WO2020149320A1 - 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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- WO2020149320A1 WO2020149320A1 PCT/JP2020/001139 JP2020001139W WO2020149320A1 WO 2020149320 A1 WO2020149320 A1 WO 2020149320A1 JP 2020001139 W JP2020001139 W JP 2020001139W WO 2020149320 A1 WO2020149320 A1 WO 2020149320A1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Definitions
- the present invention relates to a method for manufacturing a grain-oriented electrical steel sheet.
- the present application claims priority based on Japanese Patent Application No. 2019-005128 filed in Japan on January 16, 2019, the content of which is incorporated herein.
- Oriented electrical steel sheet is a soft magnetic material and is mainly used as an iron core material for transformers. Therefore, the grain-oriented electrical steel sheet is required to have magnetic properties such as high magnetization and low iron loss.
- 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.
- magnetic flux density represented by magnetic flux density B8 value when a magnetic field of 800 A/m is applied
- iron loss magnetic flux density 1.7 Tesla (T), frequency 50 Hertz (Hz).
- Energy loss W 17/50 (represented by W/kg) of 1) is required to be low.
- 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.
- Patent Document 1 Japanese Patent Publication No. 58-26405
- the present inventors observed the movement of the magnetic domains when the above-described magnetic domain subdivision was performed, it was found that some magnetic domains did not move. Therefore, in order to further reduce the iron loss value of the grain-oriented electrical steel sheet, the present inventors subdivide the magnetic domain and, at the same time, eliminate the pinning effect that inhibits the movement of the magnetic domain caused by the glass film on the surface of the steel sheet. Has come to be recognized as important.
- Patent Document 3 discloses a method in which coarse high-purity alumina is used as an annealing separator so as not to form a glass film on the surface of a steel sheet.
- W 15/60 the improvement margin of iron loss is W 15/60 of only 2% at most.
- Patent Document 4 JP-A-64-83620.
- methods such as chemical polishing/electrolytic polishing can process the material of the sample at the laboratory level, but in order to perform the above method on an industrial scale, the concentration of the chemical solution, the temperature control, and We must solve the problem of installation of pollution control equipment. Further, from the viewpoint of productivity, it is very difficult to put the above method into practical use.
- decarburization annealing is carried out in an atmosphere gas having an oxidation degree such that Fe-based oxides (Fe 2 SiO 4 , FeO, etc.) are not formed, and alumina is used as an annealing separator between the plates.
- Patent Document 5 JP-A-07-118750.
- the present invention has been made in view of the above problems, and provides a method for producing a grain-oriented electrical steel sheet having good magnetic properties while favorably performing decarburization in decarburization annealing.
- the purpose is to
- a method of manufacturing a grain-oriented electrical steel sheet according to an aspect of the present invention includes a silicon steel material manufacturing step of manufacturing a silicon steel material and a hot rolling step of hot rolling the silicon steel material to obtain a hot rolled sheet. And a cold rolling step in which the hot-rolled sheet is subjected to cold rolling once or multiple times of cold rolling sandwiching intermediate annealing to obtain a steel sheet having a final thickness, a heating zone and a soaking zone in the steel sheet.
- P1 may satisfy the following Expression 3. 0.3X+0.025 ⁇ P1 ⁇ 0.25X+0.15 ⁇ 0.20 (Formula 3)
- P1 and P2 may satisfy the following Expression 4.
- the silicon steel material is further mass% Cu: 0% or more and 0.4% or less.
- P 0% to 0.5%
- Ni 0% to 1.0%
- B 0% to 0.008%
- V 0% to 0.15%
- Nb 0% or more 0.20% or less
- Mo 0% or more and 0.10% or less
- Ti 0% or more and 0.015% or less
- Bi 0% or more and 0.010% or less
- the hot rolling is performed after the hot rolling step and before the cold rolling step.
- the method may further include a hot rolled sheet annealing step of annealing the hot rolled sheet obtained in the step.
- the numerical limit range includes a lower limit value and an upper limit value.
- the numerical value indicating “above” or “less than” is not included in the numerical range.
- “%” of chemical components in the following embodiments means “mass %”.
- a method of manufacturing a grain-oriented electrical steel sheet includes a silicon steel material manufacturing step of manufacturing a silicon steel material, a hot rolling step of hot rolling the silicon steel material to obtain a hot rolled sheet, and a hot rolling.
- the Cr content of the silicon steel material is X in mass%.
- the degree of oxidation P1 of the atmosphere gas in the heating zone satisfies the following expression 1
- the degree of oxidation P2 of the soaking atmosphere gas satisfies the following expression 2.
- the hot rolled sheet obtained by annealing the hot rolled sheet obtained in the hot rolling step is annealed. You may further include an annealing process. 0.18X ⁇ 0.008 ⁇ P1 ⁇ 0.25X+0.15 ⁇ 0.20 (Formula 1) 0.01 ⁇ P2 ⁇ 0.15 (Formula 2)
- the electric resistance becomes high and the iron loss characteristic is improved.
- the Si content exceeds 7.0%, cold rolling becomes extremely difficult and the steel material cracks during rolling. Therefore, the upper limit of the Si content is 7.0%.
- the upper limit of the Si content is preferably 4.5%, more preferably 4.0%.
- the Si content is less than 0.8%, ⁇ transformation occurs during finish annealing, and the crystal orientation of the steel sheet is impaired. Therefore, the lower limit of the Si content is 0.8%.
- the lower limit of the Si content is preferably 2.0%, more preferably 2.5%.
- the C is an element effective in controlling the primary recrystallized structure, but it adversely affects the magnetic properties, so it is necessary to remove it by performing decarburization treatment before finish annealing.
