JP5733980B2 - 亜鉛又は亜鉛合金表面を有する金属部材の黒色化成皮膜形成方法及び黒色化防錆皮膜形成方法 - Google Patents
亜鉛又は亜鉛合金表面を有する金属部材の黒色化成皮膜形成方法及び黒色化防錆皮膜形成方法 Download PDFInfo
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- JP5733980B2 JP5733980B2 JP2010529748A JP2010529748A JP5733980B2 JP 5733980 B2 JP5733980 B2 JP 5733980B2 JP 2010529748 A JP2010529748 A JP 2010529748A JP 2010529748 A JP2010529748 A JP 2010529748A JP 5733980 B2 JP5733980 B2 JP 5733980B2
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- 238000006243 chemical reaction Methods 0.000 title claims description 102
- 239000000126 substance Substances 0.000 title claims description 101
- 229910052751 metal Inorganic materials 0.000 title claims description 55
- 239000002184 metal Substances 0.000 title claims description 55
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 title claims description 53
- 238000000034 method Methods 0.000 title claims description 51
- 229910001297 Zn alloy Inorganic materials 0.000 title claims description 42
- 239000011701 zinc Substances 0.000 title claims description 40
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims description 39
- 229910052725 zinc Inorganic materials 0.000 title claims description 39
- 230000003449 preventive effect Effects 0.000 title claims description 17
- 239000007864 aqueous solution Substances 0.000 claims description 73
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 34
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 33
- -1 iron ion Chemical class 0.000 claims description 31
- 239000000243 solution Substances 0.000 claims description 25
- 238000000576 coating method Methods 0.000 claims description 22
- 239000011248 coating agent Substances 0.000 claims description 19
- 229910052684 Cerium Inorganic materials 0.000 claims description 18
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 16
- 229910052742 iron Inorganic materials 0.000 claims description 16
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 16
- 239000012756 surface treatment agent Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000000377 silicon dioxide Substances 0.000 claims description 13
- 150000001875 compounds Chemical class 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 11
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 claims description 11
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 11
- 239000010936 titanium Substances 0.000 claims description 11
- 229910052719 titanium Inorganic materials 0.000 claims description 11
- 239000013522 chelant Substances 0.000 claims description 10
- 229910001437 manganese ion Inorganic materials 0.000 claims description 10
- 239000008119 colloidal silica Substances 0.000 claims description 7
- 238000007739 conversion coating Methods 0.000 claims description 7
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 5
- 238000004453 electron probe microanalysis Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- WAEMQWOKJMHJLA-UHFFFAOYSA-N Manganese(2+) Chemical compound [Mn+2] WAEMQWOKJMHJLA-UHFFFAOYSA-N 0.000 claims description 4
- 229910001430 chromium ion Inorganic materials 0.000 claims description 4
- 238000004458 analytical method Methods 0.000 claims description 3
- 239000010408 film Substances 0.000 description 113
- 238000012360 testing method Methods 0.000 description 30
