JPWO2016104813A1 - 方向性電磁鋼板およびその製造方法 - Google Patents
方向性電磁鋼板およびその製造方法 Download PDFInfo
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- JPWO2016104813A1 JPWO2016104813A1 JP2016566585A JP2016566585A JPWO2016104813A1 JP WO2016104813 A1 JPWO2016104813 A1 JP WO2016104813A1 JP 2016566585 A JP2016566585 A JP 2016566585A JP 2016566585 A JP2016566585 A JP 2016566585A JP WO2016104813 A1 JPWO2016104813 A1 JP WO2016104813A1
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- Prior art keywords
- annealing
- rolled
- hot
- recrystallization annealing
- primary recrystallization
- Prior art date
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- 238000004519 manufacturing process Methods 0.000 title claims description 27
- 229910000976 Electrical steel Inorganic materials 0.000 title claims description 4
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 76
- 239000010959 steel Substances 0.000 claims abstract description 76
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 45
- 229910001224 Grain-oriented electrical steel Inorganic materials 0.000 claims abstract description 34
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000000576 coating method Methods 0.000 claims abstract description 27
- 239000011248 coating agent Substances 0.000 claims abstract description 25
- 229910052742 iron Inorganic materials 0.000 claims abstract description 20
- 229910052839 forsterite Inorganic materials 0.000 claims abstract description 15
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000002233 thin-film X-ray diffraction Methods 0.000 claims abstract description 11
- 238000000137 annealing Methods 0.000 claims description 136
- 238000001953 recrystallisation Methods 0.000 claims description 95
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 58
- 238000005121 nitriding Methods 0.000 claims description 49
- 229910052757 nitrogen Inorganic materials 0.000 claims description 39
- 239000012298 atmosphere Substances 0.000 claims description 38
- 229910052718 tin Inorganic materials 0.000 claims description 33
- 229910004283 SiO 4 Inorganic materials 0.000 claims description 32
- 238000002791 soaking Methods 0.000 claims description 29
- 238000000034 method Methods 0.000 claims description 27
- 238000005097 cold rolling Methods 0.000 claims description 14
- 230000008569 process Effects 0.000 claims description 14
- 150000001875 compounds Chemical class 0.000 claims description 13
- 229910052717 sulfur Inorganic materials 0.000 claims description 13
- 229910052711 selenium Inorganic materials 0.000 claims description 11
- 239000012535 impurity Substances 0.000 claims description 10
- 229910052748 manganese Inorganic materials 0.000 claims description 10
- 230000001590 oxidative effect Effects 0.000 claims description 10
