JP6547835B2 - 方向性電磁鋼板、及び方向性電磁鋼板の製造方法 - Google Patents
方向性電磁鋼板、及び方向性電磁鋼板の製造方法 Download PDFInfo
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- JP6547835B2 JP6547835B2 JP2017543521A JP2017543521A JP6547835B2 JP 6547835 B2 JP6547835 B2 JP 6547835B2 JP 2017543521 A JP2017543521 A JP 2017543521A JP 2017543521 A JP2017543521 A JP 2017543521A JP 6547835 B2 JP6547835 B2 JP 6547835B2
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- steel sheet
- metal
- insulating film
- phosphate
- mass
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- 229910000831 Steel Inorganic materials 0.000 title claims description 98
- 239000010959 steel Substances 0.000 title claims description 98
- 238000004519 manufacturing process Methods 0.000 title claims description 27
- 238000000576 coating method Methods 0.000 claims description 150
- 239000011248 coating agent Substances 0.000 claims description 149
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 130
- 229910001463 metal phosphate Inorganic materials 0.000 claims description 110
- 229910052751 metal Inorganic materials 0.000 claims description 105
- 229910001224 Grain-oriented electrical steel Inorganic materials 0.000 claims description 102
- 239000002184 metal Substances 0.000 claims description 102
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 79
- 239000008119 colloidal silica Substances 0.000 claims description 70
- 229910019142 PO4 Inorganic materials 0.000 claims description 68
- 239000010452 phosphate Substances 0.000 claims description 67
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 65
- 150000003839 salts Chemical class 0.000 claims description 65
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 63
- 239000007787 solid Substances 0.000 claims description 43
- 238000010828 elution Methods 0.000 claims description 38
- 238000006116 polymerization reaction Methods 0.000 claims description 38
- 238000009413 insulation Methods 0.000 claims description 33
- 238000002791 soaking Methods 0.000 claims description 26
- 239000007788 liquid Substances 0.000 claims description 25
- 229910052782 aluminium Inorganic materials 0.000 claims description 21
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 claims description 20
- 150000002739 metals Chemical class 0.000 claims description 20
- 150000003013 phosphoric acid derivatives Chemical class 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 229910052725 zinc Inorganic materials 0.000 claims description 19
- 229910052759 nickel Inorganic materials 0.000 claims description 17
- 229910052742 iron Inorganic materials 0.000 claims description 16
- 229910052749 magnesium Inorganic materials 0.000 claims description 16
- 239000002671 adjuvant Substances 0.000 claims description 15
- 229910052721 tungsten Inorganic materials 0.000 claims description 15
- 229910052720 vanadium Inorganic materials 0.000 claims description 15
- 229910052726 zirconium Inorganic materials 0.000 claims description 15
- 229910052748 manganese Inorganic materials 0.000 claims description 12
- 230000000630 rising effect Effects 0.000 claims description 12
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 9