- the C content of the silicon steel material is more than 0.085%, the decarburization annealing time becomes long and the productivity in industrial production is impaired. Therefore, the upper limit of the C content is 0.085%.
- the upper limit of the C content is preferably 0.070%.
- the acid-soluble Al is an essential element in the method for manufacturing a grain-oriented electrical steel sheet according to the present embodiment in order to combine with N and serve as (Al,Si)N as an inhibitor.
- the acid-soluble Al content is set to 0.010 to 0.065% at which secondary recrystallization is stable.
- the lower limit of the acid-soluble Al content is preferably 0.020%, more preferably 0.025%.
- the upper limit of the acid-soluble Al content is preferably 0.040%, more preferably 0.030%.
- the N content does not exceed 0.012%. Further, in order to combine with Al and function as an inhibitor, the N content needs to be 0.004% or more.
- the lower limit of the N content is preferably 0.006%, more preferably 0.007%.
- the upper limit of the N content is preferably 0.010%, more preferably 0.009%.
- Mn and S be contained in a range such that Mn/S ⁇ 4.
- the Mn content is preferably 1.00% or less.
- the S content is preferably 0.050% or less, more preferably 0.015% or less, still more preferably 0.010% or less, still more preferably 0.007% or less.
- S can be partially replaced with Se. Therefore, when Se is included, S+Se: 0.050% or less is preferable, and Mn/(S+Se) ⁇ 4 is preferable.
- Mn and S may be used as inhibitors of secondary recrystallization.
- the Mn content at which the secondary recrystallization is stable is in the range of 0.02 to 0.30%.
- the lower limit of the Mn content is preferably 0.05%, more preferably 0.07%.
- the upper limit of the Mn content is preferably 0.15%, more preferably 0.10%.
- the preferable S content is in the range of 0.010 to 0.050%.
- the content of S is preferably 0.015% or more, more preferably 0.020% or more.
- the S content is more preferably 0.040% or less.
- S can be replaced by Se.
- Mn and S are utilized as inhibitors of secondary recrystallization.
- Komatsu et al. for example, Japanese Patent Publication No. 62-45285
- Mn and S are not used as inhibitors of secondary recrystallization.
- Cr is an element that affects the behavior of oxide layer formation during decarburization annealing, improves decarburization, and promotes subsequent surface smoothing.
- the Cr content is 0.02 to 0.50% at which the effect of improving the decarburizing property is obtained.
- the lower limit of the Cr content is 0.05% and preferably the upper limit of the Cr content is 0.39%.
- a component of the silicon steel material in addition to the above components, if necessary, further selected from the group consisting of Cu, Ni, P, Mo, Bi, B, V, Nb and Ti 1 % Or more of Cu, 0 to 0.4%, Ni: 0 to 1.0%, P: 0 to 0.5%, Mo: 0 to 0.10%, Bi:0 May be contained in the range of up to 0.010%, B:0 to 0.008%, V:0 to 0.15%, Nb:0 to 0.20%, and Ti:0 to 0.015%.
- Cu 0% or more and 0.4% or less
- Cu (copper) is an element effective in increasing the electric resistance and reducing the iron loss. Therefore, Cu may be contained in the range of the content of 0.4% or less. When the Cu content exceeds 0.4%, the effect of reducing iron loss is saturated, and surface defects such as "copper hegginess" may occur during hot rolling.
- the lower limit of the Cu content is preferably 0.05%, more preferably 0.1%.
- the upper limit of the Cu content is preferably 0.3%, more preferably 0.2%.
- Ni 0% or more and 1.0% or less
- Ni nickel
- Ni is an element effective in increasing the electric resistance and reducing the iron loss. Further, Ni is an element effective in controlling the metallographic structure of the hot rolled sheet and enhancing the magnetic properties. Therefore, Ni may be contained in the range of the content of 1.0% or less. If the Ni content exceeds 1.0%, the secondary recrystallization may become unstable.
- the lower limit of the Ni content is preferably 0.01%, more preferably 0.02%.
- the upper limit of the Ni content is preferably 0.2%, more preferably 0.1%.
- P 0% or more and 0.5% or less
- P is an element effective in increasing the electric resistance and reducing the iron loss. Therefore, P may be contained in the range of the content of 0.5% or less. If the P content exceeds 0.5%, there may be a problem in the rollability of the silicon steel sheet.
- the lower limit of the P content is preferably 0.005%, more preferably 0.01%.
- the upper limit of the P content is preferably 0.2%, more preferably 0.15%.
- Mo 0% or more and 0.10% or less Mo (molybdenum) is also an element effective in increasing the electric resistance and reducing the iron loss. Therefore, Mo may be contained in the range of the content of 0.10% or less. If the Mo content exceeds 0.10%, problems may occur in the rollability of the steel sheet.
- the lower limit of the Mo content is preferably 0.005%, more preferably 0.01%.
- the upper limit of the Mo content is preferably 0.08%, more preferably 0.05%.
- Bi 0% or more and 0.010% or less Bi (bismuth) is an element effective in stabilizing precipitates such as sulfides and strengthening the function as an inhibitor. Therefore, Bi may be contained in the range of the content of 0.010% or less. If the Bi content exceeds 0.010%, the magnetic properties may deteriorate.
- the lower limit of the Bi content is preferably 0.001%, more preferably 0.002%.
- the upper limit of the Bi content is preferably 0.008%, more preferably 0.006%.
- B 0% or more and 0.008% or less B (boron) is an effective element that exhibits an inhibitory effect as BN. Therefore, B may be contained in the range of the content of 0.008% or less. If the B content exceeds 0.008%, the magnetic properties may deteriorate.
- the lower limit of the B content is preferably 0.0005%, more preferably 0.001%.
- the upper limit of the B content is preferably 0.005%, more preferably 0.003%.