- 238000004458 analytical method Methods 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 229910021332 silicide Inorganic materials 0.000 claims description 6
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 claims description 6
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052797 bismuth Inorganic materials 0.000 claims description 4
- 229910052906 cristobalite Inorganic materials 0.000 claims description 4
- 239000010408 film Substances 0.000 abstract description 42
- 239000007789 gas Substances 0.000 description 24
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 19
- 230000000694 effects Effects 0.000 description 15
- 239000003112 inhibitor Substances 0.000 description 13
- 238000012360 testing method Methods 0.000 description 12
- 238000002474 experimental method Methods 0.000 description 11
- 239000001257 hydrogen Substances 0.000 description 10
- 229910052739 hydrogen Inorganic materials 0.000 description 10
- 239000013078 crystal Substances 0.000 description 9
- 238000005261 decarburization Methods 0.000 description 9
- 230000006866 deterioration Effects 0.000 description 9
- 239000000395 magnesium oxide Substances 0.000 description 9
- 238000007254 oxidation reaction Methods 0.000 description 9
- 238000012795 verification Methods 0.000 description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 230000003647 oxidation Effects 0.000 description 7
- 238000005096 rolling process Methods 0.000 description 7
- 229910052782 aluminium Inorganic materials 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 238000005755 formation reaction Methods 0.000 description 5
- 238000005098 hot rolling Methods 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 230000001603 reducing effect Effects 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 229910010413 TiO 2 Inorganic materials 0.000 description 4
- 229910001860 alkaline earth metal hydroxide Inorganic materials 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 4
- 230000002401 inhibitory effect Effects 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 229910052758 niobium Inorganic materials 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 238000003303 reheating Methods 0.000 description 3
- 230000000087 stabilizing effect Effects 0.000 description 3
- 239000002344 surface layer Substances 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 229910052787 antimony Inorganic materials 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000011162 core material Substances 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- HSRJKNPTNIJEKV-UHFFFAOYSA-N Guaifenesin Chemical compound COC1=CC=CC=C1OCC(O)CO HSRJKNPTNIJEKV-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 206010039509 Scab Diseases 0.000 description 1