- 239000010410 layer Substances 0.000 description 27
- 230000002265 prevention Effects 0.000 description 25
- 229910052804 chromium Inorganic materials 0.000 description 16
- 239000011651 chromium Substances 0.000 description 16
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 15
- 238000007747 plating Methods 0.000 description 14
- 239000000047 product Substances 0.000 description 14
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 12
- 241001163841 Albugo ipomoeae-panduratae Species 0.000 description 10
- 239000000203 mixture Substances 0.000 description 10
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 9
- 238000004381 surface treatment Methods 0.000 description 9
- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 description 9
- 229910000165 zinc phosphate Inorganic materials 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 7
- 229910002651 NO3 Inorganic materials 0.000 description 7
- 229910045601 alloy Inorganic materials 0.000 description 7
- 239000000956 alloy Substances 0.000 description 7
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- 239000007921 spray Substances 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 5
- 230000002378 acidificating effect Effects 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 5
- 229910000640 Fe alloy Inorganic materials 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 3
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 3
- 229910007567 Zn-Ni Inorganic materials 0.000 description 3
- 229910007614 Zn—Ni Inorganic materials 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 229910001429 cobalt ion Inorganic materials 0.000 description 3
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 238000007598 dipping method Methods 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 239000011572 manganese Substances 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- RWLALWYNXFYRGW-UHFFFAOYSA-N 2-Ethyl-1,3-hexanediol Chemical compound CCCC(O)C(CC)CO RWLALWYNXFYRGW-UHFFFAOYSA-N 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- 229910001335 Galvanized steel Inorganic materials 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical group [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 2
- 239000002738 chelating agent Substances 0.000 description 2
- 150000001845 chromium compounds Chemical class 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 229960005082 etohexadiol Drugs 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000008397 galvanized steel Substances 0.000 description 2
- QOSATHPSBFQAML-UHFFFAOYSA-N hydrogen peroxide;hydrate Chemical compound O.OO QOSATHPSBFQAML-UHFFFAOYSA-N 0.000 description 2
- CPSYWNLKRDURMG-UHFFFAOYSA-L hydron;manganese(2+);phosphate Chemical compound [Mn+2].OP([O-])([O-])=O CPSYWNLKRDURMG-UHFFFAOYSA-L 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 229910000398 iron phosphate Inorganic materials 0.000 description 2
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 229940085991 phosphate ion Drugs 0.000 description 2
- 238000012643 polycondensation polymerization Methods 0.000 description 2
- 238000009987 spinning Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 2
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 2
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 description 1
