron loss after the stator core is punched out with a die.
  • the rotor core is first punched out of the non-oriented electrical steel sheet, then the inner diameter of the stator core is punched out, and then the outer diameter of the stator core is punched out.
  • core annealing By applying heat to the stator core by core annealing, residual stress and strain are released, and iron loss is reduced.
  • the stator core is subjected to core annealing
  • the rotor core is generally not subjected to annealing in order to increase the strength.
  • the shape change of the stator core due to the release of the residual stress during core annealing will be uneven.
  • the high roundness of the inner diameter of the stator core obtained before core annealing may be reduced by core annealing.
  • One of the causes of non-uniform residual stress distribution is structural non-uniformity of punched non-oriented electrical steel sheets.
  • Patent Document 1 controls the roundness of the cutting edge of the punching die according to the elongation rate of the non-oriented electrical steel sheet, and the dimensional accuracy after processing the non-oriented electrical steel sheet. is controlled by the dimensions of the punching die. For this reason, the technique described in Patent Document 1 does not assume that a non-oriented electrical steel sheet capable of obtaining desired dimensional accuracy can be obtained without depending on the dimensions of the punching die.
  • an object of the present invention is to provide a non-oriented electrical steel sheet capable of suppressing deterioration in dimensional accuracy after processing and subsequent core annealing (stress relief annealing).
  • the gist of the present disclosure is as follows. (1) In a non-oriented electrical steel sheet according to an embodiment of the present invention, when a boundary having a crystal orientation difference of 2° or more and less than 15° is regarded as a grain boundary in a cross section parallel to the steel sheet surface, the grain The area ratio of crystal grains having a diameter of less than 200 ⁇ m satisfies 10% or less. (2) The non-oriented electrical steel sheet described in (1) above has a maximum grain size of D15 when a boundary having a crystal orientation difference of 15° or more is regarded as a grain boundary in a cross section parallel to the steel sheet surface.
  • the non-oriented electrical steel sheet according to (1) or (2) above has a crystal orientation difference of 200 ⁇ m or more when a boundary having a crystal orientation difference of 15° or more is regarded as a grain boundary in a cross section parallel to the steel sheet surface.
  • the following formula (2) may be satisfied when the major axis length is DL and the minor axis length is DC.
  • FIG. 4 is a plan view showing a state in which the rotor core is inserted inside the stator core
  • the non-oriented electrical steel sheet used for the stator core is punched into the shape of the stator core with a die, and then subjected to heat treatment (core annealing) to reduce iron loss.
  • heat treatment core annealing
  • FIG. 1 is a plan view showing a state in which the rotor core is inserted inside the stator core.
  • a stator core 21 is constructed by laminating non-oriented electrical steel sheets in the direction perpendicular to the paper surface, and is composed of a core back 22 on the outer peripheral side and a plurality of teeth 23 protruding inward from the core back 22 .
  • a rotor core 30 is inserted inside the tips of the teeth 23 .
  • the rotor core 30 has a rotor core 31 and a plurality of magnets 32 provided on the outer peripheral side of the rotor core 31 and facing the tips of the teeth 23 .
  • the outer circumference of stator core 21 is held by case 50 .
  • a shaft 60 penetrates through the center of the rotor core 31 and is fixed to the rotor core 31 .
  • the shaft 60 is rotatably supported by the case 50 (or another fixed member) with the center O of the shaft 60 aligned with the center of the inner diameter of the stator core 21 .
  • the inner diameter of the stator core is specifically the inner diameter D of the tips of the teeth 23 .
  • the circularity of the inner diameter D decreases due to the change in the shape of the stator core 21 due to the release of the residual stress, the gap between the tips of the teeth 23 and the rotor core 31 becomes uneven. This increases the cogging torque when the rotor core 30 rotates. An increase in cogging torque causes uneven rotation, vibration, noise, and the like. Further, if the roundness of the inner diameter of the stator core 21 is further reduced, problems such as the rotor iron core 31 of the rotor core 30 coming into contact with the tips of the teeth 23 may occur.
  • the ratio obtained by dividing the difference between the maximum and minimum diameters of a circle by the average diameter is used as the roundness evaluation criterion.
  • the maximum circle diameter is the diameter of the larger circle among the above two concentric circles described in JIS B0621 (1984), and the maximum circle diameter is the diameter of the smaller circle among the above two concentric circles.
  • the average diameter is the average value of the maximum and minimum diameters of the circle. Therefore, the roundness evaluation criteria of this embodiment are the roundness, which is the radius difference between two concentric circles when the interval between two concentric circles described in JIS B0621 (1984) is the minimum, and the radius of the two circles corresponds to the ratio obtained by dividing by the average value of
  • the ratio of the difference between the maximum value and the minimum value of the inner diameter D to the average diameter exceeds 0.200%, the gap between the tip of the tooth 23 and the rotor core 31 becomes uneven, causing uneven rotation, vibration, noise, and the like. Also, the rotor core 31 of the rotor core 30 hits the tips of the teeth 23. Therefore, the ratio of the difference between the maximum value and the minimum value of the inner diameter D to the average diameter is set to 0.200% or less. This ratio is preferably 0.15% or less, more preferably 0.100% or less. Since the smaller the ratio, the better, there is no lower limit.
  • One of the causes of non-uniform residual stress distribution in the stator core is the structural non-uniformity of the punched non-oriented electrical steel sheets.
