JP2016132784A - 三価クロム黒色化成皮膜処理液、三価クロム含有水溶性仕上げ処理液及び金属基材の処理方法 - Google Patents
三価クロム黒色化成皮膜処理液、三価クロム含有水溶性仕上げ処理液及び金属基材の処理方法 Download PDFInfo
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- JP2016132784A JP2016132784A JP2015006568A JP2015006568A JP2016132784A JP 2016132784 A JP2016132784 A JP 2016132784A JP 2015006568 A JP2015006568 A JP 2015006568A JP 2015006568 A JP2015006568 A JP 2015006568A JP 2016132784 A JP2016132784 A JP 2016132784A
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- Prior art keywords
- trivalent chromium
- chemical conversion
- compound
- conversion film
- treatment liquid
- 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.)
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- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 title claims abstract description 106
- 229910052804 chromium Inorganic materials 0.000 title claims abstract description 106
- 239000011651 chromium Substances 0.000 title claims abstract description 106
- 239000000126 substance Substances 0.000 title claims abstract description 81
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 35
- 239000002184 metal Substances 0.000 title claims abstract description 35
- 239000000463 material Substances 0.000 title claims abstract description 17
- 238000007739 conversion coating Methods 0.000 title abstract description 19
- 238000000034 method Methods 0.000 title abstract description 14
- 150000001869 cobalt compounds Chemical class 0.000 claims abstract description 32
- -1 organic acid salts Chemical class 0.000 claims abstract description 32
- 150000007524 organic acids Chemical class 0.000 claims abstract description 25
- 150000001845 chromium compounds Chemical class 0.000 claims abstract description 24
- 150000002898 organic sulfur compounds Chemical class 0.000 claims abstract description 13
- 235000005985 organic acids Nutrition 0.000 claims abstract description 9
- 229910002651 NO3 Inorganic materials 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims description 66
- 238000006243 chemical reaction Methods 0.000 claims description 62
- 239000000758 substrate Substances 0.000 claims description 23
- 238000007747 plating Methods 0.000 claims description 21
- 229910017052 cobalt Inorganic materials 0.000 claims description 14
- 239000010941 cobalt Substances 0.000 claims description 14
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 14
- 150000003623 transition metal compounds Chemical class 0.000 claims description 14
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 13
- 229910052725 zinc Inorganic materials 0.000 claims description 13
- 239000011701 zinc Substances 0.000 claims description 13
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 10
- 229910001297 Zn alloy Inorganic materials 0.000 claims description 10
- 239000011737 fluorine Substances 0.000 claims description 10
- 229910052731 fluorine Inorganic materials 0.000 claims description 10
- 239000011574 phosphorus Substances 0.000 claims description 10
- 229910052698 phosphorus Inorganic materials 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 8
- 239000007795 chemical reaction product Substances 0.000 claims description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- 150000002500 ions Chemical class 0.000 claims description 5
- 239000003921 oil Substances 0.000 claims description 5
- 239000011347 resin Substances 0.000 claims description 5
- 229920005989 resin Polymers 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 238000009835 boiling Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000003672 processing method Methods 0.000 claims description 3
