JPWO2018051902A1 - クロムフリー絶縁張力被膜付き方向性電磁鋼板およびその製造方法 - Google Patents
クロムフリー絶縁張力被膜付き方向性電磁鋼板およびその製造方法 Download PDFInfo
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- JPWO2018051902A1 JPWO2018051902A1 JP2017557219A JP2017557219A JPWO2018051902A1 JP WO2018051902 A1 JPWO2018051902 A1 JP WO2018051902A1 JP 2017557219 A JP2017557219 A JP 2017557219A JP 2017557219 A JP2017557219 A JP 2017557219A JP WO2018051902 A1 JPWO2018051902 A1 JP WO2018051902A1
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- Prior art keywords
- steel sheet
- electrical steel
- grain
- oriented electrical
- chromium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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- 238000000576 coating method Methods 0.000 title claims abstract description 91
- 239000011248 coating agent Substances 0.000 title claims abstract description 86
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- 229910000976 Electrical steel Inorganic materials 0.000 title claims abstract description 4
- 229910001224 Grain-oriented electrical steel Inorganic materials 0.000 claims abstract description 50
- 150000001875 compounds Chemical class 0.000 claims abstract description 46
- 238000010438 heat treatment Methods 0.000 claims abstract description 46
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 27
- 238000000137 annealing Methods 0.000 claims abstract description 27
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 24
- 239000010452 phosphate Substances 0.000 claims abstract description 24
- 229910052742 iron Inorganic materials 0.000 claims abstract description 23
- 239000012298 atmosphere Substances 0.000 claims abstract description 21
- 239000008119 colloidal silica Substances 0.000 claims abstract description 18
- 238000011282 treatment Methods 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 229910052751 metal Inorganic materials 0.000 claims abstract description 12
- 239000002184 metal Substances 0.000 claims abstract description 12
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 11
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 10
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 10
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 8
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 8
- 229910052802 copper Inorganic materials 0.000 claims abstract description 7
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 7
- 229910052706 scandium Inorganic materials 0.000 claims abstract description 7
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 7
- 235000021317 phosphate Nutrition 0.000 claims description 25
- 230000001590 oxidative effect Effects 0.000 claims description 15
- 239000007787 solid Substances 0.000 claims description 15
- 239000013078 crystal Substances 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 3
- 150000003013 phosphoric acid derivatives Chemical class 0.000 claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims description 3
- 229910052785 arsenic Inorganic materials 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 abstract description 22
- 229910000831 Steel Inorganic materials 0.000 abstract description 18
- 239000010959 steel Substances 0.000 abstract description 18
- 238000002156 mixing Methods 0.000 abstract description 3