  • the stresses remaining in the respective structures are different, resulting in differences in the degree of stress release during core annealing.
  • the recrystallized structure and the non-recrystallized structure are finely dispersed in the non-oriented electrical steel sheet, it is relatively difficult to detect a decrease in roundness of the inner diameter of the stator core after punching.
  • the uneven distribution of the recrystallized structure and the non-recrystallized structure occurs when the average grain size of the steel sheet before the final cold rolling is relatively large, or when there are many grains larger than the average grain size in the steel sheet before the final cold rolling. easy to get up.
  • "Before final cold rolling” means after the final annealing performed before final cold rolling.
  • after hot-rolling and coiling corresponds to "before the final cold-rolling”
  • the hot-rolled sheet After annealing corresponds to "before final cold rolling”
  • after intermediate annealing corresponds to "before final cold rolling”.
  • the ⁇ 100 ⁇ 0vw> oriented grains become coarsely processed grains elongated in the rolling direction during cold rolling, and are then annealed. It remains as a coarse non-recrystallized structure.
  • the non-oriented electrical steel sheet of the present embodiment has a crystal grain size of less than 200 ⁇ m when a boundary having a crystal orientation difference of 2° or more and less than 15° is regarded as a grain boundary in a cross section parallel to the steel sheet surface.
  • the grain area ratio satisfies 10% or less.
  • the crystal misorientation of the boundary for judging the crystal boundary is limited to a small misorientation of less than 15°.
  • a region observed as a relatively fine structure with a crystal grain size of less than 200 ⁇ m due to such a grain boundary with a small crystal orientation difference is, in other words, a region in which crystals having the same crystal orientation are adjacent to each other.
  • Such regions are considered to be generated by cold rolling and annealing due to the presence of non-uniform regions in which recrystallized structures and non-recrystallized structures are unevenly distributed.
  • this area ratio is limited to 10% or less. It is preferably less than 5%.
  • the reason why the lower limit of the crystal orientation difference for judging the grain boundary is set to 2° or more is that if the crystal orientation difference for judging the grain boundary is too small (for example, about 1°), slight distortion of the crystal or This is because, depending on the accuracy of the measuring instrument, what is not a crystal boundary may be determined to be a crystal grain boundary.
  • the crystal orientation difference and the area ratio of crystal grains are measured as follows. First, a sample (crystalline sample) is taken from a non-oriented electrical steel sheet with a cross section parallel to the steel sheet surface (a cross section parallel to the rolling direction and thickness direction of the steel sheet) as an observation surface, and the observation surface is polished to a mirror surface. Finish. Next, the crystalline sample is placed in a scanning electron microscope (SEM) with a large inclination, and is irradiated with an electron beam to obtain an EBSD (Electron Back Scatter Diffraction) pattern. The EBSD pattern is continuously collected by a dedicated EBSD detector, and the EBSD pattern is indexed and the crystal orientation is calculated.
  • SEM scanning electron microscope
  • the crystal structure analysis by the EBSD method is performed at a magnification of 100, the number of fields of view: 5, and the size of one field of view is 800 ⁇ m ⁇ 1,000 ⁇ m or more.
  • the obtained data is analyzed with "OIM Analysis Version 7.3.1” (manufactured by TSL).
  • TSL "OIM Analysis Version 7.3.1”
  • the maximum grain size is D15 MAX when the boundary having a crystal orientation difference of 15° or more is regarded as the grain boundary, and the boundary having a crystal orientation difference of 2° or more
  • D2 AVE is the average crystal grain size when is regarded as a crystal grain boundary, it is preferable to satisfy the following formula (1).
  • This ratio is an index showing how continuously the crystals having the same crystal orientation are adjacent to each other and how wide they spread.
  • the grain boundary for determining D2 AVE includes the grain boundary for determining D15 MAX . That is, the crystal grain structure for determining D2 AVE is a crystal structure obtained by further dividing part of the crystal grains for determining D15 MAX at grain boundaries with a small misorientation. The smaller this ratio, the coarser the crystal grains when a boundary with a crystal misorientation of 15° or more is regarded as a grain boundary, the more coarse the crystal grains are at the crystal grain boundary with a small misorientation of 2° or more and less than 15°. Indicates a state of fragmentation.
  • D15 MAX /D2 AVE is preferably 3.0 or less.
  • the shape of the crystal grain having a crystal grain size of 200 ⁇ m or more is approximated by an ellipse.
  • DL is the length of the long axis
  • DC is the length of the short axis.
  • the approximation to an ellipse is, for example, ⁇ “Investigation of material control and material maintenance methods by evaluating strength characteristics focusing on crystal grain shape” (Harada et al., Abstracts of the Japan Society of Maintenology, 2nd, P150) can be processed according to the procedure described in .
  • a test piece having a width of 15 mm and a length of 10 mm with the rolling direction as the longitudinal direction is taken from the center of the non-oriented electrical steel sheet in the sheet width direction, and from the surface of the test piece to about 1/2 of the plate thickness. Polished to a mirror finish.
  • the mirror-finished sample is observed at an observation magnification of 100 using an EBSD-equipped SEM, and the crystal structure is analyzed by EBSD measurement.
  • Data obtained by EBSD measurement is subjected to crystal orientation analysis using "OIM Analysis Version 7.3.1" (manufactured by TSL).