- V 0% or more and 0.15% or less
- Nb 0% or more and 0.20% or less
- Ti 0% or more and 0.015% or less
- V (vanadium), Nb (niobium), and Ti (titanium) are N and C. It is an effective element that binds to and functions as an inhibitor. Therefore, V may be contained in an amount of 0.15% or less, Nb of 0.2% or less, and/or Ti of 0.015% or less. If these elements remain in the final product and the V content exceeds 0.15%, the Nb content exceeds 0.20%, or the Ti content exceeds 0.015%, the magnetic properties deteriorate. May occur.
- the lower limit of the V content is preferably 0.002%, more preferably 0.01%.
- the upper limit of the V content is preferably 0.10%, more preferably 0.05%.
- the lower limit of the Nb content is preferably 0.005%, more preferably 0.02%.
- the upper limit of the Nb content is preferably 0.10%, more preferably 0.08%.
- the lower limit of the Ti content is preferably 0.002%, more preferably 0.004%.
- the upper limit of the Ti content is preferably 0.010%, more preferably 0.008%.
- a molten steel having the above-mentioned chemical composition is cast (S100) to obtain a silicon steel material, and this silicon steel material is formed into a hot rolled sheet by a normal hot rolling step (S102).
- molten steel may be continuously cast into a ribbon.
- the hot-rolled sheet or the continuously cast ribbon is immediately or after being subjected to the hot-rolled sheet annealing step (S104), is subjected to the cold rolling step (S106).
- the annealing in the hot rolled sheet annealing step (S104) may be performed in the temperature range of 750 to 1200° C. for 30 seconds to 30 minutes.
- the hot rolled sheet annealing process is effective to enhance the magnetic properties of the product.
- the presence/absence of the hot rolled sheet annealing step may be determined according to the properties and the manufacturing cost required for the grain-oriented electrical steel sheet to be finally manufactured, and the hot rolled sheet annealing step may be omitted.
- the cold rolling in the cold rolling step (S106) is performed once or by a plurality of cold rollings including annealing.
- the rolling reduction is preferably 80% or more.
- the final cold rolling after the final annealing has a reduction ratio of 80% or more.
- the cold-rolled sheet obtained by this step is a steel sheet having a final thickness.
- the material after cold rolling undergoes a decarburization annealing step (S108) in order to remove carbon contained in steel.
- a decarburizing annealing furnace including a heating zone and a soaking zone is used to perform decarburizing annealing in a wet hydrogen atmosphere.
- the atmosphere gas in the decarburization annealing step (S108) is controlled to be an annealing degree at which an iron (Fe)-based oxide is not formed and then annealed.
- the degree of oxidation P1 of the atmosphere gas in the heating zone in the decarburization annealing step (S108) is controlled so as to satisfy the following expression 1. 0.18X ⁇ 0.008 ⁇ P1 ⁇ 0.25X+0.15 ⁇ 0.20 (Formula 1)
- X represents the Cr content (mass %) of the silicon steel material
- P1 represents the degree of oxidation of the atmosphere gas in the heating zone in the decarburization annealing step (S108).
- the degree of oxidation P1 is the degree of oxidation represented by the ratio " PH2O / PH2 " of the partial pressure of water vapor to the partial pressure of hydrogen in the atmospheric gas containing hydrogen, nitrogen, and water vapor.
- an initial oxide film containing Cr oxide is formed on the outermost surface of the steel sheet in the heating zone, It is considered that decarburization progresses favorably. It is considered that the iron-based oxide film reacts with an annealing separating agent such as alumina which is applied in a later step to inhibit surface smoothing. Decarburization is rate-controlled by the initial oxide film that is first formed on the surface in the heating zone. However, when Cr is contained, the Cr oxide deteriorates the initial oxide film and improves the decarburization property. Conceivable.
- the degree of oxidation P2 of the soaking zone atmosphere gas in the decarburization annealing step (S108) is controlled so as to satisfy the following expression 2. 0.01 ⁇ P2 ⁇ 0.15 (Formula 2)
- the degree of oxidation P2 is the degree of oxidation represented by the ratio " PH2O2 / PH2 " of the partial pressure of water vapor to the partial pressure of hydrogen in the atmospheric gas containing hydrogen, nitrogen, and water vapor.
- Fe-based oxide Fe 2 Annealing is preferably performed at an oxidation degree that does not form (SiO 4 , FeO, etc.).
- the Fe-based oxide is adjusted by adjusting the oxidation degree P2 (P H2O 2 /P H2 ) of the atmosphere gas in the soaking zone to 0.15 or less. Can be suppressed.
- the degree of oxidation P2 of the soaking atmosphere gas exceeds 0.15, inclusions are formed below the surface of the product, which becomes an obstacle to lowering iron loss. However, if the degree of oxidation P2 is lowered too much, the decarburization rate becomes slow. Considering both of them, in this temperature range, the degree of oxidation P2 (P H2O /P H2 ) of the soaking atmosphere gas is preferably in the range of 0.01 to 0.15.
- the oxidation degree P1 of the atmosphere gas in the heating zone satisfies the following expression 3. 0.3X+0.025 ⁇ P1 ⁇ 0.25X+0.15 ⁇ 0.20 (Formula 3)
- X represents the Cr content (mass %) of the silicon steel material.
- the degree of oxidation P1 of the atmosphere gas in the heating zone and the degree of oxidation P2 of the soaking zone atmosphere gas satisfy the following expression 4. Is more preferable. P1>P2 (Formula 4)
- the rate of temperature increase from room temperature to the temperature in the soaking zone is preferably 7°C/sec or more on average, and more preferably 9°C/sec or more. If the rate of temperature rise is too slow, the decarburizing property deteriorates. Further, although it is not necessary to specify the upper limit, if it is too fast, it becomes difficult to control the soaking temperature.