- 239000004327 boric acid Substances 0.000 claims description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 8
- 229910021538 borax Inorganic materials 0.000 claims description 8
- 229910052750 molybdenum Inorganic materials 0.000 claims description 8
- 239000000049 pigment Substances 0.000 claims description 8
- 239000011164 primary particle Substances 0.000 claims description 8
- 238000005096 rolling process Methods 0.000 claims description 8
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims description 8
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 8
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 8
- BSVBQGMMJUBVOD-UHFFFAOYSA-N trisodium borate Chemical compound [Na+].[Na+].[Na+].[O-]B([O-])[O-] BSVBQGMMJUBVOD-UHFFFAOYSA-N 0.000 claims description 8
- 229910000976 Electrical steel Inorganic materials 0.000 claims description 7
- IOVCWXUNBOPUCH-UHFFFAOYSA-N Nitrous acid Chemical group ON=O IOVCWXUNBOPUCH-UHFFFAOYSA-N 0.000 claims description 6
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims description 6
- 229910002113 barium titanate Inorganic materials 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 229910000476 molybdenum oxide Inorganic materials 0.000 claims description 6
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 claims description 6
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 6
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 6
- ABLZXFCXXLZCGV-UHFFFAOYSA-N Phosphorous acid Chemical compound OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 235000010288 sodium nitrite Nutrition 0.000 claims description 4
- 235000019830 sodium polyphosphate Nutrition 0.000 claims description 4
- UNXRWKVEANCORM-UHFFFAOYSA-N triphosphoric acid Chemical compound OP(O)(=O)OP(O)(=O)OP(O)(O)=O UNXRWKVEANCORM-UHFFFAOYSA-N 0.000 claims description 4
- AZFNGPAYDKGCRB-XCPIVNJJSA-M [(1s,2s)-2-amino-1,2-diphenylethyl]-(4-methylphenyl)sulfonylazanide;chlororuthenium(1+);1-methyl-4-propan-2-ylbenzene Chemical compound [Ru+]Cl.CC(C)C1=CC=C(C)C=C1.C1=CC(C)=CC=C1S(=O)(=O)[N-][C@@H](C=1C=CC=CC=1)[C@@H](N)C1=CC=CC=C1 AZFNGPAYDKGCRB-XCPIVNJJSA-M 0.000 claims description 3
- QBWCMBCROVPCKQ-UHFFFAOYSA-N chlorous acid Chemical compound OCl=O QBWCMBCROVPCKQ-UHFFFAOYSA-N 0.000 claims description 3
- HWGNBUXHKFFFIH-UHFFFAOYSA-I pentasodium;[oxido(phosphonatooxy)phosphoryl] phosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O HWGNBUXHKFFFIH-UHFFFAOYSA-I 0.000 claims description 3
- 235000010333 potassium nitrate Nutrition 0.000 claims description 3
- 239000004323 potassium nitrate Substances 0.000 claims description 3
- 235000010289 potassium nitrite Nutrition 0.000 claims description 3
- 239000004304 potassium nitrite Substances 0.000 claims description 3
- UKLNMMHNWFDKNT-UHFFFAOYSA-M sodium chlorite Chemical compound [Na+].[O-]Cl=O UKLNMMHNWFDKNT-UHFFFAOYSA-M 0.000 claims description 3
- 229960002218 sodium chlorite Drugs 0.000 claims description 3
- 235000010344 sodium nitrate Nutrition 0.000 claims description 3
- 239000004317 sodium nitrate Substances 0.000 claims description 3
- YPPQYORGOMWNMX-UHFFFAOYSA-L sodium phosphonate pentahydrate Chemical compound [Na+].[Na+].[O-]P([O-])=O YPPQYORGOMWNMX-UHFFFAOYSA-L 0.000 claims description 3
