CN113439131A - 化学转化处理剂、具有化学转化皮膜的金属材料的制造方法以及具有化学转化皮膜的金属材料 - Google Patents
化学转化处理剂、具有化学转化皮膜的金属材料的制造方法以及具有化学转化皮膜的金属材料 Download PDFInfo
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- 239000004615 ingredient Substances 0.000 description 1
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- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 description 1
- AQBLLJNPHDIAPN-LNTINUHCSA-K iron(3+);(z)-4-oxopent-2-en-2-olate Chemical compound [Fe+3].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O AQBLLJNPHDIAPN-LNTINUHCSA-K 0.000 description 1
- 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 1
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- 229910000155 iron(II) phosphate Inorganic materials 0.000 description 1
- NPFOYSMITVOQOS-UHFFFAOYSA-K iron(III) citrate Chemical compound [Fe+3].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NPFOYSMITVOQOS-UHFFFAOYSA-K 0.000 description 1
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 1
- SDEKDNPYZOERBP-UHFFFAOYSA-H iron(ii) phosphate Chemical compound [Fe+2].[Fe+2].[Fe+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O SDEKDNPYZOERBP-UHFFFAOYSA-H 0.000 description 1
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- UJVRJBAUJYZFIX-UHFFFAOYSA-N nitric acid;oxozirconium Chemical compound [Zr]=O.O[N+]([O-])=O.O[N+]([O-])=O UJVRJBAUJYZFIX-UHFFFAOYSA-N 0.000 description 1
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- UWMZZSRDUVJJDP-UHFFFAOYSA-M sodium 2-[3-(2-methylanilino)-6-(2-methyl-4-sulfonatoanilino)xanthen-10-ium-9-yl]benzoate Chemical compound [Na+].Cc1ccccc1Nc1ccc2c(-c3ccccc3C([O-])=O)c3ccc(Nc4ccc(cc4C)S([O-])(=O)=O)cc3[o+]c2c1 UWMZZSRDUVJJDP-UHFFFAOYSA-M 0.000 description 1
- AZLXCBPKSXFMET-UHFFFAOYSA-M sodium 4-[(4-sulfophenyl)diazenyl]naphthalen-1-olate Chemical compound [Na+].C12=CC=CC=C2C(O)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 AZLXCBPKSXFMET-UHFFFAOYSA-M 0.000 description 1
- 239000011775 sodium fluoride Substances 0.000 description 1
- 235000013024 sodium fluoride Nutrition 0.000 description 1
- CMZUMMUJMWNLFH-UHFFFAOYSA-N sodium metavanadate Chemical compound [Na+].[O-][V](=O)=O CMZUMMUJMWNLFH-UHFFFAOYSA-N 0.000 description 1
- GTKIEPUIFBBXJQ-UHFFFAOYSA-M sodium;2-[(4-hydroxy-9,10-dioxoanthracen-1-yl)amino]-5-methylbenzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC(C)=CC=C1NC1=CC=C(O)C2=C1C(=O)C1=CC=CC=C1C2=O GTKIEPUIFBBXJQ-UHFFFAOYSA-M 0.000 description 1
- VRDAELYOGRCZQD-NFLRKZIHSA-M sodium;4-[(2z)-2-[(5e)-5-[(2,4-dimethylphenyl)hydrazinylidene]-4,6-dioxocyclohex-2-en-1-ylidene]hydrazinyl]benzenesulfonate Chemical compound [Na+].CC1=CC(C)=CC=C1N\N=C(/C(=O)C=C\1)C(=O)C/1=N\NC1=CC=C(S([O-])(=O)=O)C=C1 VRDAELYOGRCZQD-NFLRKZIHSA-M 0.000 description 1
- BFXAWOHHDUIALU-UHFFFAOYSA-M sodium;hydron;difluoride Chemical compound F.[F-].[Na+] BFXAWOHHDUIALU-UHFFFAOYSA-M 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 125000000020 sulfo group Chemical group O=S(=O)([*])O[H] 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- MPCYPRXRVWZKGF-UHFFFAOYSA-J tetrasodium 5-amino-3-[[4-[4-[(8-amino-1-hydroxy-3,6-disulfonatonaphthalen-2-yl)diazenyl]phenyl]phenyl]diazenyl]-4-hydroxynaphthalene-2,7-disulfonate Chemical compound [Na+].[Na+].[Na+].[Na+].C1=C(S([O-])(=O)=O)C=C2C=C(S([O-])(=O)=O)C(N=NC3=CC=C(C=C3)C3=CC=C(C=C3)N=NC3=C(C=C4C=C(C=C(C4=C3O)N)S([O-])(=O)=O)S([O-])(=O)=O)=C(O)C2=C1N MPCYPRXRVWZKGF-UHFFFAOYSA-J 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 229910000349 titanium oxysulfate Inorganic materials 0.000 description 1