  • DL/DC is calculated individually and averaged.
  • the present embodiment defines a situation in which coarse crystal grains are finely divided at crystal grain boundaries with a small misorientation of 2° or more and less than 15°.
  • coarse crystal grains refers to crystal grains when a boundary having a crystal orientation difference of 15° or more is regarded as a crystal grain boundary.
  • Coarse crystal grains to be split are stretched by cold rolling in the manufacturing process, and fine crystal grains dividing them tend to occur in such stretched regions. In other words, even if coarse crystal grains exist, if they are not stretched, the coarse crystal grains will have a recrystallized structure and a non-recrystallized structure that cause uneven distribution of residual stress as described above. It should be considered that it occurred independently of the ubiquitous organization. In other words, it is an index that indicates that there was no structure that would cause uneven distribution of residual stress that would reduce the roundness.
  • DL/DC is 3.0 or less.
  • the average grain size of the steel sheet before the final cold rolling is 200 ⁇ m or less, and the existence ratio of crystal grains exceeding 200 ⁇ m is 10% or less of the whole.
  • the existence ratio of ⁇ 100 ⁇ ⁇ 0vw> oriented grains in the steel sheet before the final cold rolling is 10% or less of the whole.
  • Such a base sheet is a steel sheet in which uneven distribution of the recrystallized structure and the non-recrystallized structure is suppressed as described above, and it is possible to avoid a decrease in roundness during punching and subsequent annealing.
  • the "original sheet of non-oriented electrical steel sheet” in this embodiment can be used as a motor core as it is.
  • the structure of the present embodiment is referred to as an "original plate”
  • the steel sheet is also expected to be used as it is as a non-oriented electrical steel sheet, which is a material for motor cores.
  • Crystal grain boundaries, crystal grain sizes, and crystal orientations are determined using "OIM Analysis Version 7.3.1" (manufactured by TSL) to obtain measured values.
  • Typical measurement conditions are a beam diameter of 1 ⁇ m and a crystal orientation likelihood of 10°.
  • the chemical composition of the non-oriented electrical steel sheet according to the present embodiment contains Si, optionally contains selective elements, and the balance consists of Fe and impurities. Each element will be described below.
  • C 0% or more and 0.0050% or less C (carbon) is an element that is contained as an impurity and deteriorates magnetic properties. Therefore, the C content should be 0.0050% or less. Preferably, it is 0.0030% or less. Since the C content is preferably small, there is no need to limit the lower limit, and the lower limit may be 0%. However, since it is not easy to make the content 0% industrially, the lower limit may be more than 0%, or 0.0010% or more.
  • Si 2.00% or more and 3.25% or less
  • Si is an element effective in increasing the specific resistance of the steel sheet and reducing iron loss. Therefore, the Si content should be 2.00% or more.
  • Si is an effective element for achieving both magnetic properties and mechanical anisotropy as a non-oriented electrical steel sheet.
  • the Si content is preferably more than 2.50%, more preferably 2.70% or more, further preferably 2.90% or more, and 3.00% or more. is more preferred.
  • an excessive Si content significantly lowers the magnetic flux density. Therefore, the Si content should be 3.25% or less.
  • the Si content is preferably 3.20% or less, more preferably 3.15% or less.
  • sol. Al 0% or more and 1.10% or less
  • Al aluminum
  • sol. Al content is less than 1.10%. sol.
  • sol. Al There is no need to limit the lower limit of Al, and the lower limit may be 0%. However, in order to more reliably obtain the effect of the above action, sol. It is preferable to set the Al content to 0.10% or more.
  • sol. Al means acid-soluble aluminum.
  • Mn 0% or more and 1.10% or less
  • Mn manganese
  • P 0% or more and 0.30% or less
  • P phosphorus
  • P is an element generally contained as an impurity.
  • P since it has the effect of improving the texture of the non-oriented electrical steel sheet and improving the magnetic properties, it may be contained as necessary.
  • P since P is also a solid-solution strengthening element, an excessive P content hardens the steel sheet and makes cold rolling difficult. Therefore, the P content should be 0.30% or less.
  • the P content is preferably 0.20% or less. There is no need to limit the lower limit of P, and the lower limit may be 0%. However, in order to more reliably obtain the effects of the above action, the P content is preferably 0.001% or more, more preferably 0.015% or more.
  • S 0% or more and 0.0100% or less S (sulfur) is contained as an impurity, combines with Mn in the steel to form fine MnS, inhibits the growth of grains during annealing, It degrades the magnetic properties of the electrical steel sheet. Therefore, the S content is set to 0.0100% or less.
  • the S content is preferably 0.0050% or less, more preferably 0.0030% or less. Since the S content is preferably small, there is no need to limit the lower limit, and the lower limit may be 0%. However, since it is not easy to reduce the content to 0% industrially, the lower limit may be set to 0.0001%.
  • N 0% or more and 0.0100% or less N (nitrogen) is contained as an impurity, combines with Al to form fine AlN, inhibits the growth of crystal grains during annealing, and degrades magnetic properties. Therefore, the N content is set to 0.0100% or less.
  • the N content is preferably 0.0050% or less, more preferably 0.0030% or less. Since the N content is preferably small, there is no need to limit the lower limit, and the lower limit may be 0%. However, since it is not easy to reduce the content to 0% industrially, the lower limit may be 0.0001% or more, may be more than 0.0015%, or may be 0.0020% or more.