- 150000003018 phosphorus compounds Chemical class 0.000 claims description 2
- 238000007730 finishing process Methods 0.000 claims 1
- 238000005260 corrosion Methods 0.000 abstract description 28
- 230000007797 corrosion Effects 0.000 abstract description 28
- 230000007613 environmental effect Effects 0.000 abstract description 5
- 238000012360 testing method Methods 0.000 description 23
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 16
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 14
- 238000012545 processing Methods 0.000 description 12
- 150000003839 salts Chemical class 0.000 description 9
- PHFQLYPOURZARY-UHFFFAOYSA-N chromium trinitrate Chemical compound [Cr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PHFQLYPOURZARY-UHFFFAOYSA-N 0.000 description 8
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 7
- 238000013461 design Methods 0.000 description 7
- 229940093915 gynecological organic acid Drugs 0.000 description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 238000001556 precipitation Methods 0.000 description 6
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 description 6
- 235000015165 citric acid Nutrition 0.000 description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical class O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- 229910017604 nitric acid Inorganic materials 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 229910000151 chromium(III) phosphate Inorganic materials 0.000 description 3
- IKZBVTPSNGOVRJ-UHFFFAOYSA-K chromium(iii) phosphate Chemical compound [Cr+3].[O-]P([O-])([O-])=O IKZBVTPSNGOVRJ-UHFFFAOYSA-K 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- 239000011593 sulfur Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 2
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 235000001014 amino acid Nutrition 0.000 description 2
- 150000001413 amino acids Chemical class 0.000 description 2
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 description 2
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical class [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 2
- 239000013522 chelant Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 2
- 239000005002 finish coating Substances 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical class [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 235000006408 oxalic acid Nutrition 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- 231100000615 substance of very high concern Toxicity 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical class [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 1
- 241001163841 Albugo ipomoeae-panduratae Species 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 229940126062 Compound A Drugs 0.000 description 1
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 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
- QEVGZEDELICMKH-UHFFFAOYSA-N Diglycolic acid Chemical compound OC(=O)COCC(O)=O QEVGZEDELICMKH-UHFFFAOYSA-N 0.000 description 1
- 229910001335 Galvanized steel Inorganic materials 0.000 description 1
- WHUUTDBJXJRKMK-UHFFFAOYSA-N Glutamic acid Natural products OC(=O)C(N)CCC(O)=O WHUUTDBJXJRKMK-UHFFFAOYSA-N 0.000 description 1
- NLDMNSXOCDLTTB-UHFFFAOYSA-N Heterophylliin A Natural products O1C2COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC2C(OC(=O)C=2C=C(O)C(O)=C(O)C=2)C(O)C1OC(=O)C1=CC(O)=C(O)C(O)=C1 NLDMNSXOCDLTTB-UHFFFAOYSA-N 0.000 description 1
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 description 1