- 229910008484 TiSi Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- -1 alkaline earth metal sulfate Chemical class 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000008119 colloidal silica Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- XLJMAIOERFSOGZ-UHFFFAOYSA-M cyanate Chemical compound [O-]C#N XLJMAIOERFSOGZ-UHFFFAOYSA-M 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000002075 main ingredient Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000009628 steelmaking Methods 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000012418 validation experiment Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
- C21D8/1277—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties involving a particular surface treatment
- C21D8/1288—Application of a tension-inducing coating
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
- C21D8/1244—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
- C21D8/1244—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest
- C21D8/1261—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest following hot rolling
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
- C21D8/1244—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest
- C21D8/1272—Final recrystallisation annealing
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
- C21D8/1277—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties involving a particular surface treatment
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
- C21D8/1277—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties involving a particular surface treatment
- C21D8/1283—Application of a separating or insulating coating
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- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/46—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for sheet metals
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
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- C22C38/001—Ferrous alloys, e.g. steel alloys containing N
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- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
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- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/004—Very low carbon steels, i.e. having a carbon content of less than 0,01%
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- C22C—ALLOYS
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- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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- C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/08—Ferrous alloys, e.g. steel alloys containing nickel
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
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- C—CHEMISTRY; METALLURGY
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- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
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- C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