- MYLBTCQBKAKUTJ-UHFFFAOYSA-N 7-methyl-6,8-bis(methylsulfanyl)pyrrolo[1,2-a]pyrazine Chemical compound C1=CN=CC2=C(SC)C(C)=C(SC)N21 MYLBTCQBKAKUTJ-UHFFFAOYSA-N 0.000 abstract 1
- 229910052750 molybdenum Inorganic materials 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 37
- 238000000034 method Methods 0.000 description 32
- 239000012299 nitrogen atmosphere Substances 0.000 description 30
- 238000009413 insulation Methods 0.000 description 16
- 238000010828 elution Methods 0.000 description 14
- 239000000843 powder Substances 0.000 description 12
- 238000012360 testing method Methods 0.000 description 12
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 11
- 239000011651 chromium Substances 0.000 description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 10
- 229910052804 chromium Inorganic materials 0.000 description 10
- 239000001301 oxygen Substances 0.000 description 10
- 229910052760 oxygen Inorganic materials 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 8
- 239000002245 particle Substances 0.000 description 8
- 239000010949 copper Substances 0.000 description 7
- 239000011777 magnesium Substances 0.000 description 7
- 239000011572 manganese Substances 0.000 description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 238000002425 crystallisation Methods 0.000 description 6
- 230000008025 crystallization Effects 0.000 description 6
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 6
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 5
- 229910052839 forsterite Inorganic materials 0.000 description 5
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 5
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 4
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 238000000975 co-precipitation Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000003746 solid phase reaction Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- GVALZJMUIHGIMD-UHFFFAOYSA-H magnesium phosphate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GVALZJMUIHGIMD-UHFFFAOYSA-H 0.000 description 2
- 239000004137 magnesium phosphate Substances 0.000 description 2
- 229960002261 magnesium phosphate Drugs 0.000 description 2
- 229910000157 magnesium phosphate Inorganic materials 0.000 description 2
- 235000010994 magnesium phosphates Nutrition 0.000 description 2
- GEYXPJBPASPPLI-UHFFFAOYSA-N manganese(iii) oxide Chemical compound O=[Mn]O[Mn]=O GEYXPJBPASPPLI-UHFFFAOYSA-N 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- -1 organic acid salt Chemical class 0.000 description 2
- 238000004445 quantitative analysis Methods 0.000 description 2
- 238000001953 recrystallisation Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000000790 scattering method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- JIPBPJZISZCBJQ-UHFFFAOYSA-N 1-[(2-methylpropan-2-yl)oxycarbonyl]-3-(pyridin-4-ylmethyl)piperidine-3-carboxylic acid Chemical compound C1N(C(=O)OC(C)(C)C)CCCC1(C(O)=O)CC1=CC=NC=C1 JIPBPJZISZCBJQ-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 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
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 150000001639 boron compounds Chemical class 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 150000001845 chromium compounds Chemical class 0.000 description 1