- WHUUTDBJXJRKMK-VKHMYHEASA-N L-glutamic acid Chemical compound OC(=O)[C@@H](N)CCC(O)=O WHUUTDBJXJRKMK-VKHMYHEASA-N 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-L Malonate Chemical compound [O-]C(=O)CC([O-])=O OFOBLEOULBTSOW-UHFFFAOYSA-L 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 241000221535 Pucciniales Species 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 1
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 239000011668 ascorbic acid Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000013475 authorization Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 150000001844 chromium Chemical class 0.000 description 1
- GRWVQDDAKZFPFI-UHFFFAOYSA-H chromium(III) sulfate Chemical compound [Cr+3].[Cr+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GRWVQDDAKZFPFI-UHFFFAOYSA-H 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 235000018417 cysteine Nutrition 0.000 description 1
- XUJNEKJLAYXESH-UHFFFAOYSA-N cysteine Natural products SCC(N)C(O)=O XUJNEKJLAYXESH-UHFFFAOYSA-N 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 150000002019 disulfides Chemical class 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- ZEUUVJSRINKECZ-UHFFFAOYSA-N ethanedithioic acid Chemical compound CC(S)=S ZEUUVJSRINKECZ-UHFFFAOYSA-N 0.000 description 1
- 239000008397 galvanized steel Substances 0.000 description 1
- 239000000174 gluconic acid Substances 0.000 description 1
- 235000012208 gluconic acid Nutrition 0.000 description 1
- 239000004220 glutamic acid Substances 0.000 description 1
- 235000013922 glutamic acid Nutrition 0.000 description 1
- 230000009931 harmful effect Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 239000001630 malic acid Substances 0.000 description 1
- 235000011090 malic acid Nutrition 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- YPJKMVATUPSWOH-UHFFFAOYSA-N nitrooxidanyl Chemical compound [O][N+]([O-])=O YPJKMVATUPSWOH-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- KOODSCBKXPPKHE-UHFFFAOYSA-N propanethioic s-acid Chemical compound CCC(S)=O KOODSCBKXPPKHE-UHFFFAOYSA-N 0.000 description 1
- KOUKXHPPRFNWPP-UHFFFAOYSA-N pyrazine-2,5-dicarboxylic acid;hydrate Chemical compound O.OC(=O)C1=CN=C(C(O)=O)C=N1 KOUKXHPPRFNWPP-UHFFFAOYSA-N 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000005871 repellent Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- UVZICZIVKIMRNE-UHFFFAOYSA-N thiodiacetic acid Chemical compound OC(=O)CSCC(O)=O UVZICZIVKIMRNE-UHFFFAOYSA-N 0.000 description 1
- NJRXVEJTAYWCQJ-UHFFFAOYSA-N thiomalic acid Chemical compound OC(=O)CC(S)C(O)=O NJRXVEJTAYWCQJ-UHFFFAOYSA-N 0.000 description 1
- 238000013519 translation Methods 0.000 description 1
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 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
- 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
-
- 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
- C23C22/17—Orthophosphates containing zinc cations containing also organic acids
-
- 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
- C23C22/34—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 fluorides or complex fluorides
-
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Abstract
Description
本発明の三価クロム黒色化成皮膜処理液は、金属基材の表面に対する化成皮膜処理液であって、三価クロム化合物と、二種類以上の有機酸または有機酸塩、或いは、一種類以上の有機硫黄化合物と、硝酸イオンとを含有し、且つ、コバルト化合物を含有しない。金属基材は、特に限定されないが、亜鉛めっき又は亜鉛合金めっき材であるのが好ましい。
本発明の三価クロム含有水溶性仕上げ処理液は、亜鉛めっき又は亜鉛合金めっき材等の金属基材上に形成された、三価クロム化合物を含有しコバルト化合物を含有しない三価クロム黒色化成皮膜の表面に対する仕上げ処理液であって、三価クロム化合物と、リンの酸素酸イオンと、コバルトを除く一種類以上の遷移金属化合物と、シリコンオイル又はフッ素系から選択される一種類以上の化合物もしくは樹脂と、を含有し、且つ、コバルト化合物を含有しない。