- the temperature in the soaking zone and the holding time in the soaking zone are preferably 750 to 900°C and 10 to 600 seconds. If the soaking temperature (annealing temperature) is lower than 750° C., the decarburization rate becomes slow and the productivity decreases. On the other hand, if it exceeds 900° C., the primary recrystallized grain size exceeds the desired size, so that the magnetic properties after finish annealing deteriorate. Further, if the holding time is less than 10 seconds, decarburization cannot be sufficiently performed. On the other hand, if it exceeds 600 seconds, the productivity decreases.
- a nitriding step (S110) may be included between before the decarburization annealing step (S108) and before the secondary recrystallization in the finish annealing step (S112).
- the method of this nitriding treatment is not particularly limited, and there are a method of performing it in an atmosphere gas having a nitriding ability such as ammonia and a method of adding a nitride having a nitriding ability to the annealing separator.
- a nitriding ability such as ammonia
- a method of adding a nitride having a nitriding ability to the annealing separator for example, in the nitriding treatment step (S110), nitriding treatment by Komatsu et al., which uses (Al,Si)N as a main inhibitor (Japanese Patent Publication No. 62-45285), is preferably used.
- an annealing separating agent containing alumina as a main component (containing 50% by mass or more of alumina) is applied to the steel sheet.
- the annealing separator preferably contains 5 to 50% by mass of magnesia in addition to alumina.
- the inclusion of magnesia suppresses the formation of inclusions such as mullite (3Al 2 O 3 .2SiO 2 ) on the surface of the steel sheet, and the iron loss is stably improved.
- the surface of the steel sheet having an oxide layer is coated with the above-described annealing separator containing alumina as a main component, dried, and then wound into a coil, and finish annealing (secondary recrystallization annealing is performed. ).
- an annealing separator containing alumina as the main component When an annealing separator containing alumina as the main component is used, it is possible to suppress the formation of a film of an inorganic mineral substance such as forsterite on the surface of the steel sheet even if finish annealing is performed.
- the annealing separator when laminating (coiling) decarburized annealing plates, apply the annealing separator whose main component is alumina, which is difficult to react with silica, in water slurry or by electrostatic coating method. Is preferred.
- This laminated decarburized annealed plate is finish annealed to perform secondary recrystallization and purification of nitrides, sulfides and the like. It is effective to increase the magnetic flux density by performing the secondary recrystallization in a predetermined temperature range by holding the secondary recrystallization at a constant temperature.
- the finish annealing may be carried out under the condition that the temperature is raised to 1150 to 1250° C.
- the annealing is performed for 10 to 30 hours in an atmosphere gas containing hydrogen and nitrogen.
- an atmosphere gas containing hydrogen and nitrogen it is preferable to anneal at a temperature of 1100° C. or higher in a 100% hydrogen atmosphere. After the finish annealing as described above, the surface becomes mirror-like and the iron loss can be greatly reduced.
- an insulating film that gives tension to the steel sheet is formed on the surface of the steel sheet.
- magnetic domain subdivision processing may be performed between the above-mentioned steps by a mechanical method such as a tooth profile, a chemical method such as etching, laser irradiation or electron beam irradiation.
- controlling the degree of oxidation and annealing is a main feature of the method for manufacturing a grain-oriented electrical steel sheet according to the embodiment of the present invention. ..
- a nitriding process step may be further included. Specifically, whether the nitriding process is performed independently before the decarburization annealing process, or in the decarburization annealing process in one or more steps of heating, soaking, and cooling. Alternatively, it may be carried out independently after the deannealing step, or by adding a nitrogen compound to the annealing separator before the secondary recrystallization in the finish annealing step.
- the grain-oriented electrical steel sheet obtained by the manufacturing method of the above-described embodiment can be mainly used as an iron core of a transformer or other electric equipment.
- the inventors of the present invention considered that the decarburization behavior on the surface of the silicon steel sheet had a great influence on the subsequent decarburization behavior by the oxide layer formed in the initial stage of decarburization annealing, and conducted various experiments related thereto. went.
- Example 1 The mass obtained by casting is Si: 3.3%, Mn: 0.14%, C: 0.05%, S: 0.007%, acid-soluble Al: 0.027%, N: 0.008. %, and the remaining silicon steel slab consisting of Fe and impurities was heated and then hot-rolled to a plate thickness of 2.0 mm. The hot-rolled sheet was heated to 1100° C., cooled to 900° C., annealed for 30 seconds, and then cold-rolled once so that the final sheet thickness was 0.22 mm.
- This cold-rolled sheet was heated in an atmosphere gas containing 75% hydrogen and 25% nitrogen to change the degree of oxidation (P H2O /P H2 ) by changing the dew point, and the heating rate up to 830°C at a heating rate of 7°C/sec.
- Decarburization annealing was performed by raising the temperature and holding it for 120 seconds.
- the degree of oxidation of the heating zone is equal to that of soaking.
- the amount of nitrogen in the steel was increased to 0.02 mass% (nitriding treatment) in ammonia gas to strengthen the inhibitor.
- This decarburized annealed plate was coated with an annealing separator containing alumina as a main component (80% by mass of alumina+20% by mass of magnesia) in the form of a water slurry, and then in an atmosphere gas containing 75% of hydrogen and 25% of nitrogen. After that, the temperature was raised to 1200° C., the atmosphere was changed to 100% hydrogen atmosphere gas, and then the final annealing was performed at 1200° C. for 20 hours.
- the reason why the amount of carbon is not reduced to 0.0030% or less depends on the quality and morphology of the oxide formed on the surface of the steel sheet during the heating process of decarburization annealing.