  • Ti 0% or more and 0.1000% or less
  • Ti is an element that is unavoidably mixed in steel, and can combine with carbon or nitrogen to form precipitates (carbides, nitrides). When carbides or nitrides are formed, these precipitates themselves deteriorate the magnetic properties of the non-oriented electrical steel sheet. Furthermore, carbides or nitrides inhibit the growth of grains during final annealing, degrading the magnetic properties of the non-oriented electrical steel sheet. Therefore, the Ti content should be 0.1000% or less.
  • the Ti content is preferably 0.0100% or less, more preferably 0.0050% or less, even more preferably 0.0020% or less.
  • the Ti content may be 0%. Note that an extreme reduction in the Ti content may cause an increase in manufacturing costs, so the Ti content is preferably 0.0005% or more.
  • Ca 0% or more and 0.010% or less
  • Ca (calcium) suppresses the precipitation of fine sulfides (MnS, Cu 2 S, etc.) by forming coarse sulfides, so it is an effective choice for inclusion control. It is an element, and when added in an appropriate amount, it has the effect of improving crystal grain growth and improving magnetic properties (for example, iron loss). However, if it is contained excessively, the effects due to the above action become saturated, leading to an increase in cost. Therefore, the Ca content should be 0.010% or less.
  • the Ca content is preferably 0.008% or less, more preferably 0.005% or less. There is no need to limit the lower limit of Ca, and the lower limit may be 0%. However, in order to more reliably obtain the effects of the above action, the Ca content is preferably 0.0003% or more.
  • the Ca content is preferably 0.001% or more, more preferably 0.003% or more.
  • Cr 0% or more and 5.000% or less
  • Cr chromium
  • the Cr content is preferably 0.500% or less, more preferably 0.100% or less.
  • the lower limit may be 0%.
  • the Cr content is preferably 0.0010% or more in order to more reliably obtain the effects of the above action.
  • Ni 0% or more and 5.000% or less
  • Ni (nickel) is a selective element that improves magnetic properties (for example, saturation magnetic flux density).
  • the Ni content should be 5.000% or less.
  • the Ni content is preferably 0.500% or less, more preferably 0.100% or less.
  • the lower limit may be 0%.
  • the Ni content is preferably 0.0010% or more in order to more reliably obtain the effects of the above action.
  • Cu 0% or more and 5.000% or less
  • Cu (copper) is a selective element that improves the steel sheet strength.
  • the saturation magnetic flux density may be lowered, and the effect due to the above action is saturated, leading to an increase in cost. Therefore, the Cu content is set to 5.000% or less.
  • the Cu content is preferably 0.100% or less.
  • the lower limit may be 0%.
  • the Cu content is preferably 0.0010% or more in order to more reliably obtain the effects of the above action.
  • Sn 0% or more and 0.100% or less
  • Sb 0% or more and 0.100% or less
  • Sn (tin) and Sb (antimony) improve the texture of the non-oriented electrical steel sheet and improve the magnetic properties (e.g., magnetic flux density ), it may be contained as necessary. However, if it is contained excessively, it may embrittle the steel and cause cold-rolling fracture, and may deteriorate the magnetic properties. Therefore, the contents of Sn and Sb are each set to 0.100% or less. Sn and Sb do not need to have a lower limit, and the lower limit may be 0%. However, in order to more reliably obtain the effects of the above action, the Sn content is preferably 0.001% or more, more preferably 0.010% or more. The Sb content is preferably 0.001% or more, preferably 0.002% or more, more preferably 0.010% or more, and more than 0.025%. More preferred.
  • Ce 0% or more and 0.100% or less
  • Ce suppresses the precipitation of fine sulfides (MnS, Cu 2 S, etc.) by producing coarse sulfides and oxysulfides, and improves grain growth.
  • MnS, Cu 2 S, etc. fine sulfides
  • the Ce content should be 0.100% or less.
  • the Ce content is preferably 0.010% or less, more preferably 0.009% or less, and even more preferably 0.008% or less.
  • the Ce content is preferably 0.001% or more in order to more reliably obtain the effects of the above action.
  • the Ce content is more preferably 0.002% or more, more preferably 0.003% or more, and even more preferably 0.005% or more.
  • the chemical composition of the non-oriented electrical steel sheet according to the present embodiment includes, in addition to the above elements, selected elements such as B, O, Mg, Ti, V, Zr, Nd, Bi, W, Mo, Nb and Y may be contained.
  • selected elements such as B, O, Mg, Ti, V, Zr, Nd, Bi, W, Mo, Nb and Y may be contained.
  • the content of these selective elements may be controlled based on known knowledge. For example, the content of these selective elements may be as follows.
  • V 0% or more and 0.100% or less
  • Zr 0% or more and 0.100% or less
  • Nb 0% or more and 0.100% or less
  • B 0% or more and 0.100% or less
  • O 0% or more and 0.100% or less
  • Mg 0% or more and 0.100% or less
  • Nd 0% or more and 0.100% or less
  • Bi 0% or more and 0.100% or less
  • W 0% or more and 0.100% or less
  • Mo 0% or more and 0.100% or less
  • Y 0% or more and 0.100% or less.