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 3
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 claims description 2
- 229910001919 chlorite Inorganic materials 0.000 claims description 2
- 229910052619 chlorite group Inorganic materials 0.000 claims description 2
- 229920000137 polyphosphoric acid Polymers 0.000 claims description 2
- 229940048102 triphosphoric acid Drugs 0.000 claims description 2
- 235000021317 phosphate Nutrition 0.000 description 66
- 238000000034 method Methods 0.000 description 37
- 238000012545 processing Methods 0.000 description 36
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 29
- 238000005260 corrosion Methods 0.000 description 19
- 230000007797 corrosion Effects 0.000 description 19
- 239000000126 substance Substances 0.000 description 16
- 238000006243 chemical reaction Methods 0.000 description 15
- 238000013329 compounding Methods 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 14
- 239000002245 particle Substances 0.000 description 14
- 238000000137 annealing Methods 0.000 description 13
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 10
- 239000000463 material Substances 0.000 description 10
- 230000000694 effects Effects 0.000 description 8
- -1 organic acid salt Chemical class 0.000 description 7
- 238000002156 mixing Methods 0.000 description 6
- 229910052698 phosphorus Inorganic materials 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 238000009835 boiling Methods 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
- 230000007423 decrease Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 150000001845 chromium compounds Chemical class 0.000 description 4
- 229910052839 forsterite Inorganic materials 0.000 description 4
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 3
- 239000012752 auxiliary agent Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000011162 core material Substances 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 229910052788 barium Inorganic materials 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 238000000921 elemental analysis Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 150000002484 inorganic compounds Chemical class 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 238000005554 pickling Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000012756 surface treatment agent Substances 0.000 description 2
- 235000011178 triphosphate Nutrition 0.000 description 2
- 239000001226 triphosphate Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- FUSNOPLQVRUIIM-UHFFFAOYSA-N 4-amino-2-(4,4-dimethyl-2-oxoimidazolidin-1-yl)-n-[3-(trifluoromethyl)phenyl]pyrimidine-5-carboxamide Chemical compound O=C1NC(C)(C)CN1C(N=C1N)=NC=C1C(=O)NC1=CC=CC(C(F)(F)F)=C1 FUSNOPLQVRUIIM-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 229920000298 Cellophane Polymers 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 description 1
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- BDAGIHXWWSANSR-UHFFFAOYSA-M Formate Chemical compound [O-]C=O BDAGIHXWWSANSR-UHFFFAOYSA-M 0.000 description 1
- JVTAAEKCZFNVCJ-UHFFFAOYSA-M Lactate Chemical compound CC(O)C([O-])=O JVTAAEKCZFNVCJ-UHFFFAOYSA-M 0.000 description 1
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 1