- a decarburization (oxidation of carbon in steel) reaction and an oxide formation of silica or the like (oxidation of silicon in steel) are generally performed in competition with moisture in the atmosphere. From the results of Example 1, it is considered that when annealing is performed in a low-oxidation atmosphere gas in which iron-based oxides are not formed, silica on the surface of the steel sheet is generally formed in a dense film and inhibits decarburization.
- Example 2 Further, other oxide forming elements were examined, and it was examined that by containing an appropriate amount of Cr, Cr oxide was formed on the surface of the steel sheet, and the decarburization reaction was promoted by suppressing the silica formation reaction. The result will be described below as a second embodiment.
- the mass obtained by casting is Si: 3.3%, Mn: 0.14%, C: 0.05%, S: 0.007%, acid-soluble Al: 0.027%, N: 0.008. %, Cr: 0.12%, and the silicon steel slab containing the balance Fe and impurities was heated and then hot-rolled to a plate thickness of 2.0 mm.
- the hot-rolled sheet was heated to 1100° C., cooled to 900° C., annealed for 30 seconds, and then cold-rolled once so that the final sheet thickness was 0.22 mm.
- This cold-rolled sheet was heated in an atmosphere gas containing 75% hydrogen and 25% nitrogen to change the degree of oxidation (P H2O /P H2 ) by changing the dew point, and the heating rate up to 830°C at a heating rate of 7°C/sec.
- Decarburization annealing was performed by raising the temperature and holding it for 120 seconds.
- the degree of oxidation of the heating zone and the degree of oxidation of the soaking zone are equal.
- the amount of nitrogen in steel was increased to 0.02 mass% in ammonia gas to strengthen the inhibitor.
- This decarburized annealed plate was coated with an annealing separator containing alumina as a main component (50% by mass of alumina+50% by mass of magnesia) in the form of a water slurry, and then in an atmosphere gas containing 75% of hydrogen and 25% of nitrogen. The temperature was raised to 1200° C., after which the atmosphere gas was switched to 100% hydrogen, and the final annealing was performed at 1200° C. for 20 hours.
- alumina as a main component
- the mass obtained by casting is Si: 3.3%, Mn: 0.14%, C: 0.05%, S: 0.007%, acid-soluble Al: 0.027%, N: 0.008. %, Cr: 0 to 0.62%, and a silicon steel slab containing the balance Fe and impurities was heated and then hot-rolled to a plate thickness of 2.0 mm.
- the hot-rolled sheet was heated to 1100° C., cooled to 900° C., annealed for 30 seconds, and then cold-rolled once so that the final sheet thickness was 0.22 mm.
- the temperature was raised to 830°C.
- Decarburization annealing was performed at 830° C. for 120 seconds with the atmospheric gas oxidation degree (P2) set to 0.06.
- the amount of nitrogen in steel was increased to 0.02 mass% in ammonia gas to strengthen the inhibitor.
- This decarburized annealed plate was coated with an annealing separator containing alumina as a main component (70% by mass of alumina+30% by mass of magnesia) in the form of a water slurry, and then in an atmosphere gas containing 75% of hydrogen and 25% of nitrogen. Then, the temperature was raised to 1200° C. and then the atmosphere was switched to 100% hydrogen atmosphere gas, and the final annealing was performed at 1200° C. for 20 hours.
- the sample produced by the above steps was washed with water, sheared with the sample, further annealed for strain relief, further formed with an insulating coating (tension coating was applied), laser irradiation was performed, and the magnetic field was measured by the SST method. The measurement was performed.
- FIG. 2 is a diagram showing the relationship between the Cr content X (mass %) and the atmospheric gas oxidation degree P1 of the heating zone of decarburization annealing, which affects the carbon content after decarburization annealing and the iron loss of the product. ..
- the plot of “ ⁇ ” is a good experimental example in which the carbon content is 0.0030% or less and the iron loss (W 17/50 ) is 0.65 (W/kg) or less, and the plot of “ ⁇ ” is shown.
- the plot of " ⁇ " shows that the carbon content is 0.0030%.
- the iron loss (W 17/50 ) is 0.70 or less will be shown.
- the plot of “x” indicates an experimental example in which the carbon content is more than 0.0030% or the iron loss (W 17/50 ) is more than 0.70 (W/kg).
- the remaining hot-rolled sheet was cold-rolled to a sheet thickness of 2.0 mm without annealing the hot-rolled sheet, heated to 1120° C., cooled to 950° C., and held for 30 seconds (intermediate annealing). Then, it cold-rolled so that final board thickness might be set to 0.22 mm (process B). The cold rolling rate after the final annealing was 89% in each case.
- This cold-rolled sheet was heated to a temperature of 830° C. at a heating rate of 30° C./sec in an atmosphere gas containing 75% hydrogen and 25% nitrogen at an oxidation degree of 0.06 (PH 2 O 2 /PH 2 ). Decarburization annealing was performed for 120 seconds. In Example 4, the degree of oxidation of the heating zone and the degree of oxidation of the soaking zone are equal.
- the amount of nitrogen in steel was increased to 0.025 mass% in ammonia gas to strengthen the inhibitor.
- This decarburized annealed plate was coated with an annealing separator containing alumina as a main component (alumina 90% by mass+magnesia 10% by mass) in the form of a water slurry, and then in an atmosphere gas containing 75% hydrogen and 25% nitrogen. The temperature was raised to 1200° C., after which the atmosphere gas was switched to 100% hydrogen, and the final annealing was performed at 1200° C. for 20 hours.
- alumina alumina 90% by mass+magnesia 10% by mass
- Example 5 Furthermore, the influence of the composition of the silicon steel slab on the properties was examined. The results will be described below as Example 5.