  • the non-oriented electrical steel sheet according to the present embodiment has a chemical composition of, in mass%, C: 0.0010% or more and 0.0050% or less, sol. Al: 0.10% or more and less than 1.10%, Mn: 0.0010% or more and 1.10% or less, P: 0.0010% or more and 0.30% or less, S: 0.0001% or more and 0.0100% or less, N: more than 0.0015% and 0.0100% or less, Ti: 0.0001% or more and 0.1000% or less, V: 0.0001% or more and 0.100% or less, Zr: 0.0002% or more and 0.100% or less, Nb: 0.0001% or more and 0.100% or less, B: 0.0001% or more and 0.100% or less, O: 0.0001% or more and 0.100% or less, Mg: 0.0001% or more and 0.100% or less, Ca: 0.0003% or more and 0.010% or less, Cr: 0.0010% or more and 5.000% or less, Ni: 0.0010, sol
  • the B content is preferably 0.01% or less
  • the O content is preferably 0.01% or less
  • the Mg content is preferably 0.005% or less
  • the Ti content is preferably 0.002% or less
  • the V content is preferably 0.002% or less
  • the Zr content is preferably 0.002% or less
  • the Nd content is 0.01%
  • Bi content is preferably 0.01% or less
  • W content is preferably 0.01% or less
  • Nb content is preferably 0.002% or less
  • the Y content is 0.01% or less
  • the Ti content is preferably 0.001% or more
  • the V content is preferably 0.002% or more
  • the Nb content is preferably 0.002% or more.
  • the above chemical composition can be measured by a general analysis method for steel.
  • the chemical composition may be measured using ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry).
  • sol. Al can be measured by ICP-AES using the filtrate obtained by thermally decomposing the sample with acid.
  • Si uses the silicon dioxide gravimetric method
  • C and S use the combustion-infrared absorption method
  • N uses the inert gas melting-thermal conductivity method
  • O uses the inert gas melting-nondispersive infrared absorption method. It can be measured using the method.
  • the above chemical composition is the composition of a non-oriented electrical steel sheet that does not contain an insulating coating or the like. If the non-oriented electrical steel sheet used as the measurement sample has an insulating coating or the like on the surface, the measurement is performed after removing this.
  • the insulating coating or the like may be removed by the following method. First, a non-oriented electrical steel sheet having an insulating coating or the like is immersed in an aqueous sodium hydroxide solution, an aqueous sulfuric acid solution, and an aqueous nitric acid solution in that order, and then washed. Finally, it is dried with warm air. Thereby, a non-oriented electrical steel sheet from which the insulating coating is removed can be obtained. Alternatively, the insulating coating or the like may be removed by grinding.
  • non-oriented electrical steel sheet of the present embodiment may contain Sr, Ba, La, Pr, Zn and Cd in addition to the above elements.
  • Sr, Ba, La, Pr, Zn and Cd coarsen sulfides that inhibit grain growth and facilitate grain growth, so they are appropriately contained as necessary.
  • a non-oriented electrical steel sheet can be obtained by performing, for example, steelmaking, hot rolling, hot-rolled sheet annealing, pickling, cold rolling, and annealing on steel containing the above chemical components.
  • molten steel may be directly hot-rolled by a rapid solidification method, or a hot-rolled sheet may be obtained by thin slab casting and continuous hot rolling.
  • Hot-rolled sheet annealing is a process in which a hot-rolled sheet in which a worked structure remains is heated to 800-1050°C to recrystallize and grow grains. This makes it possible to create a texture favorable for magnetic properties after subsequent cold rolling and annealing.
  • hot-rolled sheet annealing may be performed in order not to cause surface unevenness called ridging in cold rolling, but hot-rolled sheet annealing is not performed in this embodiment. may
  • the hot-rolled sheet (or hot-rolled and annealed sheet) is cold-rolled to obtain a predetermined thickness.
  • the cold rolling may be a single cold rolling method without intermediate annealing, a double cold rolling method with intermediate annealing, or a multiple cold rolling method with multiple intermediate annealings.
  • annealing finish annealing
  • the insulating coating may be formed by applying an insulating material to the surface of the non-oriented electrical steel sheet and baking it.
  • the average grain size of the steel sheet before the final cold rolling is 200 ⁇ m or less, and the existence ratio of crystal grains exceeding 200 ⁇ m is 10% or less of the total grains.
  • the following conditions are particularly satisfied.
  • the average temperature increase rate in the temperature range of 700°C or higher is 50°C/second or more
  • the maximum temperature (annealing temperature) is 1050°C or less
  • the soaking time is 3 minutes or less.
  • the average heating rate in the temperature range of 700° C. or higher is 60° C./second or higher.
  • the maximum plate temperature is preferably 1000° C. or less.
  • the soaking time is preferably 2 minutes or less, more preferably 1 minute or less.
  • the annealing atmosphere in hot-rolled sheet annealing or intermediate annealing before final cold rolling is a dry nitrogen atmosphere.
  • the annealing atmosphere in hot-rolled sheet annealing or intermediate annealing before final cold rolling is preferably a dry nitrogen atmosphere.
  • the average grain size before and after final cold rolling may be measured by the cutting method specified in JIS G0551:2020.
  • a vertical cross-sectional structure photograph an average value of grain sizes measured by a cutting method in the plate thickness direction and the rolling direction may be used.