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- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
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- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/60—Ferrous alloys, e.g. steel alloys containing lead, selenium, tellurium, or antimony, or more than 0.04% by weight of sulfur
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/02—Pretreatment of the material to be coated
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
- C23C8/24—Nitriding
- C23C8/26—Nitriding of ferrous surfaces
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/40—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using liquids, e.g. salt baths, liquid suspensions
- C23C8/42—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using liquids, e.g. salt baths, liquid suspensions only one element being applied
- C23C8/48—Nitriding
- C23C8/50—Nitriding of ferrous surfaces
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- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/80—After-treatment
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
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Abstract
Description
C:0.04質量%、Si:3.0質量%、Mn:0.05質量%、S:0.005質量%、Sb:0.01質量%、Al:60質量ppm、N:30質量ppmを含有し、残部がFe及び不可避的不純物からなる成分組成の鋼スラブを、1230℃で加熱し、熱間圧延して2.0mm厚の熱延コイルとした。これに1030℃の熱延板焼鈍を行ない、圧延時に200℃、1分以上となる時効時間を満たす冷間圧延によって0.30mm厚の冷延板とし、この冷延板に800℃の水素・窒素混合の湿潤雰囲気下で脱炭焼鈍を兼ねる一次再結晶焼鈍を行なった。
1.薄膜X線回折を用いた分析で、42°<2θ<43°の範囲に認められるTiN(Osbornite)のピーク値PTiNと、23°<2θ<25°に認められるSiO2(Cristobalite)のピークの値PSiO2とが、ともに0超えであり、かつ、PTiN≧PSiO2の関係を満足する下地被膜を有し、鉄損W17/50が1.0W/kg以下であることを特徴とする方向性電磁鋼板。
質量%で、C:0.001〜0.10%、Si:1.0〜5.0%、Mn:0.01〜0.5%、S及びSeのうちから選んだ1種又は2種を合計で0.002〜0.040%、sol.Al:0.001〜0.050%、およびN:0.0010〜0.020%を含有し、残部がFeおよび不可避的不純物からなる成分組成の鋼スラブを、熱間圧延して熱延板を得る工程と、
必要に応じて前記熱延板に熱延板焼鈍を施す工程と、
その後、前記熱延板に1回もしくは中間焼鈍を挟む2回以上の冷間圧延を施して最終板厚を有する冷延板を得る工程と、
その後、前記冷延板に一次再結晶焼鈍を施して一次再結晶焼鈍板を得る工程と、
前記一次再結晶焼鈍中に前記冷延板に、または、前記一次再結晶焼鈍後に前記一次再結晶焼鈍板に、窒化処理を施す工程と、
その後、前記一次再結晶焼鈍板に焼鈍分離剤を塗布し、二次再結晶焼鈍を実施する工程と、を有し、
前記窒化処理後の鋼中窒素量を150質量ppm以上1000質量ppm以下とし、
前記焼鈍分離剤に、Ti化合物をTi質量換算で0.10g/m2以上1.5g/m2以下含有させ、
前記二次再結晶焼鈍において、800〜950℃の所定温度でPH2O/PH2:0.05以上の酸化性雰囲気下で20時間以上の均熱焼鈍を行い、その後、1000℃以上の温度範囲においてH2を含有する雰囲気で5時間以上焼鈍することを特徴とする方向性電磁鋼板の製造方法。
質量%で、C:0.001〜0.10%、Si:1.0〜5.0%、Mn:0.01〜0.5%、S及びSeのうちから選んだ1種又は2種を合計で0.002〜0.040%、sol.Al:0.001〜0.050%、N:0.0010〜0.020%を含有し、残部がFeおよび不可避的不純物からなる成分組成の鋼スラブを、熱間圧延して熱延板を得る工程と、
必要に応じて前記熱延板に熱延板焼鈍を施す工程と、
その後、前記熱延板に1回もしくは中間焼鈍を挟む2回以上の冷間圧延を施して最終板厚を有する冷延板を得る工程と、
その後、前記冷延板に一次再結晶焼鈍を施して一次再結晶焼鈍板を得る工程と、
前記一次再結晶焼鈍中に前記冷延板に、または、前記一次再結晶焼鈍後に前記一次再結晶焼鈍板に、窒化処理を施す工程と、
その後、前記一次再結晶焼鈍板に焼鈍分離剤を塗布し、二次再結晶焼鈍を実施する工程と、を有し、
前記窒化処理後の鋼中窒素量を150質量ppm以上1000質量ppm以下とし、
前記焼鈍分離剤に、主剤としてMgOを含有し、Ti酸化物またはTi珪化物をTi質量換算で0.10g/m2以上1.5g/m2以下の範囲で含有させ、
前記二次再結晶焼鈍において、800〜950℃の所定温度でPH2O/PH2:0.05以上の酸化性雰囲気下で20時間以上の均熱焼鈍を行い、その後、1000℃以上の温度範囲においてH2を含有する雰囲気で5時間以上焼鈍することを特徴とする方向性電磁鋼板の製造方法。