- a silicon steel slab containing the components shown in Table 4 obtained by casting and consisting of the balance Fe and impurities was heated and then hot-rolled to a plate thickness of 2.3 mm.
- the hot rolled sheet was heated to 1120° C., cooled to 950° C., annealed for 30 seconds, and then cold-rolled once so that the final sheet thickness was 0.22 mm.
- This cold-rolled sheet was heated to a temperature of 830° C. in an atmosphere gas containing 75% of hydrogen and 25% of nitrogen at an oxidation degree of 0.10 (PH 2 O 2 /PH 2 ) at a heating rate of 30° C./sec. Then, decarburization annealing was performed by switching to an oxidation degree of 0.06 (P H2O /P H2 ) and holding for 120 seconds.
- the amount of nitrogen in steel was increased to 0.025 mass% in ammonia gas to strengthen the inhibitor.
- This decarburized annealed plate was coated with an annealing separator containing alumina as a main component (60% by mass of alumina+40% by mass of magnesia) in the form of a water slurry, and then in an atmosphere gas containing 75% of hydrogen and 25% of nitrogen. The temperature was raised to 1200° C., after which the atmosphere gas was switched to 100% hydrogen, and the final annealing was performed at 1200° C. for 20 hours.
- alumina as a main component
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Abstract
Description
本願は、2019年01月16日に、日本に出願された特願2019-005128号に基づき優先権を主張し、その内容をここに援用する。
0.18X-0.008≦P1≦0.25X+0.15≦0.20 (式1)
0.01≦P2≦0.15 (式2)
0.3X+0.025≦P1≦0.25X+0.15≦0.20 (式3)
P1>P2 (式4)
また、以下の実施形態の独立した各要素は、本発明の範囲において、互いに組み合わせ可能であることも自明である。
また、特に断りのない限り、以下の実施形態における化学成分の「%」は「質量%」を意味する。
0.18X-0.008≦P1≦0.25X+0.15≦0.20 (式1)
0.01≦P2≦0.15 (式2)
Siは、含有量を多くすると電気抵抗が高くなり、鉄損特性が改善される。しかし、Si含有量が7.0%を超えると冷延が極めて困難となり、圧延時に鋼素材割れてしまう。そのため、Si含有量の上限を7.0%とする。Si含有量の上限は好ましくは4.5%、さらに好ましくは4.0%である。
また、Si含有量が0.8%より少ないと、仕上げ焼鈍時にγ変態が生じ、鋼板の結晶方位が損なわれてしまう。そのため、Si含有量の下限を0.8%とする。Si含有量の下限は、好ましくは2.0%、さらに好ましくは2.5%である。
珪素鋼素材のC含有量が0.085%より多いと、脱炭焼鈍時間が長くなり、工業生産における生産性が損なわれてしまう。そのため、C含有量の上限を0.085%とする。C含有量の上限は、好ましくは0.070%である。
酸可溶性Al含有量の下限は、好ましくは0.020%、さらに好ましくは0.025%である。酸可溶性Al含有量の上限は、好ましくは0.040%、さらに好ましくは0.030%である。
また、Sはその一部をSeで置き換えることができる。そのため、Seを含む場合、S+Se:0.050%以下であることが好ましく、Mn/(S+Se)≧4となる範囲であることが好ましい。
一方、小松等による製造法(たとえば特公昭62-45285号公報)においては、MnとSとは、二次再結晶のインヒビターとして用いない。
Cr含有量は、脱炭性の改善効果が得られる0.02~0.50%とする。好ましくは、Cr含有量の下限は、0.05%であり、好ましくは、Cr含有量の上限は、0.39%である。
Cu(銅)は、電気抵抗を高めて鉄損を低減するのに有効な元素である。従って、Cuを0.4%以下の含有量の範囲で含有させてもよい。Cu含有量が0.4%を超えると、鉄損低減効果が飽和してしまうとともに、熱間圧延時に“カッパーヘゲ”という表面疵の原因になることがある。Cu含有量の下限は、0.05%であることが好ましく、0.1%であることがより好ましい。Cu含有量の上限は、0.3%であることが好ましく、0.2%であることがより好ましい。
Ni(ニッケル)は、電気抵抗を高めて鉄損を低減するのに有効な元素である。また、Niは、熱延板の金属組織を制御して、磁気特性を高めるうえで有効な元素である。従って、Niを1.0%以下の含有量の範囲で含有させてもよい。Ni含有量が1.0%を超えると、二次再結晶が不安定になることがある。Ni含有量の下限は、0.01%であることが好ましく、0.02%であることがより好ましい。Ni含有量の上限は、0.2%であることが好ましく、0.1%であることがより好ましい。