  • An optical microscopic photograph can be used as the longitudinal section structure photograph, and for example, a photograph taken at a magnification of 50 times may be used.
  • the presence ratio of ⁇ 100 ⁇ ⁇ 0vw> oriented grains in the steel sheet before the final cold rolling is 10% or less of the total crystal grains. meet.
  • the degree of superheat is preferably 15° C. or less, more preferably 10° C. or less, and even more preferably 5° C. or less.
  • the average cooling rate of 900° C. or higher in the cooling process is set to 20° C./second (72000° C./hr.) or less.
  • the average cooling rate is desirably 10°C/sec (36000°C/hr.) or less, more desirably 5°C/sec (18000°C/hr.) or less.
  • the heating temperature is set to 1100° C. or less and the heating time is set to 2 hours or less, preferably 1 hour or less.
  • the existence ratio of ⁇ 100 ⁇ 0vw> oriented grains is measured as follows. Using OIM Analysis Version 7.3.1 (manufactured by TSL), the area ratio of each oriented grain of interest is extracted from the observation field by a scanning electron microscope observed under the following measurement conditions (tolerance is 10 ° ). The extracted area is divided by the area of the observation field to obtain a percentage. Let this percentage be the area ratio of each oriented grain.
  • ⁇ Measuring device Scanning electron microscope with electron beam backscatter diffraction device (SEM-EBSD)
  • SEM Scanning electron microscope with electron beam backscatter diffraction device
  • SEM "JSM-6400" (manufactured by JEOL)
  • EBSD detector “HIKARI” (manufactured by TSL)
  • Step interval 2 ⁇ m
  • ⁇ Measurement object Center layer (1/2 plate thickness) of the Z plane of the steel plate (the cut surface of the steel plate cut in the plate thickness direction)
  • ⁇ Measurement area 8000 ⁇ m ⁇ 2400 ⁇ m area
  • ⁇ Grain boundary The angle difference in crystal orientation is 15 ° or more (a continuous region with an angle difference of less than 15 ° is regarded as one crystal grain)
  • the thickness of the non-oriented electrical steel sheet according to this embodiment may be 0.35 mm or less. More preferably, it is 0.30 mm or less. On the other hand, excessive thinning significantly reduces the productivity of steel sheets and motors, so the thickness is preferably 0.10 mm or more. More preferably, it is 0.15 mm or more. Moreover, the average crystal grain size of the non-oriented electrical steel sheet according to the present embodiment is 10 ⁇ m or more and 200 ⁇ m or less.
  • the plate thickness can be measured with a micrometer.
  • the non-oriented electrical steel sheet used as a measurement sample has an insulating film etc. on the surface, it measures after removing this.
  • Example 1 Regarding symbols 1F and 1G in Table 1, in mass %, Si: 3.00%, sol.
  • a steel containing 0.50% Al, 0.20% Mn, 0.01% C, and other inevitable impurities was melted and hot-rolled to a thickness of 2 mm.
  • the hot-rolled sheet was heated to the annealing temperature (1,000° C. to 1,200° C.) at the average heating rate shown in Table 1 and annealed for 2 minutes.
  • the hot-rolled sheet was decarburized with a wet hydrogen atmosphere as the annealing atmosphere.
  • a hot-rolled and annealed sheet having a metal structure shown in Table 1 and having a thickness of 2 mm was obtained.
  • the hot-rolled and annealed sheet was cold-rolled to a sheet thickness of 0.25 mm, and annealed at 750° C. for 30 seconds (finish annealing) to obtain a non-oriented electrical steel sheet.
  • Cold rolling was performed by a single cold rolling method.
  • Table 1 shows the annealing temperature, average heating rate, and annealing atmosphere of the hot-rolled and annealed sheets.
  • the average grain size of the raw sheet before the final cold rolling was measured and shown in Table 1.
  • a disk having a diameter of ⁇ 60 mm was punched from the obtained non-oriented electrical steel sheet with a die, subjected to strain relief annealing (core annealing) at 750° C.
  • Magnetic properties were evaluated in the following manner. First, a square sample of 16 ⁇ 16 mm was cut out from the obtained non-oriented electrical steel sheet for magnetic measurement. Then, the cut samples were subjected to stress relief annealing (core annealing) at 750° C. for 2 hours, and iron loss W10/400 and magnetic flux density B50 were measured. When the iron loss W10/400 was 14.0 W/kg or less and the magnetic flux density B50 was 1.65 T or more, the non-oriented electrical steel sheet had excellent magnetic properties and was judged to pass. On the other hand, when at least one of the iron loss W10/400 of 14.0 W/kg or more and the magnetic flux density B50 of 1.65 T or less was satisfied, the magnetic properties were evaluated as inferior and were rejected.
  • stress relief annealing core annealing
  • the ratio of the difference between the maximum value and the minimum value of the diameter of the disc to the average diameter is 0.200% or less, and is shown in Table 1 as a pass (invention example).
  • those having a ratio of the difference between the maximum diameter and the minimum diameter to the average diameter exceeding 0.200% are shown in Table 1 as failure (comparative example).
  • 1A and 1B have an average grain size of more than 200 ⁇ m in the steel plate before the final cold rolling, and the existence ratio of grains with a size of more than 200 ⁇ m is more than 10%, and the circularity after stress relief annealing is It was disqualified because it did not meet the evaluation criteria.