- 229920000388 Polyphosphate Polymers 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 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
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 description 1
- 229910052586 apatite Inorganic materials 0.000 description 1
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- XTEGARKTQYYJKE-UHFFFAOYSA-N chloric acid Chemical compound OCl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-N 0.000 description 1
- 229940005991 chloric acid Drugs 0.000 description 1
- 229940077239 chlorous acid Drugs 0.000 description 1
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Chemical class O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000005097 cold rolling Methods 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000005261 decarburization Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000012024 dehydrating agents Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 238000004993 emission spectroscopy Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012493 hydrazine sulfate Substances 0.000 description 1
- 229910000377 hydrazine sulfate Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000011835 investigation 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
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- VSIIXMUUUJUKCM-UHFFFAOYSA-D pentacalcium;fluoride;triphosphate Chemical compound [F-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O VSIIXMUUUJUKCM-UHFFFAOYSA-D 0.000 description 1
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 1
- 229940116254 phosphonic acid Drugs 0.000 description 1
- 239000001205 polyphosphate Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- YGSDEFSMJLZEOE-UHFFFAOYSA-M salicylate Chemical compound OC1=CC=CC=C1C([O-])=O YGSDEFSMJLZEOE-UHFFFAOYSA-M 0.000 description 1
- 229960001860 salicylate Drugs 0.000 description 1
- 230000009291 secondary effect Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- RPACBEVZENYWOL-XFULWGLBSA-M sodium;(2r)-2-[6-(4-chlorophenoxy)hexyl]oxirane-2-carboxylate Chemical compound [Na+].C=1C=C(Cl)C=CC=1OCCCCCC[C@]1(C(=O)[O-])CO1 RPACBEVZENYWOL-XFULWGLBSA-M 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- KDYFGRWQOYBRFD-UHFFFAOYSA-L succinate(2-) Chemical compound [O-]C(=O)CCC([O-])=O KDYFGRWQOYBRFD-UHFFFAOYSA-L 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 229940095064 tartrate Drugs 0.000 description 1
- 239000011882 ultra-fine particle Substances 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
Images
Classifications
-
- 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
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/07—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing phosphates
-
- 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
- C21D8/1288—Application of a tension-inducing coating
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/34—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing cold phosphate binders
- C04B28/344—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing cold phosphate binders the phosphate binder being present in the starting composition solely as one or more phosphates
-
- 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