Ni:0.005〜1.50%、
Sn:0.01〜0.50%、
Sb:0.005〜0.50%、
Cu:0.01〜0.50%、
Cr:0.01〜1.50%、
P:0.0050〜0.50%、
Mo:0.01〜0.50%、
Nb:0.0005〜0.0100%、
Ti:0.0005〜0.0100%、
B:0.0001〜0.0100%および
Bi:0.0005〜0.0100%
のうちから選んだ1種または2種以上を含有する前記3または4に記載の方向性電磁鋼板の製造方法。
Cは、一次再結晶集合組織を改善する上で有用な元素であるが、C含有量が0.10%を超えるとかえって一次再結晶集合組織の劣化を招くので、C含有量は0.10%以下が好ましい。また、最終製品でCが残留すると磁気時効と呼ばれる磁性劣化が生じるので、高いC量は脱炭焼鈍の負荷も高めることにつながる。そのためC含有量は0.08%以下とすることがより望ましい。一方、集合組織改善の観点から望ましいC含有量は、0.01%以上であるが、要求される磁気特性のレベルがさほど高くない場合には、一次再結晶焼鈍における脱炭過程を省略あるいは簡略化するために、C含有量の下限を0.001%に低減してもよい。
Siは、電気抵抗を高めることによって鉄損を改善する有用元素であるため1.0%以上含有させることが望ましい。しかしながら、Si含有量が5.0%を超えると冷間圧延性が著しく劣化するので、Si含有量は5.0%以下が好ましい。また、鉄損と製造性の観点からより望ましいSi含有量は、1.5〜4.5%の範囲である。
Mnは、SやSeと結合してMnSeやMnSを形成しインヒビター作用を発揮する成分である。また、製造時における熱間加工性を向上させる効果も有している。しかしながら、0.01%以下のMn含有量ではこうした効果を得ることができない。一方、Mn含有量が0.5%を超えた場合には、一次再結晶集合組織が悪化して磁気特性の劣化を招くので、上限は0.5%が好ましい。
Alは、鋼中でAlNを形成して分散第二相としてインヒビターの作用をする有用成分であるが、Al含有量が0.01%に満たないと十分に析出量が確保できない。一方、0.050%を超えて添加すると窒化後に析出するAlN量が過剰となるため、粒成長の抑制力が高くなりすぎ、高温まで焼鈍しても二次再結晶しない。但し、Alを0.01%未満とした場合であっても、窒素量との兼ね合いにより、Alを含有しないSi3N4が析出する場合もある。Si3N4をインヒビターとして機能させる場合は、必ずしもAlは多量に含まれていなくても良いが、Al自身は酸素親和力が高いため、製鋼段階において微量添加することにより鋼中の溶存酸素量を低減し、鋼中酸化物・介在物を低減することを介して特性劣化抑制の効果を有する。このため、本発明では、酸可溶性Alとして0.001%以上の範囲で添加することにより磁性劣化を抑制できる。
NもAlと同様に、AlNを形成するために必要な成分である。二次再結晶時にインヒビターとして必要な窒素は後工程にて窒化により供給することができるが、N含有量が0.0010%を下回ると、窒化工程までの間の焼鈍工程で結晶粒成長が過剰となり、冷間圧延工程での粒界割れなどの原因となる場合がある。また0.020%を超えて添加するとスラブ加熱時にふくれ等を生じる。このため、N含有量は0.0010〜0.020%の範囲が好ましい。
S及びSeは、MnやCuと結合してMnSe、MnS、Cu2−xSe、Cu2−xSを形成し、鋼中の分散第二相としてインヒビターの作用を発揮する有用成分である。これらS、Seの合計含有量が0.002%に満たないとその添加効果に乏しい一方で、0.040%を超えると、スラブ加熱時の固溶が不完全となるだけでなく、製品表面の欠陥の原因ともなる。このため、単独添加又は複合添加いずれの場合も合計含有量は0.002〜0.040%の範囲が好ましい。
Niは、熱延板組織の均一性を高めることにより、磁気特性を改善する働きがあり、そのためには0.005%以上含有させることが好ましいが、Ni含有量が1.50%を超えると二次再結晶が困難となり、磁気特性が劣化するので、Ni含有量は0.005〜1.50%とすることが望ましい。
Snは、二次再結晶焼鈍中の鋼板の窒化や酸化を抑制し、良好な結晶方位を有する結晶粒の二次再結晶を促進して磁気特性を向上させる有用元素であり、そのためには0.01%以上含有させることが好ましいが、0.50%を超えて含有されると冷間圧延性が劣化するので、Sn含有量は0.01〜0.50%とすることが望ましい。
Sbは、二次再結晶焼鈍中の鋼板の窒化や酸化を抑制し、良好な結晶方位を有する結晶粒の二次再結晶を促進して磁気特性を効果的に向上させる有用元素であり、その目的のためには0.005%以上含有させることが好ましいが、0.50%を超えて含有されると冷間圧延性が劣化するので、Sb含有量は0.005〜0.50%とすることが望ましい。
Cuは、二次再結晶焼鈍中の鋼板の酸化を抑制し、良好な結晶方位を有する結晶粒の二次再結晶を促進して磁気特性を効果的に向上させる働きがあり、そのためには0.01%以上含有させることが好ましいが、0.50%を超えて含有されると熱間圧延性の劣化を招くので、Cu含有量は0.01〜0.50%とすることが望ましい。
Crは、フォルステライト被膜の形成を安定化させる働きがあり、そのためには0.01%以上含有させることが好ましいが、一方でCr含有量が1.50%を超えると二次再結晶が困難となり、磁気特性が劣化するので、Cr含有量は0.01〜1.50%とすることが望ましい。
Pは、フォルステライト被膜の形成を安定化させる働きがあり、そのためには0.0050%以上含有させることが好ましいが、P含有量が0.50%を超えると冷間圧延性が劣化するので、P含有量は0.0050〜0.50%とすることが望ましい。
Mo、Nbは、スラブ加熱時の温度変化による割れの抑制等を介して、熱延後のヘゲを抑制する効果を有している。これらは上記下限以上含有させなければヘゲ抑制の効果は小さく、上記上限超では炭化物、窒化物を形成するなどして最終製品まで残留した際、鉄損劣化を引き起こす。このため、上述の範囲とすることが望ましい。
これらの成分は、窒化した際に析出物を形成したり、自身が偏析するなどしたりして、補助的なインヒビターとして機能し、二次再結晶を安定化させる効果を有する場合がある。これらは上記下限未満では補助インヒビターとしての効果を得るに乏しく、上記上限超では形成した析出物が純化後にも残留して磁気特性劣化の原因となったり、粒界を脆化させてベンド特性を劣化させたりする場合がある。