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- 108010010803 Gelatin Proteins 0.000 description 1
- AEMRFAOFKBGASW-UHFFFAOYSA-M Glycolate Chemical compound OCC([O-])=O AEMRFAOFKBGASW-UHFFFAOYSA-M 0.000 description 1
- 241000282412 Homo Species 0.000 description 1
- 206010020751 Hypersensitivity Diseases 0.000 description 1
- 229910021380 Manganese Chloride Inorganic materials 0.000 description 1
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 229910001229 Pot metal Inorganic materials 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 125000003158 alcohol group Chemical group 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 208000026935 allergic disease Diseases 0.000 description 1
- 230000007815 allergy Effects 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000011088 calibration curve Methods 0.000 description 1
- 238000009924 canning Methods 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 150000001785 cerium compounds Chemical class 0.000 description 1
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000009500 colour coating Methods 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 229960002089 ferrous chloride Drugs 0.000 description 1
- 229910001448 ferrous ion Inorganic materials 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000005246 galvanizing Methods 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000013461 intermediate chemical Substances 0.000 description 1
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 1
- KFZAUHNPPZCSCR-UHFFFAOYSA-N iron zinc Chemical compound [Fe].[Zn] KFZAUHNPPZCSCR-UHFFFAOYSA-N 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
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 239000011565 manganese chloride Substances 0.000 description 1
- 235000002867 manganese chloride Nutrition 0.000 description 1
- 229940099607 manganese chloride Drugs 0.000 description 1
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 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
- 239000012528 membrane Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- QELJHCBNGDEXLD-UHFFFAOYSA-N nickel zinc Chemical compound [Ni].[Zn] QELJHCBNGDEXLD-UHFFFAOYSA-N 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 235000018553 tannin Nutrition 0.000 description 1
- 229920001864 tannin Polymers 0.000 description 1
- 239000001648 tannin Substances 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 238000013519 translation Methods 0.000 description 1
- 229910001456 vanadium ion Inorganic materials 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
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
- C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
- C23C10/18—Solid state diffusion of only metal elements or silicon into metallic material surfaces using liquids, e.g. salt baths, liquid suspensions
- C23C10/20—Solid state diffusion of only metal elements or silicon into metallic material surfaces using liquids, e.g. salt baths, liquid suspensions only one element being diffused
- C23C10/24—Salt bath containing the element to be diffused
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/48—After-treatment of electroplated surfaces
-
- 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
- C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