- IUYLTEAJCNAMJK-UHFFFAOYSA-N cobalt(2+);oxygen(2-) Chemical compound [O-2].[Co+2] IUYLTEAJCNAMJK-UHFFFAOYSA-N 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(II) oxide Inorganic materials [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 238000005097 cold rolling Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910000365 copper sulfate Inorganic materials 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- MSNWSDPPULHLDL-UHFFFAOYSA-K ferric hydroxide Chemical compound [OH-].[OH-].[OH-].[Fe+3] MSNWSDPPULHLDL-UHFFFAOYSA-K 0.000 description 1
- 239000000383 hazardous chemical Substances 0.000 description 1
- 238000005098 hot rolling Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 235000014413 iron hydroxide Nutrition 0.000 description 1
- 229910000358 iron sulfate Inorganic materials 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- SZQUEWJRBJDHSM-UHFFFAOYSA-N iron(3+);trinitrate;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O SZQUEWJRBJDHSM-UHFFFAOYSA-N 0.000 description 1
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- SEGOJYCSWLUCKJ-UHFFFAOYSA-N magnesium dinitrate tetrahydrate Chemical compound O.O.O.O.[Mg++].[O-][N+]([O-])=O.[O-][N+]([O-])=O SEGOJYCSWLUCKJ-UHFFFAOYSA-N 0.000 description 1
- 230000005381 magnetic domain Effects 0.000 description 1
- 229940099596 manganese sulfate Drugs 0.000 description 1
- 235000007079 manganese sulphate Nutrition 0.000 description 1
- 239000011702 manganese sulphate Substances 0.000 description 1
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Classifications
-
- 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
- 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
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
-
- 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
- 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
- C23C22/08—Orthophosphates
-
- 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
- C23C22/08—Orthophosphates
- C23C22/12—Orthophosphates containing zinc cations
-
- 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
- C23C22/08—Orthophosphates
- C23C22/12—Orthophosphates containing zinc cations
- C23C22/13—Orthophosphates containing zinc cations containing also nitrate or nitrite anions
-
- 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
- C23C22/08—Orthophosphates
- C23C22/18—Orthophosphates containing manganese cations
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Abstract
Description
ただし、一般式(1)中、MII、MIIIは、それぞれ独立して、Sc,Ti,V,Mn,Fe,Co,Ni,Cu,Mgのうちから選ばれる1種または2種以上であり、XVは、P,V,Moのうちから選ばれる1種または2種以上である。
耐吸湿性は、絶縁張力被膜付き方向性電磁鋼板から作製した50mm×50mmの試験片3枚を、100℃の蒸留水中で5分間浸漬煮沸することにより絶縁張力被膜表面からリンを溶出させ、その溶出量[μg/150cm2]によって絶縁張力被膜の水に対する溶解のしやすさを判断するものである。溶出量が150[μg/150cm2]以下を良好とした。P(リン)の溶出量測定方法は特に限定するものではないが、本願では、ICP発光分析で定量分析を行った。
[1]方向性電磁鋼板の少なくとも一方の表面にリン酸塩とシリカを含有する絶縁張力被膜を有し、かつ前記被膜内部に下記一般式(1)で表される結晶性の化合物が存在することを特徴とする、クロムフリー絶縁張力被膜付き方向性電磁鋼板。
MII 3MIII 4(XVO4)6 ・・・(1)
ただし、一般式(1)中、MII、MIIIは、それぞれ独立して、Sc,Ti,V,Mn,Fe,Co,Ni,Cu,Mgのうちから選ばれる1種または2種以上であり、XVは、P,V,Moのうちから選ばれる1種または2種以上である。
[2]前記一般式(1)中、MIIIがFeであり、XVがPであることを特徴とする、[1]に記載のクロムフリー絶縁張力被膜付き方向性電磁鋼板。
[3]前記一般式(1)で表される結晶性の化合物がFe7(PO4)6であることを特徴とする、[1]または[2]に記載のクロムフリー絶縁張力被膜付き方向性電磁鋼板。