P(燐)は、電気抵抗を高めて鉄損を低減するのに有効な元素である。従って、Pを0.5%以下の含有量の範囲で含有させてもよい。P含有量が0.5%を超えると、珪素鋼板の圧延性に問題が生じることがある。P含有量の下限は、0.005%であることが好ましく、0.01%であることがより好ましい。P含有量の上限は、0.2%であることが好ましく、0.15%であることがより好ましい。
Mo(モリブデン)も、電気抵抗を高めて鉄損を低減するのに有効な元素である。従って、Moを0.10%以下の含有量の範囲で含有させてもよい。Mo含有量が0.10%を超えると、鋼板の圧延性に問題が生じることがある。Mo含有量の下限は、0.005%であることが好ましく、0.01%であることがより好ましい。Mo含有量の上限は、0.08%であることが好ましく、0.05%であることがより好ましい。
Bi(ビスマス)は、硫化物等の析出物を安定化してインヒビターとしての機能を強化するのに有効な元素である。従って、Biを0.010%以下の含有量の範囲で含有させてもよい。Bi含有量が0.010%を超えると、磁気特性が劣化することがある。Bi含有量の下限は、0.001%であることが好ましく、0.002%であることがより好ましい。Bi含有量の上限は、0.008%であることが好ましく、0.006%であることがより好ましい。
B(ホウ素)は、BNとしてインヒビター効果を発揮する有効な元素である。従って、Bを0.008%以下の含有量の範囲で含有させてもよい。B含有量が0.008%を超えると、磁気特性が劣化するおそれがある。B含有量の下限は、0.0005%であることが好ましく、0.001%であることがより好ましい。B含有量の上限は、0.005%であることが好ましく、0.003%であることがより好ましい。
Nb:0%以上0.20%以下
Ti:0%以上0.015%以下
V(バナジウム)、Nb(ニオブ)、及びTi(チタン)は、NやCと結合してインヒビターとして機能する、有効な元素である。従って、Vを0.15%以下、Nbを0.2%以下、および/またはTiを0.015%以下の含有量の範囲で含有させてもよい。これらの元素が最終製品に残留して、V含有量が0.15%を超え、Nb含有量が0.20%を超え、またはTi含有量が0.015%を超えると、磁気特性が劣化するおそれがある。
V含有量の下限は、0.002%であることが好ましく、0.01%であることがより好ましい。V含有量の上限は、0.10%であることが好ましく、0.05%であることがより好ましい。
Nb含有量の下限は、0.005%であることが好ましく、0.02%であることがより好ましい。Nb含有量の上限は、0.10%であることが好ましく、0.08%であることがより好ましい。
Ti含有量の下限は、0.002%であることが好ましく、0.004%であることがより好ましい。Ti含有量の上限は、0.010%であることが好ましく、0.008%であることがより好ましい。
上述した化学組成の珪素鋼素材から{110}<001>方位に発達した集合組織を有する方向性電磁鋼板を製造するためには、次のような工程を経る。
熱延板焼鈍工程(S104)における焼鈍は、750~1200℃の温度域で30秒~30分間行われてもよい。
0.18X-0.008≦P1≦0.25X+0.15≦0.20 (式1)
脱炭焼鈍工程(S108)における加熱帯の雰囲気ガスの酸化度P1を上記の式1で規定することで、加熱帯において鋼板最表面にCr酸化物を含有する形態の初期酸化膜が形成され、脱炭が好ましく進行すると考えられる。鉄系酸化膜は、たとえば後工程で塗布されるアルミナなどの焼鈍分離剤と反応して、表面平滑化を阻害すると考えられる。脱炭性は、加熱帯で最初に表面に形成される初期酸化膜に律速されるが、Crを含有させることで、Cr酸化物が初期酸化膜を変質させ、脱炭性が改善されると考えられる。
0.01≦P2≦0.15 (式2)
0.3X+0.025≦P1≦0.25X+0.15≦0.20 (式3)
式3中で、Xは珪素鋼素材のCr含有量(質量%)を表す。
P1>P2 (式4)
たとえば、窒化処理工程(S110)は、小松等による(Al,Si)Nを主インヒビタ-として用いる製造法(特公昭62-45285号公報)等)の窒化処理が好ましく用いられる。
仕上げ焼鈍工程では、酸化層を有する鋼板の表面に、上記のアルミナを主成分とする焼鈍分離剤を塗布して乾燥させ、乾燥後、コイル状に巻き取って、仕上げ焼鈍(二次再結晶焼鈍)に供する。
この積層した脱炭焼鈍板を仕上げ焼鈍して、二次再結晶と窒化物や硫化物などの純化とを行う。二次再結晶を、一定の温度で保持する等の手段により所定の温度域で行うことは、磁束密度を上げるうえで有効である。
仕上げ焼鈍は例えば水素及び窒素を含有する雰囲気ガス中で、1150~1250℃まで昇温し、10~30時間焼鈍する条件で行えばよいが、窒化物や硫化物などの純化等を行う場合、二次再結晶完了後、100%水素雰囲気中で1100℃以上の温度で焼鈍することが好ましい。
上記のような仕上げ焼鈍後、表面が鏡面状となり、鉄損を大きく低下させることができる。
鋳造によって得られた質量で、Si:3.3%、Mn:0.14%、C:0.05%、S:0.007%、酸可溶性Al:0.027%、N:0.008%を含有し、残部Feおよび不純物からなる珪素鋼スラブを加熱後、板厚2.0mmまで熱間圧延した。この熱延板を1100℃に加熱後900℃に降温して30秒保持する焼鈍を実施した後、最終板厚が0.22mmとなるように1回の冷間圧延を行った。
しかしながら、鋼中炭素量が0.0030%(30ppm)超となっているために、磁気時効(経時変化に伴う磁気特性の劣化)の懸念がある。
また、酸化度が0.20以上の湿潤ガス雰囲気下で焼鈍した場合は、鋼中炭素量は0.0030%以下となるが、良好な鉄損は得られていない。
実施例1の結果より、鉄系酸化物が形成しないような低酸化度雰囲気ガス中で焼鈍すると、一般に鋼板表面のシリカは稠密な膜状で生成し、脱炭を阻害するものと考えられる。
さらに、他の酸化物形成元素について検討を行い、Crを適量含有させることにより、鋼板表面にCr酸化物を形成させ、シリカ形成反応を抑制することによって脱炭反応を促進させることを検討した。その結果を実施例2として以下に説明する。
表2より、珪素鋼素材にCrを適量含有させることによって、酸化度が0.01~0.15の湿潤ガス(水蒸気-水素-窒素混合ガス)雰囲気中で焼鈍した場合は、良好な鉄損が得られると共に、鋼中炭素量が0.0030%(30ppm)以下となることが分かる。