本発明の金属基材の処理方法は、亜鉛めっき又は亜鉛合金めっき材等の金属基材を、上述の三価クロム黒色化成皮膜処理液に浸漬して金属基材表面に三価クロム黒色化成皮膜を形成した後、上述の三価クロム含有水溶性仕上げ処理液に浸漬して前記三価クロム黒色化成皮膜の表面に三価クロム含有仕上げ皮膜を形成する。このような処理方法により、コバルト化合物を含有せず、耐食性及び耐傷性に優れ、処理液の安定性が高く、環境問題等にも配慮した金属基材の皮膜処理等が可能となる。
めっきの膜厚は8〜10μm、耐食性評価はJIS Z 2371に従う塩水噴霧試験で行った。また、耐傷性評価は処理後の試験片に対しカッターナイフでX字に傷をつけたものをJIS Z 2371に従う塩水噴霧試験で行った。ここで、各条件あたり試験片数を5点もしくは10点投入して塩水噴霧試験の耐食性及び耐傷性を確認した。この際に、規定時間時の状態として「全品腐食無しなら○」「一部点数に腐食が発生なら△」「全品腐食発生なら×」と評価した。
また、各処理液の安定性については処理後に放置し沈殿の発生や濁りが無いかを確認した。当該安定性の評価基準は、「〇:沈殿も濁りも無く透明」、「△:濁りがある」、「×:沈殿がある」、「−:240時間経過時点で沈殿が発生していたため評価外」とした。
亜鉛めっきを施した鉄板(表面積1dm2)を、硝酸クロムを15g/L、有機酸としてマロン酸1g/L、クエン酸を5g/L、有機硫黄化合物としてチオグリコール酸を5g/L、及び、硝酸根が20g/Lになるように硝酸ソーダを含有し、温度30℃、pH2.0に調整した三価クロム黒色化成皮膜処理液に30秒浸漬し、軽く水洗した後にリン酸クロム(III)を20g/L、バナジン酸アンモンを1g/L、マロン酸を5g/L、及び、シリコンオイルとして東レ・ダウコーニング製DK Q1−1247を0.10g/L含有し、温度30℃、pH4.0に調整した三価クロム含有水溶性仕上げ処理液に10秒間浸漬し、水洗せずに試験片を乾燥させた後、耐食性、耐傷性および外観を評価した。さらに三価クロム黒色化成皮膜処理液を室温放置した後の安定性を評価し、その時点で再度試験を行ない、耐食性、耐傷性、外観を評価した。
実施例1のマロン酸の代わりに表1に示す有機酸を使用して実施例1と同条件で試験を行った。
実施例1のクエン酸の代わりに表2に示す有機酸を使用して実施例1と同条件で試験を行った。
実施例1の三価クロム黒色化成皮膜処理液中の硝酸クロムとマロン酸の代わりに、硝酸クロム15g/Lとマロン酸1g/L及びクエン酸 5g/Lを水に溶解し、80℃において60分反応させた加熱反応性生物を三価クロム黒色化成皮膜処理液において使用し、実施例1と同条件で試験を行った。
実施例1の三価クロム黒色化成皮膜処理液中のチオグリコール酸の代わりに表3に示す有機硫黄化合物を使用して実施例1と同条件で試験を行った。
三価クロム黒色化成皮膜処理液に表4に示す有機硫黄化合物を更に添加して実施例1と同条件で試験を行った。
三価クロム黒色化成皮膜処理液に表5に示す遷移金属化合物を更に添加して実施例1と同条件で試験を行った。
三価クロム黒色化成皮膜処理液に表6に示すリン化合物を添加して実施例1と同条件で試験を行った。
実施例1の条件を表7に示すように変化させて試験を行った。
実施例59〜62については、実施例1において、化成皮膜処理のpHをそれぞれ、pH1.5(実施例59)、pH2.0(実施例60)、pH2.5(実施例61)、pH3.0(実施例62)として実施した。
実施例63〜65については、実施例1において、化成皮膜処理の温度をそれぞれ、温度20℃(実施例63)、40℃(実施例64)、50℃(実施例65)として実施した。
実施例66〜68については、実施例1において、化成皮膜処理の処理時間をそれぞれ、20秒(実施例66)、60秒(実施例67)、90秒(実施例68)として実施した。
実施例69〜73については、実施例1の三価クロム含有水溶性仕上げ処理液のバナジン酸アンモンの代わりに表8に示す遷移金属化合物を添加して実施例1と同条件で試験を行った。
比較例1:亜鉛めっきを施した鉄板(表面積1dm2)を市販の亜鉛めっき用三価クロム黒色化成皮膜処理液(TR−184FG:製品名、日本表面化学株式会社製、三価クロム、硝酸イオン、有機酸、有機硫黄化合物及びコバルトを含む。TR−184F:80mL/L、TR−184G:50mL/L)を温度30℃、pH2.0に調整した処理液に60秒浸漬し、三価クロム化成皮膜を形成した。次に、軽く水洗した後、三価クロム含有水溶性仕上げ処理液(FT−190:製品名、日本表面化学株式会社製、コバルトを含む。FT−190:100mL/L)を温度40℃、pH無調整とした処理液に10秒浸漬後、乾燥させ、実施例と同様に、耐食性、耐傷性および外観を評価した。
比較例2として、三価クロム黒色化成皮膜処理液からマロン酸を抜いた処理液を用いた以外は実施例1と同条件で試験を行った。
比較例3として、三価クロム黒色化成皮膜処理液からクエン酸を抜いた処理液を用いた以外は実施例1と同条件で試験を行った。
比較例4として、三価クロム黒色化成皮膜処理液にコバルトを添加した処理液を用いた以外は実施例1と同条件で試験を行った。
比較例5として、三価クロム含有水溶性仕上げ処理液からバナジン酸アンモニウムを抜いた処理液を用いた以外は実施例1と同条件で試験を行った。
比較例6として、三価クロム含有水溶性仕上げ処理液からDK Q1−1247を抜いた処理液を用いた以外は実施例1と同条件で試験を行った。
Claims (8)
- 金属基材の表面に対する化成皮膜処理液であって、
三価クロム化合物と、
二種類以上の有機酸または有機酸塩、或いは、一種類以上の有機硫黄化合物と、
硝酸イオンと、
を含有し、且つ、コバルト化合物を含有しない三価クロム黒色化成皮膜処理液。 - 前記金属基材が、亜鉛めっき又は亜鉛合金めっき材である請求項1に記載の三価クロム黒色化成皮膜処理液。
- 三価クロム化合物と有機酸または有機酸塩とを含有する、若しくは、
三価クロム化合物と有機酸または有機酸塩とを50℃〜沸点未満の温度で反応させて得られる加熱反応生成物を含有する、
請求項1または2に記載の三価クロム黒色化成皮膜処理液。 - 更に、コバルトを除く一種類以上の遷移金属化合物を含有する請求項1〜3のいずれか一項に記載の三価クロム黒色化成皮膜処理液。
- 更に、一種類以上のリン化合物を含有する請求項1〜4のいずれか一項に記載の三価クロム黒色化成皮膜処理液。
- 金属基材上に形成された、三価クロム化合物を含有しコバルト化合物を含有しない三価クロム黒色化成皮膜の表面に対する仕上げ処理液であって、
三価クロム化合物と、
リンの酸素酸イオンと、
コバルトを除く一種類以上の遷移金属化合物と、
シリコンオイル又はフッ素含有化合物又はフッ素含有樹脂と、
を含有し、且つ、コバルト化合物を含有しない三価クロム含有水溶性仕上げ処理液。 - 前記金属基材が、亜鉛めっき又は亜鉛合金めっき材である請求項6に記載の三価クロム含有水溶性仕上げ処理液。
- 金属基材を請求項1〜5のいずれか一項に記載の三価クロム黒色化成皮膜処理液に浸漬して金属基材表面に三価クロム黒色化成皮膜を形成した後、請求項6または7に記載の三価クロム含有水溶性仕上げ処理液に浸漬して前記三価クロム黒色化成皮膜の表面に三価クロム含有仕上げ皮膜を形成する金属基材の処理方法。
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JP7340900B1 (ja) * | 2023-06-01 | 2023-09-08 | ユケン工業株式会社 | 3価クロム黒色化成処理用組成物および化成被膜を備える部材の製造方法 |
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US10968520B2 (en) | 2021-04-06 |
JP6532003B2 (ja) | 2019-06-19 |
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EP3045564B1 (en) | 2019-03-06 |
EP3045564A1 (en) | 2016-07-20 |
US20160208390A1 (en) | 2016-07-21 |
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