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/26—Methods of annealing
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
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Description
本願は、2015年9月29日に、日本に出願された特願2015−191155号に基づき優先権を主張し、その内容をここに援用する。
しかしながら、方向性電磁鋼板の絶縁被膜の緻密さと、絶縁被膜が方向性電磁鋼板に付与し得る張力との関係、及び方向性電磁鋼板のクロム酸塩を含まない絶縁被膜の緻密化の方法について従来技術では十分には検討されていなかった。
(1)本発明の一態様に係る方向性電磁鋼板は、鋼板と絶縁被膜とを備える方向性電磁鋼板であって、前記絶縁被膜が、Al、Fe、Mg、Mn、Ni、およびZnの中から選ばれる1種または2種以上の金属のリン酸金属塩である第一のリン酸金属塩と;Co、Mo、V、W、およびZrの中から選ばれる1種または2種以上の金属のリン酸金属塩である第二のリン酸金属塩と;シリカと;を含有し、前記絶縁被膜がクロム酸塩を含有せず、前記方向性電磁鋼板を沸騰させた純水中で10分間煮沸し、前記純水中に溶出したリン酸の量を測定し、前記リン酸の量を煮沸された前記方向性電磁鋼板の前記絶縁被膜の面積で割ることで測定される、前記絶縁被膜のリン酸溶出量が30mg/m2以下である(ただし、前記絶縁被膜中に塩化物または塩化物イオンを含有するものを除く)。
(2)上記(1)に記載の方向性電磁鋼板は、前記第一のリン酸金属塩が、Al、Mg、Ni、およびZnの中から選ばれる1種または2種以上の前記金属の前記リン酸金属塩であってもよい。
(3)上記(1)または(2)に記載の方向性電磁鋼板は、前記第二のリン酸金属塩が、V、W、およびZrの中から選ばれる1種または2種以上の前記金属の前記リン酸金属塩であってもよい。
(4)上記(1)〜(3)のいずれか一項に記載の方向性電磁鋼板は、前記第二のリン酸金属塩の含有率は、前記絶縁被膜の総質量に対して0.5〜10.0質量%であってもよい。
(5)上記(1)〜(4)のいずれか一項に記載の方向性電磁鋼板は、前記シリカの含有率は、前記絶縁被膜の総質量に対して、25〜55質量%であってもよい。
(6)上記(1)〜(5)のいずれか一項に記載の方向性電磁鋼板は、前記絶縁被膜の被膜量が2.0〜7.0g/m2であってもよい。
(7)上記(1)〜(6)のいずれか一項に記載の方向性電磁鋼板は、前記絶縁被膜が、さらに、ホウ酸、ホウ酸ナトリウム、酸化チタン、酸化モリブテン、顔料、およびチタン酸バリウムからなる群から選択される一種以上を含んでもよい。
(8)上記(1)〜(7)のいずれか一項に記載の方向性電磁鋼板は、前記鋼板が、単位質量%で、C:0.005%以下、Si:2.5〜7.0%、Mn:0〜1.0%、Al:0〜0.03%、N:0.01%以下、P:0.01%以下、及びS:0.01%以下を含有し、残部がFeおよび不純物からなり、前記鋼板の平均結晶粒径は、1〜10mmであり、前記鋼板の(110)[001]の結晶方位と圧延方向とのなす角は、平均で8°以下であってもよい。
(9)本発明の別の態様による方向性電磁鋼板の製造方法は、絶縁被膜処理液を鋼板の表面に塗布する工程と;前記絶縁被膜処理液を焼き付けて絶縁被膜を成膜する工程と;を備え、前記絶縁被膜処理液は、固形分換算で100質量部の、Al、Fe、Mg、Mn、Ni、およびZnの中から選ばれる1種または2種以上の金属のリン酸金属塩である第一のリン酸金属塩と;固形分換算で3〜20質量部の、Co、Mo、V、W、およびZrの中から選ばれる1種または2種以上の金属のリン酸金属塩である第二のリン酸金属塩と;固形分換算で35〜125質量部のコロイド状シリカと;0.3〜6.0質量部の重合補助剤と;を含有し、前記焼き付けでは、100〜800℃の温度範囲での昇温速度30℃/秒以上、焼付均熱温度800〜1000℃、及び均熱保持時間10〜60秒とされ、前記コロイド状シリカの平均一次粒径が7〜30nmである。
(10)上記(9)に記載の方向性電磁鋼板の製造方法は、前記第一のリン酸金属塩が、Al、Mg、Ni、およびZnの中から選ばれる1種または2種以上の前記金属の前記リン酸金属塩であってもよい。
(11)上記(9)または(10)に記載の方向性電磁鋼板の製造方法は、前記第二のリン酸金属塩が、V、W、およびZrの中から選ばれる1種または2種以上の前記金属の前記リン酸金属塩であってもよい。
(12)上記(9)〜(11)のいずれか一項に記載の方向性電磁鋼板の製造方法は、前記重合補助剤が、亜硝酸、亜硝酸ナトリウム、亜硝酸カリウム、硝酸、硝酸ナトリウム、硝酸カリウム、亜塩素酸、亜塩素酸ナトリウム、ホスホン酸、ホスホン酸ナトリウム、トリリン酸、トリリン酸ナトリウム、ポリリン酸、及びポリリン酸ナトリウムからなる群から選択される一種以上であってもよい。
(13)上記(9)〜(12)のいずれか一項に記載の方向性電磁鋼板の製造方法は、前記絶縁被膜処理液が、さらに、ホウ酸、ホウ酸ナトリウム、酸化チタン、酸化モリブテン、顔料、およびチタン酸バリウムからなる群から選択される一種以上を含んでもよい。
(14)上記(9)〜(13)のいずれか一項に記載の方向性電磁鋼板の製造方法は、前記鋼板が、単位質量%で、C:0.005%以下、Si:2.5〜7.0%、Mn:0〜1.0%、Al:0〜0.03%、N:0.01%以下、P:0.01%以下、及びS:0.01%以下を含有し、残部がFeおよび不純物からなり、前記鋼板の平均結晶粒径は、1〜10mmであり、前記鋼板の(110)[001]の結晶方位と圧延方向とのなす角は、平均で8°以下であってもよい。
また、密着性は、各鋼板にセロハンテープを貼り付け後、各鋼板を10mm、20mm、30mmの各直径の丸棒に巻き付けた際に、絶縁被膜が剥離した径にて評価した。なお、表3において、「0」は、鋼板を巻きつける丸棒の径が10mm径でも絶縁被膜が剥離しなかった場合を示す。20mmまたは30mmの各直径の丸棒に巻き付けた際に絶縁被膜に剥離が生じなかった試料は、密着性について合格と判断された。
各種磁気特性は、JIS C2556に規定されている単板磁気特性試験(Single Sheet Tester:SST試験)により測定した。B8が1.91以上であり、且つW17/50が0.83以下であった試料は、磁気特性について合格と判断された。
耐蝕性は5%塩水噴霧試験で評価した。暴露時間は10時間とした。発錆状況を10段階評価し、錆発生無しの試料を耐蝕性10とみなし、発錆箇所の面積率50%の試料を耐蝕性1とみなした。耐蝕性7以上の試料を、耐蝕性に関して合格とした。
Claims (14)
- 鋼板と絶縁被膜とを備える方向性電磁鋼板であって、
前記絶縁被膜が、
Al、Fe、Mg、Mn、Ni、およびZnの中から選ばれる1種または2種以上の金属のリン酸金属塩である第一のリン酸金属塩と;
Co、Mo、V、W、およびZrの中から選ばれる1種または2種以上の金属のリン酸金属塩である第二のリン酸金属塩と;
シリカと;
を含有し、
前記絶縁被膜がクロム酸塩を含有せず、