実施例2において、含有させたCrは脱炭焼鈍の加熱過程で酸化物を形成して、脱炭反応を阻害するシリカ形成を抑制しているのではないかと推定された。そこで、加熱帯における雰囲気ガスの酸化度(P1=PH2O/PH2)とCr含有量との関係を検討した。
図2において、「×」のプロットは、炭素量が0.0030%超、あるいは鉄損(W17/50)が0.70(W/kg)超の実験例を示す。
0.18X-0.008≦P1≦0.25X+0.15≦0.20 (式1)
0.3X+0.025≦P1≦0.25X+0.15≦0.20 (式3)
さらに、冷間圧延工程の特性への影響について検討した。その結果を以下に説明する。
以上の工程により作製された試料につき、水洗、試料剪断の後、さらに歪取り焼鈍を行い、さらに、鋼板に張力を与える絶縁被膜を形成した(張力コーティングを施した)後、レーザー照射を行い、SST法にて磁気測定を行った。
脱炭焼鈍後の炭素量及び上記磁気測定によって得られた鉄損(W17/50)の値を表3に示す。
表3に示す通り、いずれの工程を経た場合でも、脱炭後の鋼中炭素量が0.0030%(30ppm)以下となるとともに、良好な鉄損が得られた。
さらに、珪素鋼スラブの成分の特性への影響について検討した。その結果を実施例5として以下に説明する。
以上の工程により作製された試料につき、水洗、試料剪断の後、さらに歪取り焼鈍を行い、さらに、鋼板に張力を与える絶縁被膜を形成した(張力コーティングを施した)後、レーザー照射を行い、SST法にて磁気測定を行った。
脱炭焼鈍後の炭素量及び上記磁気測定によって得られた鉄損(W17/50)の値を表4に示す。
Claims (6)
- 珪素鋼素材を製造する珪素鋼素材製造工程と、
前記珪素鋼素材を熱間圧延して熱延板を得る熱間圧延工程と、
前記熱延板に一回の冷間圧延もしくは中間焼鈍を挟む複数回の冷間圧延を施して最終板厚の鋼板を得る冷間圧延工程と、
前記鋼板に、加熱帯と均熱帯を備える脱炭焼鈍炉を用いて脱炭焼鈍を施す脱炭焼鈍工程と、
前記鋼板に、アルミナを主成分とする焼鈍分離剤を塗布し、仕上げ焼鈍を施す仕上げ焼鈍工程と、を含み、
前記珪素鋼素材が、質量%で、
Si:0.8~7.0%、
C:0.085%以下、
酸可溶性Al:0.010~0.065%、
N:0.004~0.012%、
Mn:1.00%以下、
S:0.050%以下、および
Cr:0.02~0.50%、
を含有し、残部がFe及び不純物からなり、
前記脱炭焼鈍工程では、
前記珪素鋼素材のCr含有量を質量%でXとしたとき、前記加熱帯の雰囲気ガスの酸化度P1が下記の式1を満足し、かつ前記均熱帯の雰囲気ガスの酸化度P2が下記の式2を満足する
ことを特徴とする方向性電磁鋼板の製造方法。
0.18X-0.008≦P1≦0.25X+0.15≦0.20 (式1)
0.01≦P2≦0.15 (式2) - 前記P1が下記の式3を満足す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。
0.3X+0.025≦P1≦0.25X+0.15≦0.20 (式3) - 前記P1、および前記P2が下記の式4を満足する
ことを特徴とする請求項1又は2に記載の方向性電磁鋼板の製造方法。
P1>P2 (式4) - 前記珪素鋼素材が、さらに、質量%で、
Cu:0%以上0.4%以下、
P:0%以上0.5%以下、
Ni:0%以上1.0%以下、
B:0%以上0.008%以下、
V:0%以上0.15%以下、
Nb:0%以上0.20%以下、
Mo:0%以上0.10%以下、
Ti:0%以上0.015%以下、及び
Bi:0%以上0.010%以下、
を含有する
ことを特徴とする請求項1から3のいずれか1項に記載の方向性電磁鋼板の製造方法。 - 前記脱炭焼鈍工程の前から前記仕上げ焼鈍工程での二次再結晶発現前までに、窒化処理工程をさらに含む
ことを特徴とする請求項1から4のいずれか1項に記載の方向性電磁鋼板の製造方法。 - 前記熱間圧延工程の後、かつ前記冷間圧延工程の前に、前記熱間圧延工程で得られた前記熱延板を焼鈍する熱延板焼鈍工程をさらに含む
ことを特徴とする請求項1から5のいずれか1項に記載の方向性電磁鋼板の製造方法。
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- 2020-01-16 KR KR1020217024425A patent/KR102576381B1/ko active IP Right Grant
- 2020-01-16 US US17/422,618 patent/US20210388459A1/en active Pending
- 2020-01-16 JP JP2020566440A patent/JP7188459B2/ja active Active
- 2020-01-16 CN CN202080009136.2A patent/CN113286909B/zh active Active
- 2020-01-16 BR BR112021013639-8A patent/BR112021013639A2/pt active Search and Examination
- 2020-01-16 EP EP20741980.5A patent/EP3913094A4/en active Pending
- 2020-01-16 WO PCT/JP2020/001139 patent/WO2020149320A1/ja unknown
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KR20210110366A (ko) | 2021-09-07 |
KR102576381B1 (ko) | 2023-09-11 |
CN113286909B (zh) | 2023-06-06 |
CN113286909A (zh) | 2021-08-20 |
US20210388459A1 (en) | 2021-12-16 |
BR112021013639A2 (pt) | 2021-09-14 |
JP7188459B2 (ja) | 2022-12-13 |
EP3913094A4 (en) | 2022-10-12 |
EP3913094A1 (en) | 2021-11-24 |
JPWO2020149320A1 (ja) | 2021-12-02 |
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