Si:3.13%、C:0.05%、Mn:0.06%、S:0.003%を含有しAlとNを表1に示す比率で含有し、その他成分として、Ni、Sn、Sb、Cu、Cr、P、Mo、Nb、Tiを表1に示す比率で含有し、残部がFeおよび不可避的不純物からなる成分組成の鋼スラブを、1200℃、40分加熱後、熱間圧延して2.4mmの板厚の熱延板とした。この熱延板に、1000℃×1分間の焼鈍を施した後、冷間圧延により0.27mmの最終板厚とし、得られた冷間圧延コイルの中央部から、100mm×400mmサイズの試料を採取し、ラボにて一次再結晶と脱炭を兼ねた焼鈍を行ない、一次再結晶焼鈍板を得た。
Si:3.2%、C:0.03%、Mn:0.08%、S:0.001%、Se:0.003%、Al:0.016%、N:0.004%、Bi:0.001%を含有し、残部がFeおよび不可避的不純物からなる成分組成の鋼スラブを、1180℃、50分加熱後、熱間圧延して2.0mmの板厚の熱延板とした。この熱延板に、1050℃×1分間の焼鈍を施した後、1080℃の中間焼鈍を挟み冷間圧延により0.23mmの最終板厚とし、得られた冷間圧延コイルの中央部から、100mm×400mmサイズの試料を採取し、ラボにて一次再結晶と脱炭を兼ねた焼鈍を行ない、一次再結晶焼鈍板を得た。
Si:3.4%、C:0.04%、Mn:0.03%、S:0.01%、Al:0.006%、N:0.004%を含有し、残部がFeおよび不可避的不純物からなる成分組成の鋼スラブを、を1200℃、60分加熱後、熱間圧延して2.0mmの板厚の熱延板とした。この熱延板に、1050℃×2分間の焼鈍を施した後、冷間圧延により0.23mmの最終板厚を有する冷延板とした。この冷延板に一次再結晶と脱炭を兼ねた焼鈍を行い、得られたコイルの中央部から、100mm×400mmサイズの試料(一次再結晶焼鈍板)を採取した。その後、一次再結晶焼鈍板にNH3ガス雰囲気中で鋼中窒素量を300質量ppmとなるまで窒化処理を行った。
Claims (5)
- 薄膜X線回折を用いた分析で、42°<2θ<43°の範囲に認められるTiN(Osbornite)のピーク値PTiNと、23°<2θ<25°に認められるSiO2(Cristobalite)のピークの値PSiO2とが、ともに0超えであり、かつ、PTiN≧PSiO2の関係を満足する下地被膜を有し、鉄損W17/50が1.0W/kg以下であることを特徴とする方向性電磁鋼板。
- 薄膜X線回折を用いた分析で、42°<2θ<43°の範囲に認められるTiN(Osbornite)のピーク値PTiNと、35°<2θ<36°に認められるMg2SiO4(Forsterite)のピークの値PMg2SiO4とが、ともに0超えであり、かつ、PTiN≧PMg2SiO4の関係を満足する下地被膜を有し、鉄損W17/50が1.0W/kg以下であることを特徴とする方向性電磁鋼板。
- 請求項1または2に記載の方向性電磁鋼板を製造する方法であって、
質量%で、C:0.001〜0.10%、Si:1.0〜5.0%、Mn:0.01〜0.5%、S及びSeのうちから選んだ1種又は2種を合計で0.002〜0.040%、sol.Al:0.001〜0.050%、およびN:0.0010〜0.020%を含有し、残部がFeおよび不可避的不純物からなる成分組成の鋼スラブを、熱間圧延して熱延板を得る工程と、
必要に応じて前記熱延板に熱延板焼鈍を施す工程と、
その後、前記熱延板に1回もしくは中間焼鈍を挟む2回以上の冷間圧延を施して最終板厚を有する冷延板を得る工程と、
その後、前記冷延板に一次再結晶焼鈍を施して一次再結晶焼鈍板を得る工程と、
前記一次再結晶焼鈍中に前記冷延板に、または、前記一次再結晶焼鈍後に前記一次再結晶焼鈍板に、窒化処理を施す工程と、
その後、前記一次再結晶焼鈍板に焼鈍分離剤を塗布し、二次再結晶焼鈍を実施する工程と、を有し、
前記窒化処理後の鋼中窒素量を150質量ppm以上1000質量ppm以下とし、
前記焼鈍分離剤に、Ti化合物をTi質量換算で0.10g/m2以上1.5g/m2以下含有させ、
前記二次再結晶焼鈍において、800〜950℃の所定温度でPH2O/PH2:0.05以上の酸化性雰囲気下で20時間以上の均熱焼鈍を行い、その後、1000℃以上の温度範囲においてH2を含有する雰囲気で5時間以上焼鈍することを特徴とする方向性電磁鋼板の製造方法。 - 請求項2に記載の方向性電磁鋼板を製造する方法であって、
質量%で、C:0.001〜0.10%、Si:1.0〜5.0%、Mn:0.01〜0.5%、S及びSeのうちから選んだ1種又は2種を合計で0.002〜0.040%、sol.Al:0.001〜0.050%、およびN:0.0010〜0.020%を含有し、残部がFeおよび不可避的不純物からなる成分組成の鋼スラブを、熱間圧延して熱延板を得る工程と、
必要に応じて前記熱延板に熱延板焼鈍を施す工程と、
その後、前記熱延板に1回もしくは中間焼鈍を挟む2回以上の冷間圧延を施して最終板厚を有する冷延板を得る工程と、
その後、前記冷延板に一次再結晶焼鈍を施して一次再結晶焼鈍板を得る工程と、
前記一次再結晶焼鈍中に前記冷延板に、または、前記一次再結晶焼鈍後に前記一次再結晶焼鈍板に、窒化処理を施す工程と、
その後、前記一次再結晶焼鈍板に焼鈍分離剤を塗布し、二次再結晶焼鈍を実施する工程と、を有し、
前記窒化処理後の鋼中窒素量を150質量ppm以上1000質量ppm以下とし、
前記焼鈍分離剤に、主剤としてMgOを含有し、Ti酸化物またはTi珪化物をTi質量換算で0.10g/m2以上1.5g/m2以下の範囲で含有させ、
前記二次再結晶焼鈍において、800〜950℃の所定温度でPH2O/PH2:0.05以上の酸化性雰囲気下で20時間以上の均熱焼鈍を行い、その後、1000℃以上の温度範囲においてH2を含有する雰囲気で5時間以上焼鈍することを特徴とする方向性電磁鋼板の製造方法。 - 前記鋼スラブに、さらに質量%で、
Ni:0.005〜1.50%、
Sn:0.01〜0.50%、
Sb:0.005〜0.50%、
Cu:0.01〜0.50%、
Cr:0.01〜1.50%、
P:0.0050〜0.50%、
Mo:0.01〜0.50%、
Nb:0.0005〜0.0100%、
Ti:0.0005〜0.0100%、
B:0.0001〜0.0100%および
Bi:0.0005〜0.0100%
のうちから選んだ1種または2種以上を含有する請求項3または4に記載の方向性電磁鋼板の製造方法。
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