  • the temperature reached by hot-rolled sheet annealing exceeded 1050 ° C., so the average grain size of the steel sheet before the final cold rolling was over 200 ⁇ m, and the abundance ratio of crystal grains over 200 ⁇ m was 10%. It is considered super.
  • the existence ratio of crystal grains exceeding 200 ⁇ m was 10%, but the average crystal grain size of the steel sheet before the final cold rolling was over 200 ⁇ m, and the roundness after stress relief annealing was outside the evaluation criteria. was unsuccessful.
  • the temperature reached by the hot-rolled sheet annealing exceeded 1050° C., and therefore the average grain size of the steel sheet before the final cold rolling exceeded 200 ⁇ m.
  • the average crystal grain size of the steel sheet before the final cold rolling was 200 ⁇ m or less, but the existence ratio of crystal grains exceeding 200 ⁇ m was more than 10%, and the roundness after annealing was outside the evaluation criteria. , was unsuccessful.
  • the hot-rolled sheet annealing reached a temperature of 1050°C, but the annealing was performed in a humid hydrogen atmosphere, so it is considered that the existence ratio of crystal grains exceeding 200 ⁇ m exceeded 10%.
  • 1I was rejected because the roundness after strain relief annealing was out of the standard.
  • the average heating rate of hot-rolled sheet annealing was 45° C./second, so it is considered that the existence ratio of crystal grains exceeding 200 ⁇ m exceeded 10%.
  • the average grain size of the steel sheet before final cold rolling is 200 ⁇ m or less, and the abundance ratio of grains exceeding 200 ⁇ m is 10% or less, and the roundness after annealing satisfies the evaluation criteria, so it was passed.
  • the average grain size of the steel sheet before the final cold rolling becomes 200 ⁇ m or less and exceeds 200 ⁇ m. 10% or less of the total crystal grains, and the desired circularity can be obtained after punching.
  • all of 1D, 1E, 1H, 1J to 1N which are examples of the present invention, provide low iron loss and sufficient magnetic flux density (good magnetic properties).
  • Example 2 (Example 2) % by mass, Si: 3.00%, sol. Melt steel containing 0.50% Al, 0.20% Mn, 0.0020% C, and other unavoidable impurities, and adjust the deoxidation time to change the amount of oxygen in the molten steel. let me Molten steel was poured into a mold, and ingots were produced by changing the degree of superheat of the molten steel and the average cooling rate at 900° C. or higher as shown in Table 2. The average cooling rate was as shown in Table 2. After heating the ingot at 1,100° C. to 1,200° C. for 1 to 5 hours, it was hot rolled to a sheet thickness of 1.8 mm. The hot-rolled sheet was annealed at 1,050° C.
  • the hot-rolled and annealed sheet was cold-rolled to a sheet thickness of 0.20 mm, and annealed at 750° C. for 30 seconds (finish annealing) to obtain a non-oriented electrical steel sheet.
  • Cold rolling was performed by a single cold rolling method. A disk having a diameter of ⁇ 60 mm was punched from the obtained non-oriented electrical steel sheet with a die, subjected to strain relief annealing (core annealing) at 750° C. for 2 hours, and the roundness was measured before and after the annealing.
  • the ratio of the difference between the maximum and minimum diameters to the average diameter is 0.200% or less, and is shown in Table 2 as a pass (invention example). Also, in Table 2, samples with a ratio of the difference between the maximum diameter and the minimum diameter to the average diameter exceeding 0.200% were rejected (comparative examples).
  • 2A, 2B, 2F, and 2G had an abundance ratio of ⁇ 100 ⁇ ⁇ 0vw> oriented grains of more than 10%, and the circularity after stress relief annealing was out of the evaluation criteria, so they were disqualified.
  • the heating temperature of the ingot before hot rolling exceeded 1100° C.
  • the heating time exceeded 2 hours.
  • the heating time of the ingot was 2 hours, but the heating temperature exceeded 1100°C.
  • the heating temperature of the ingot was 1100°C, and the heating time was 1 hour. It is considered that the existence ratio of grains exceeded 10%.
  • 2C, 2D, 2E, 2H, 2K to 2N had ⁇ 100 ⁇ ⁇ 0vw> oriented grains at an abundance ratio of 10% or less, and the circularity after annealing satisfied the evaluation criteria, so they passed. From the above, by setting the ingot heating temperature to 1100° C. or less, the heating time to 1 hour or less, and the cooling rate to 20° C./second (72000° C./hr.) or less, the ⁇ 100 ⁇ It can be seen that the existence ratio of 0vw> oriented grains is 10% or less of the total crystal grains, and the desired roundness is obtained after punching.
  • Example 3 Regarding symbols 1F and 1G in Table 3, in mass %, Si: 3.00%, sol.
  • a steel containing 0.50% Al, 0.20% Mn, 0.01% C, and other inevitable impurities was melted and hot-rolled to a thickness of 2 mm.
  • the hot-rolled sheet was heated to the annealing temperature (1,000° C. to 1,200° C.) at the average heating rate shown in Table 1 and annealed for 2 minutes.
  • the hot-rolled sheet was decarburized with a wet hydrogen atmosphere as the annealing atmosphere.
  • a hot-rolled and annealed sheet having a metal structure shown in Table 3 and having a thickness of 2 mm was obtained.