[4]前記リン酸塩がMg,Fe,Al,Ca,MnおよびZnのリン酸塩のうちから選ばれる1種または2種以上からなることを特徴とする、[1]〜[3]のいずれかに記載のクロムフリー絶縁張力被膜付き方向性電磁鋼板。
[1]から[4]のいずれかに記載のクロムフリー絶縁張力被膜付き方向性電磁鋼板の製造方法であって、仕上焼鈍後の方向性電磁鋼板の少なくとも一方の表面に、固形分換算でコロイド状シリカ20質量部に対して、リン酸塩10〜80質量部と、酸化物換算で金属元素Mを含む化合物(ただし、前記金属元素Mは、Sc,Ti,V,Mn,Fe,Co,Ni,Cu,Mgのうちから選ばれる1種または2種以上)5〜10質量部を配合した絶縁張力被膜用処理液を塗布して、非酸化性のガスを用いかつ露点を0℃以下とした雰囲気下で900℃以上に加熱する熱処理を少なくとも1回行うことを特徴とする、クロムフリー絶縁張力被膜付き方向性電磁鋼板の製造方法。
[6][1]から[4]のいずれかに記載のクロムフリー絶縁張力被膜付き方向性電磁鋼板の製造方法であって、
仕上焼鈍後の方向性電磁鋼板の少なくとも一方の表面に、固形分換算でコロイド状シリカ20質量部に対して、リン酸塩10〜80質量部と、前記一般式(1)で表される結晶性の化合物を配合した絶縁張力被膜用処理液を塗布して、非酸化性雰囲気下で少なくとも1回の加熱処理を行うことを特徴とする、クロムフリー絶縁張力被膜付き方向性電磁鋼板の製造方法。
仕上焼鈍後の方向性電磁鋼板の表面に、表2に示した配合の絶縁張力被膜用処理液を両面合計で10g/m2となるように塗布して、あらかじめ乾燥炉で250℃×120秒間で乾燥し、露点−20℃のN2雰囲気で800℃×2分間の加熱処理を施した。
耐吸湿性は、絶縁張力被膜付き方向性電磁鋼板から作製した50mm×50mmの試験片3枚を、100℃の蒸留水中で5分間浸漬煮沸することにより絶縁張力被膜表面からリンを溶出させ、その溶出量[μg/150cm2]によって絶縁張力被膜の水に対する溶解のしやすさを判断するものである。溶出量が150[μg/150cm2]以下を良好とした。Pの溶出量測定方法は特に限定するものではないが、本願では、ICP発光分析で定量分析を行った。
固形分換算でコロイド状シリカ20質量部に対し、第1リン酸アルミニウム40質量部と、表3に示したMII 3MIII 4(XVO4)6 で表される結晶性の化合物5質量部を添加した絶縁張力被膜用処理液を調製した。なお、表3に示した前記結晶性の化合物は、それぞれ以下の手順で調製し、得られた粉末をX線回折分析して回折ピークによりその存在を確認した。また、得られた粉末の平均粒径をレーザー回折散乱法によって測定し、平均粒径が1.0μm以下であることを確認した。なお、X線回折分析はCuターゲットを用い20kV、250mAの条件で測定を行い、X線回折パターン解析ソフトウェアJADE(Rigaku社製)を用いて、回折パターンのバックグラウンドを除し、観測された回折ピークから結晶系の同定を行った。
記号イ、記号ウ、記号エ:硝酸マグネシウム(II)四水和物と硝酸マンガン(II)六水和物、硝酸鉄(III)九水和物を溶解させたリン酸にアンモニアを加えることで粉末を析出させた(共沈法)。
記号オ:酸化銅(II)、酸化鉄(III)、五酸化バナジウムの粉末を混合したものを900℃、48時間で反応させて粉末を得た(固相反応法)。
記号カ:酸化コバルト(II)、酸化鉄(III)、五酸化バナジウムの粉末を混合したものを800℃、20時間で反応させて粉末を得た(固相反応法)。
記号キ:酸化マンガン(III)、酸化鉄(III)、五酸化バナジウムの粉末を混合したものを700℃、20時間で反応させて粉末を得た(固相反応法)。
Claims (6)
- 方向性電磁鋼板の少なくとも一方の表面にリン酸塩とシリカを含有する絶縁張力被膜を有し、かつ前記被膜内部に下記一般式(1)で表される結晶性の化合物が存在することを特徴とする、クロムフリー絶縁張力被膜付き方向性電磁鋼板。
MII 3MIII 4(XVO4)6 ・・・(1)
ただし、一般式(1)中、MII、MIIIは、それぞれ独立して、Sc,Ti,V,Mn,Fe,Co,Ni,Cu,Mgのうちから選ばれる1種または2種以上であり、XVは、P,V,Moのうちから選ばれる1種または2種以上である。 - 前記一般式(1)中、MIIIがFeであり、XVがPであることを特徴とする、請求項1に記載のクロムフリー絶縁張力被膜付き方向性電磁鋼板。
- 前記一般式(1)で表される結晶性の化合物がFe7(PO4)6であることを特徴とする、請求項1または請求項2に記載のクロムフリー絶縁張力被膜付き方向性電磁鋼板。
- 前記リン酸塩がMg,Fe,Al,Ca,MnおよびZnのリン酸塩のうちから選ばれる1種または2種以上からな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クロムフリー絶縁張力被膜付き方向性電磁鋼板。
- 請求項1から4のいずれか一項に記載のクロムフリー絶縁張力被膜付き方向性電磁鋼板の製造方法であって、
仕上焼鈍後の方向性電磁鋼板の少なくとも一方の表面に、固形分換算でコロイド状シリカ20質量部に対して、リン酸塩10〜80質量部と、酸化物換算で金属元素Mを含む化合物(ただし、前記金属元素Mは、Sc,Ti,V,Mn,Fe,Co,Ni,Cu,Mgのうちから選ばれる1種または2種以上)5〜10質量部を配合した絶縁張力被膜用処理液を塗布して、非酸化性のガスを用いかつ露点を0℃以下とした雰囲気下で900℃以上に加熱する熱処理を少なくとも1回行うことを特徴とする、クロムフリー絶縁張力被膜付き方向性電磁鋼板の製造方法。 - 請求項1から4のいずれか一項に記載のクロムフリー絶縁張力被膜付き方向性電磁鋼板の製造方法であって、
仕上焼鈍後の方向性電磁鋼板の少なくとも一方の表面に、固形分換算でコロイド状シリカ20質量部に対して、リン酸塩10〜80質量部と、前記一般式(1)で表される結晶性の化合物を配合した絶縁張力被膜用処理液を塗布して、非酸化性雰囲気下で少なくとも1回の加熱処理を行うことを特徴とする、クロムフリー絶縁張力被膜付き方向性電磁鋼板の製造方法。
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KR102189461B1 (ko) | 2020-12-11 |
US11756713B2 (en) | 2023-09-12 |
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US20210287834A1 (en) | 2021-09-16 |
KR20190027871A (ko) | 2019-03-15 |
JP6299938B1 (ja) | 2018-03-28 |
CN109563626B (zh) | 2021-04-13 |
WO2018051902A1 (ja) | 2018-03-22 |
EP3476976B1 (en) | 2021-04-14 |
EP3476976A4 (en) | 2019-06-05 |
CA3032648C (en) | 2021-02-02 |
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CN109563626A (zh) | 2019-04-02 |
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