- C23C10/18—Solid state diffusion of only metal elements or silicon into metallic material surfaces using liquids, e.g. salt baths, liquid suspensions
- C23C10/26—Solid state diffusion of only metal elements or silicon into metallic material surfaces using liquids, e.g. salt baths, liquid suspensions more than one element being diffused
-
- 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
- C23C12/00—Solid state diffusion of at least one non-metal element other than silicon and at least one metal element or silicon into metallic material surfaces
-
- 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
- C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
- C23C2/04—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor characterised by the coating material
- C23C2/06—Zinc or cadmium or alloys based thereon
-
- 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
- C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
- C23C2/26—After-treatment
-
- 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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- 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
- C23C22/48—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 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
- C23C22/53—Treatment of zinc or alloys based thereon
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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
- 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
- C23C22/82—After-treatment
- C23C22/83—Chemical after-treatment
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
- C25D3/565—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of zinc
Description
亜鉛めっき表面を黒色化するには、黒色化成分を含む化成処理液を用いるのが好ましいが、化成処理液を用いる方法の他に、Ni,Co,Fe,Cu,Cr,Mo,Sn等の黒色化成分と亜鉛とからなる合金をめっきし、この亜鉛合金めっき表面を硝酸イオンとリン酸イオンを含む酸性溶液で処理する方法も知られている(特許文献13)。この方法では、亜鉛合金めっき表面から亜鉛イオンと金属イオンが溶解し、金属の酸化物とリン酸塩化合物からなる黒色外観の複合皮膜が亜鉛合金めっきの溶解部分に置換されて形成される。この方法は、コストが安価な故に多用されている亜鉛めっきと比べて、合金成分を亜鉛めっきに含ませることが必要になり、合金めっき浴の管理が難しくなる他、金属イオンの溶解量や皮膜の組成を制御することが難しい等の理由によりコスト高となる。
さらに、重亜硫酸塩と、硫酸アルミニウム又はゼラチンを含む水溶液による亜鉛又は亜鉛合金めっき表面の化成処理方法が提案されている(特許文献5)が、防錆性能は低く、塩水噴霧試験において48時間で白錆が発生するので実用レベルの防錆性能を満たしているとは言い難い。また、亜鉛又は亜鉛合金めっき表面のクロムフリーの防錆皮膜処理方法として2層構造以上の皮膜を形成する方法が提案されている(特許文献6)が、黒色の色調を呈する表面処理方法は開示されていない。また、セリウム(Ce)陽イオンと過酸化水素を含有する酸性水溶液から、アルミニウムや亜鉛に耐食性のセリウムを含む表面コーティングを形成する方法が知られている(特許文献7、8、非特許文献1)。
リン酸イオンを5〜20g、2価鉄イオンを0.1〜3g、2価マンガンイオンを1〜1
0g、硝酸イオンを1〜3g含み、pHが1〜3である水溶液中に亜鉛又は亜鉛合金表面
を有する金属部材を、水溶液の温度5〜40℃で10〜60秒浸漬して化成処理すること
を特徴とする黒色化成皮膜の形成方法、である。
色皮膜が形成される。
る金属部材の表面に黒色の第一の化成皮膜を形成した後、水洗し、次いで、(B)該金属
部材を、1リットル中に3価セリウムイオンを0.3〜6.5g含み、pHを1〜4に調
整した水溶液中に浸漬して化成処理することによって該表面にセリウム酸化物からなる皮
膜である第二の化成皮膜を形成した後、水洗し、次いで、(C)シリカ成分の供給源物質
を含有する表面処理剤を第二の化成皮膜上に塗布して、シリカ質皮膜である第三の皮膜を
形成する、ことを特徴とする亜鉛又は亜鉛合金表面を有する金属部材のクロムフリー黒色
化防錆皮膜形成方法、である。
リカ水溶液を混合し、第二の化成皮膜中にシリカ成分が1〜30重量%含まれるようにす
ることが好ましい。
処理剤が、チタンのキレート化合物と反応させた重量平均分子量が1,000〜10,0
00であるアルコキシシランオリゴマーのアルコール溶液からなるようにすることが好ま
しい。
の化成皮膜の厚さが0.1〜1.0μm、第三の皮膜の厚さが0.4〜2.0μmである
ことが好ましい。なお、本発明において皮膜の厚さは、表面処理された金属部材断面の顕
微鏡写真を撮り、顕微鏡写真の画像で測定して求めた値である。
析で実質的に四三酸化鉄(Fe3O4)である黒色の第一の化成皮膜、第一の化成皮膜上の
セリウム酸化物からなる皮膜である第二の化成皮膜、及び第二の化成皮膜上にシリカ質皮
膜である第三の皮膜の少なくとも3層からなる黒色の色調を呈する防錆皮膜を有し、第一
の化成皮膜が第1の本発明の方法で形成されたものであることを特徴とする金属部材、で
ある。