  • the mass % Si 3.00%, sol.
  • a steel containing 0.50% Al, 0.20% Mn, 0.0020% C, and other unavoidable impurities was melted and hot-rolled to a thickness of 2 mm.
  • the hot-rolled sheet was heated to the annealing temperature (1,000° C. to 1,200° C.) at the average heating rate shown in Table 1 and annealed for 2 minutes.
  • the annealing atmosphere was a dry nitrogen atmosphere.
  • a hot-rolled and annealed sheet having a metal structure shown in Table 3 and having a thickness of 2 mm was obtained.
  • the hot-rolled and annealed sheet was cold-rolled to a sheet thickness of 0.25 mm, and annealed at 750° C. for 30 seconds (finish annealing) to obtain a non-oriented electrical steel sheet.
  • Cold rolling was performed by a single cold rolling method.
  • Table 3 "Conditions for production of raw sheet”, shows the annealing temperature, average heating rate, and annealing atmosphere of the hot-rolled and annealed sheet.
  • the average grain size of the raw sheet before the final cold rolling was measured and shown in Table 3.
  • a disk having a diameter of ⁇ 60 mm was punched from the obtained non-oriented electrical steel sheet with a die, subjected to stress relief annealing (core annealing) at 750° C.
  • the average crystal grain size of the steel sheet before the final cold rolling is over 200 ⁇ m
  • the existence ratio of crystal grains over 200 ⁇ m is over 10%
  • the circularity after stress relief annealing is outside the evaluation criteria. Therefore, it was unsuccessful.
  • the temperature reached by hot-rolled sheet annealing exceeded 1050 ° C., so the average grain size of the steel sheet before the final cold rolling was over 200 ⁇ m, and the abundance ratio of crystal grains exceeding 200 ⁇ m was 10%. It is considered super.
  • the existence ratio of crystal grains exceeding 200 ⁇ m was 10%, but the average crystal grain size of the steel sheet before the final cold rolling was over 200 ⁇ m, and the circularity after stress relief annealing was outside the evaluation criteria.
  • the average grain size of the steel sheet before the final cold rolling is 200 ⁇ m or less
  • the existence ratio of crystal grains exceeding 200 ⁇ m is 10% or less
  • the circularity after annealing satisfies the evaluation criteria. Therefore, it passed.
  • the average grain size of the steel sheet before the final cold rolling becomes 200 ⁇ m or less and exceeds 200 ⁇ m. 10% or less of the total crystal grains, and the desired circularity can be obtained after punching.
  • the roundness before strain relief annealing did not satisfy the evaluation criteria, but the average grain size of the steel sheet before the final cold rolling was 200 ⁇ m or less, and the abundance ratio of grains exceeding 200 ⁇ m was 10% or less. , and the circularity after stress relief annealing satisfied the evaluation criteria, so it was passed.
  • both the circularity before stress relief annealing and the circularity after stress relief annealing satisfy the evaluation criteria, and the circularity before stress relief annealing does not satisfy the evaluation criteria but after stress relief annealing Circularity that satisfies the evaluation criteria is included.
  • examples of the invention also include those whose roundness before stress relief annealing satisfies the evaluation criteria, including rotor cores that are not subjected to stress relief annealing. Therefore, in the invention examples, at least one of the circularity before stress relief annealing and the circularity after stress relief annealing satisfies the evaluation criteria.
  • Example 4 A steel containing the components shown in Tables 4A and 4B in mass % and containing other unavoidable impurities was melted and hot-rolled to a thickness of 2 mm.
  • the hot-rolled sheet was annealed at 1,050°C for 2 minutes.
  • the annealing atmosphere was a dry nitrogen atmosphere, and hot-rolled and annealed sheets with a thickness of 2 mm and having metallographic structures shown in Tables 4A and 4B were obtained.
  • the hot-rolled and annealed sheet was cold-rolled to a sheet thickness of 0.25 mm, and annealed at 750° C. for 30 seconds (finish annealing) to obtain a non-oriented electrical steel sheet.
  • Cold rolling was performed by a single cold rolling method.
  • the average grain size of the raw sheet before the final cold rolling and the existence ratio of grains of more than 200 ⁇ m were measured.
  • a disk having a diameter of ⁇ 60 mm was punched from the obtained non-oriented electrical steel sheet with a die, subjected to stress relief annealing (core annealing) at 750° C. for 2 hours, and the roundness before and after stress relief annealing was measured.
  • core annealing stress relief annealing
  • the ratio of the difference between the maximum and minimum diameters to the average diameter of 0.200% or less is shown in Table 5 as passing (invention example).
  • a 16 ⁇ 16 mm square sample for magnetic measurement was cut from the obtained non-oriented electrical steel sheet, subjected to strain relief annealing (core annealing) at 750 ° C. for 2 hours, and iron loss W10/400 and magnetic flux density B50 were measured. did.
  • core annealing strain relief annealing
  • iron loss W10/400 was 14.00 W/kg or less
  • the magnetic flux density B50 was 1.650 T or more
  • stator core 22 core back 23 tooth 30 rotor core 31 rotor iron core 32 magnet 50 case 60 shaft

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WO2026084308A1 (ko) * 2024-10-14 2026-04-23 현대제철 주식회사 무방향성 전기강판 및 무방향성 전기강판의 제조방법

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