前記方向性電磁鋼板を沸騰させた純水中で10分間煮沸し、前記純水中に溶出したリン酸の量を測定し、前記リン酸の量を煮沸された前記方向性電磁鋼板の前記絶縁被膜の面積で割ることで測定される、前記絶縁被膜のリン酸溶出量が30mg/m2以下である
ことを特徴とする方向性電磁鋼板(ただし、前記絶縁被膜中に塩化物または塩化物イオンを含有するものを除く)。 - 前記第一のリン酸金属塩が、Al、Mg、Ni、およびZnの中から選ばれる1種または2種以上の前記金属の前記リン酸金属塩であることを特徴とする請求項1に記載の方向性電磁鋼板。
- 前記第二のリン酸金属塩が、V、W、およびZrの中から選ばれる1種または2種以上の前記金属の前記リン酸金属塩であることを特徴とする請求項1または2に記載の方向性電磁鋼板。
- 前記第二のリン酸金属塩の含有率は、前記絶縁被膜の総質量に対して0.5〜10.0質量%であることを特徴とする請求項1〜3のいずれか一項に記載の方向性電磁鋼板。
- 前記シリカの含有率は、前記絶縁被膜の総質量に対して、25〜55質量%であることを特徴とする請求項1〜4のいずれか一項に記載の方向性電磁鋼板。
- 前記絶縁被膜の被膜量が2.0〜7.0g/m2であることを特徴とする請求項1〜5のいずれか一項に記載の方向性電磁鋼板。
- 前記絶縁被膜が、さらに、ホウ酸、ホウ酸ナトリウム、酸化チタン、酸化モリブテン、顔料、およびチタン酸バリウムからなる群から選択される一種以上を含むことを特徴とする請求項1〜6のいずれか一項に記載の方向性電磁鋼板。
- 前記鋼板は、単位質量%で、
C:0.005%以下、
Si:2.5〜7.0%、
Mn:0〜1.0%、
Al:0〜0.03%、
N:0.01%以下、
P:0.01%以下、及び
S:0.01%以下
を含有し、残部がFeおよび不純物からなり、
前記鋼板の平均結晶粒径は、1〜10mmであり、
前記鋼板の(110)[001]の結晶方位と圧延方向とのなす角は、平均で8°以下である
ことを特徴とする請求項1〜7のいずれか一項に記載の方向性電磁鋼板。 - 絶縁被膜処理液を鋼板の表面に塗布する工程と;
前記絶縁被膜処理液を焼き付けて絶縁被膜を成膜する工程と;
を備え、
前記絶縁被膜処理液は、
固形分換算で100質量部の、Al、Fe、Mg、Mn、Ni、およびZnの中から選ばれる1種または2種以上の金属のリン酸金属塩である第一のリン酸金属塩と;
固形分換算で3〜20質量部の、Co、Mo、V、W、およびZrの中から選ばれる1種または2種以上の金属のリン酸金属塩である第二のリン酸金属塩と;
固形分換算で35〜125質量部のコロイド状シリカと;
0.3〜6.0質量部の重合補助剤と;
を含有し、
前記焼き付けでは、100〜800℃の温度範囲での昇温速度30℃/秒以上、焼付均熱温度800〜1000℃、及び均熱保持時間10〜60秒とされ、
前記コロイド状シリカの平均一次粒径が7〜30nmである
ことを特徴とする方向性電磁鋼板の製造方法。 - 前記第一のリン酸金属塩が、Al、Mg、Ni、およびZnの中から選ばれる1種または2種以上の前記金属の前記リン酸金属塩であることを特徴とする請求項9に記載の方向性電磁鋼板の製造方法。
- 前記第二のリン酸金属塩が、V、W、およびZrの中から選ばれる1種または2種以上の前記金属の前記リン酸金属塩であることを特徴とする請求項9または10に記載の方向性電磁鋼板の製造方法。
- 前記重合補助剤が、亜硝酸、亜硝酸ナトリウム、亜硝酸カリウム、硝酸、硝酸ナトリウム、硝酸カリウム、亜塩素酸、亜塩素酸ナトリウム、ホスホン酸、ホスホン酸ナトリウム、トリリン酸、トリリン酸ナトリウム、ポリリン酸、及びポリリン酸ナトリウムからなる群から選択される一種以上であることを特徴とする請求項9〜11のいずれか一項に記載の方向性電磁鋼板の製造方法。
- 前記絶縁被膜処理液が、さらに、ホウ酸、ホウ酸ナトリウム、酸化チタン、酸化モリブテン、顔料、およびチタン酸バリウムからなる群から選択される一種以上を含むことを特徴とする請求項9〜12のいずれか一項に記載の方向性電磁鋼板の製造方法。
- 前記鋼板は、単位質量%で、
C:0.005%以下、
Si:2.5〜7.0%、
Mn:0〜1.0%、
Al:0〜0.03%、
N:0.01%以下、
P:0.01%以下、及び
S:0.01%以下
を含有し、残部がFeおよび不純物からなり、
前記鋼板の平均結晶粒径は、1〜10mmであり、
前記鋼板の(110)[001]の結晶方位と圧延方向とのなす角は、平均で8°以下である
ことを特徴とする請求項9〜13のいずれか一項に記載の方向性電磁鋼板の製造方法。
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ES2800478T3 (es) * | 2015-02-03 | 2020-12-30 | Nippon Steel Corp | Lámina de acero para un depósito de combustible |
EP3276043B1 (en) * | 2015-03-27 | 2021-12-15 | JFE Steel Corporation | Insulating-coated oriented magnetic steel sheet and method for manufacturing same |
DE102016205814A1 (de) * | 2015-04-07 | 2016-10-13 | Chemetall Gmbh | Verfahren zur gezielten Einstellung der elektrischen Leitfähigkeit von Konversionsbeschichtungen |
CN107923046B (zh) * | 2015-09-02 | 2020-11-17 | 杰富意钢铁株式会社 | 绝缘被膜处理液和带有绝缘被膜的金属的制造方法 |
KR20170073311A (ko) * | 2015-12-18 | 2017-06-28 | 주식회사 포스코 | 방향성 전기강판용 절연피막 조성물, 방향성 전기강판의 절연피막 형성 방법, 및 절연피막이 형성된 방향성 전기강판 |
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PL3358041T3 (pl) | 2021-09-06 |
EP3358041B1 (en) | 2021-03-24 |
RU2688982C1 (ru) | 2019-05-23 |
JPWO2017057513A1 (ja) | 2018-08-30 |
US11072861B2 (en) | 2021-07-27 |
KR102071515B1 (ko) | 2020-01-30 |
CN108026645B (zh) | 2020-09-08 |
EP3358041A4 (en) | 2019-04-03 |
WO2017057513A1 (ja) | 2017-04-06 |
KR20180044947A (ko) | 2018-05-03 |
US20190186018A1 (en) | 2019-06-20 |
CN108026645A (zh) | 2018-05-11 |
EP3358041A1 (en) | 2018-08-08 |
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