SWCH(冷間圧造用炭素鋼線材)で作られた六角ボルト(M8×45半ネジ)にジンケート浴(カニングジャパン(株)製CFZ20)を用いて厚さ8〜10μmの亜鉛めっきを施したボルトを試験片に用いた。純水中に表1の上段に示す質量(g)の化合物を記載順に溶解して実施例(1)、(2)及び(3)の黒色化化成処理用水溶液を1リットル調製した。表1の下段に各イオンの含有量をg/Lで示す。全化合物を溶解した時点で水溶液のpHは2であった。亜鉛めっきボルトの試験片3個を25℃の黒色化化成処理用水溶液に30秒間浸漬して取り出した。
六角ボルト(M8×45半ネジ)3個に、厚さ8〜10μmのZn−Ni合金めっき(Niの共析率約15重量%)を施した以外は、実施例3と同様にして表面処理をZn−Ni合金めっきボルトの試験片に施し、Zn−Ni合金めっき層の表面に3層の皮膜を形成した。
六角ボルト(M8×45半ネジ)3個に、厚さ8〜10μmのZn−Fe合金めっき(Feの共析率約0.3重量%)を施した以外は、実施例3と同様にして表面処理をZn−Fe合金めっきボルトの試験片に施し、Zn−Fe合金めっき層の表面に3層の皮膜を形成した。
実施例1〜3と同じ六角ボルト(M8×45半ネジ)の亜鉛めっきされた試験片を用い、実施例1〜3の黒色化化成処理用水溶液を用いてそれぞれ化成処理した。化成処理した3個の試験片について、比較例1は、セリウム化成皮膜とシリカ質皮膜形成の両方をしなかった。比較例2,3は、いずれか一方の表面処理を施さなかった。
表6に示す黒色化化成処理用水溶液を用いて亜鉛めっきボルトの試験片をそれぞれ化成処理した。次に、実施例1〜3と同様に二層目と三層目の皮膜を形成した。
2 第一の化成皮膜
3 第二の化成皮膜
4 シリカ質皮膜
Claims (6)
- 3価及び6価のクロムイオンを含まず、1リットルの該水溶液中に、リン酸イオンを5
〜20g、2価鉄イオンを0.1〜3g、2価マンガンイオンを1〜10g、硝酸イオン
を1〜3g含み、pHが1〜3である水溶液中に亜鉛又は亜鉛合金表面を有する金属部材
を、水溶液の温度5〜40℃で10〜60秒浸漬して化成処理することによって該表面に
EPMA分析で実質的に四三酸化鉄(Fe 3 O 4 )である黒色皮膜を形成することを特徴と
する黒色化成皮膜の形成方法。 - (A)請求項1記載の方法によって亜鉛又は亜鉛合金表面を有する金属部材の表面に黒色
の第一の化成皮膜を形成した後、水洗し、次いで、
(B)該金属部材を、1リットル中に3価セリウムイオンを0.3〜6.5g含み、pH
を1〜4に調整した水溶液中に浸漬して化成処理することによって該表面にセリウム酸化
物からなる皮膜である第二の化成皮膜を形成した後、水洗し、次いで、
(C)シリカ成分の供給源物質を含有する表面処理剤を第二の化成皮膜上に塗布して、シ
リカ質皮膜である第三の皮膜を形成する、
ことを特徴とする亜鉛又は亜鉛合金表面を有する金属部材のクロムフリー黒色化防錆皮膜
形成方法。 - 請求項2記載の方法において、前記(B)工程のセリウムイオンを含む水溶液中にコロ
イダルシリカ水溶液を混合し、第二の化成皮膜中にシリカ成分が1〜30重量%含まれる
ようにすることを特徴とする黒色化防錆皮膜形成方法。 - 請求項2記載の方法において、前記(C)工程のシリカ成分の供給源物質を含有する表
面処理剤が、チタンのキレート化合物と反応させた重量平均分子量が1,000〜10,
000であるアルコキシシランオリゴマーのアルコール溶液からなることを特徴とする黒
色化防錆皮膜形成方法。 - 請求項2記載の方法において、黒色の第一の化成皮膜の厚さが0.1〜1.0μm、第
二の化成皮膜の厚さが0.1〜1.0μm、第三の皮膜の厚さが0.4〜2.0μmであ
ることを特徴とする黒色化防錆皮膜形成方法。 - 亜鉛又は亜鉛合金表面を有する金属部材の表面にEPMA分析で実質的に四三酸化鉄(
Fe 3 O 4 )である黒色の第一の化成皮膜、第一の化成皮膜上のセリウム酸化物からなる皮
膜である第二の化成皮膜、及び第二の化成皮膜上にシリカ質皮膜である第三の皮膜の少な
くとも3層からなる黒色の色調を呈する防錆皮膜を有し、第一の化成皮膜が請求項1記載
の方法で形成されたものであることを特徴とする金属部材。
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JP2006322048A (ja) | 2005-05-19 | 2006-11-30 | Three G Giken:Kk | 化成処理溶液および化成処理方法 |
JP2007058137A (ja) | 2005-08-26 | 2007-03-08 | Fuji Xerox Co Ltd | 電子写真用トナー、及びその製造方法 |
CN101426871B (zh) | 2006-04-18 | 2012-07-04 | 株式会社放电精密加工研究所 | 具有锌表面的金属构件用非铬防锈表面处理剂和具有被其防锈膜被覆的锌表面的金属构件 |
JP2008121101A (ja) | 2006-11-15 | 2008-05-29 | Okada Chelate:Kk | 亜鉛または亜鉛合金めっきされた金属表面上の防錆処理液および防錆皮膜処理方法 |
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2009
- 2009-09-14 WO PCT/JP2009/065991 patent/WO2010032702A1/ja active Application Filing
- 2009-09-14 JP JP2010529748A patent/JP5733980B2/ja active Active
- 2009-09-14 KR KR1020117005790A patent/KR20110054009A/ko active IP Right Grant
- 2009-09-14 CN CN200980135956.XA patent/CN102149848B/zh not_active Expired - Fee Related
- 2009-09-14 US US13/119,045 patent/US20110165426A1/en not_active Abandoned
- 2009-09-14 EP EP09814547A patent/EP2341164A1/en not_active Withdrawn
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JPS5051432A (ja) * | 1973-09-08 | 1975-05-08 | ||
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Publication number | Publication date |
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WO2010032702A1 (ja) | 2010-03-25 |
TW201026894A (en) | 2010-07-16 |
TWI445841B (zh) | 2014-07-21 |
KR20110054009A (ko) | 2011-05-24 |
CN102149848B (zh) | 2014-01-29 |
CN102149848A (zh) | 2011-08-10 |
JPWO2010032702A1 (ja) | 2012-02-09 |
EP2341164A1 (en) | 2011-07-06 |
US20110165426A1 (en) | 2011-07-07 |
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