- 229910000348 titanium sulfate Inorganic materials 0.000 description 1
- FKVXIGHJGBQFIH-UHFFFAOYSA-K trisodium 5-amino-3-[[4-[4-[(7-amino-1-hydroxy-3-sulfonatonaphthalen-2-yl)diazenyl]phenyl]phenyl]diazenyl]-4-hydroxynaphthalene-2,7-disulfonate Chemical compound C1=CC(=CC=C1C2=CC=C(C=C2)N=NC3=C(C=C4C=CC(=CC4=C3[O-])N)S(=O)(=O)O)N=NC5=C(C6=C(C=C(C=C6C=C5S(=O)(=O)O)S(=O)(=O)[O-])N)[O-].[Na+].[Na+].[Na+] FKVXIGHJGBQFIH-UHFFFAOYSA-K 0.000 description 1
- SWGJCIMEBVHMTA-UHFFFAOYSA-K trisodium;6-oxido-4-sulfo-5-[(4-sulfonatonaphthalen-1-yl)diazenyl]naphthalene-2-sulfonate Chemical compound [Na+].[Na+].[Na+].C1=CC=C2C(N=NC3=C4C(=CC(=CC4=CC=C3O)S([O-])(=O)=O)S([O-])(=O)=O)=CC=C(S([O-])(=O)=O)C2=C1 SWGJCIMEBVHMTA-UHFFFAOYSA-K 0.000 description 1
- YXZRCLVVNRLPTP-UHFFFAOYSA-J turquoise blue Chemical compound [Na+].[Na+].[Na+].[Na+].[Cu+2].NC1=NC(Cl)=NC(NC=2C=C(NS(=O)(=O)C3=CC=4C(=C5NC=4NC=4[N-]C(=C6C=CC(=CC6=4)S([O-])(=O)=O)NC=4NC(=C6C=C(C=CC6=4)S([O-])(=O)=O)NC=4[N-]C(=C6C=CC(=CC6=4)S([O-])(=O)=O)N5)C=C3)C(=CC=2)S([O-])(=O)=O)=N1 YXZRCLVVNRLPTP-UHFFFAOYSA-J 0.000 description 1
- IBYSTTGVDIFUAY-UHFFFAOYSA-N vanadium monoxide Chemical compound [V]=O IBYSTTGVDIFUAY-UHFFFAOYSA-N 0.000 description 1
- 239000012002 vanadium phosphate Substances 0.000 description 1
- 125000005287 vanadyl group Chemical group 0.000 description 1
- UUUGYDOQQLOJQA-UHFFFAOYSA-L vanadyl sulfate Chemical compound [V+2]=O.[O-]S([O-])(=O)=O UUUGYDOQQLOJQA-UHFFFAOYSA-L 0.000 description 1
- 229910000352 vanadyl sulfate Inorganic materials 0.000 description 1
- 229940041260 vanadyl sulfate Drugs 0.000 description 1
- PEAGNRWWSMMRPZ-UHFFFAOYSA-L woodstain scarlet Chemical compound [Na+].[Na+].OC1=CC=C2C=C(S([O-])(=O)=O)C=C(S([O-])(=O)=O)C2=C1N=NC(C=C1)=CC=C1N=NC1=CC=CC=C1 PEAGNRWWSMMRPZ-UHFFFAOYSA-L 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
- XJUNLJFOHNHSAR-UHFFFAOYSA-J zirconium(4+);dicarbonate Chemical compound [Zr+4].[O-]C([O-])=O.[O-]C([O-])=O XJUNLJFOHNHSAR-UHFFFAOYSA-J 0.000 description 1
Classifications
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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
- C23C22/34—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
-
- 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
- C23C22/40—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 molybdates, tungstates or vanadates
- C23C22/44—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 molybdates, tungstates or vanadates containing also fluorides or complex fluorides
-
- 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
- C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Treatment Of Metals (AREA)
Abstract
本发明的目的在于提供能够在金属材料的表面或表面上形成耐腐蚀性优异的、着色的化学转化皮膜的化学转化处理剂等。本发明通过含有离子(A)、离子(B)、包含氟的离子(C)及酸性染料(D)的、上述离子(C)的摩尔浓度相对于上述离子(A)的摩尔浓度为6倍以上的化学转化处理剂实现了上述目的,上述离子(A)包含选自锆、钛及铪中的金属元素,上述离子(B)包含选自铬、铁、钴、钒及铜中的金属元素。
Description
技术领域
本发明涉及在金属材料的表面或表面上制造化学转化皮膜的化学转化处理剂、使用了该化学转化处理剂的具有化学转化皮膜的金属材料的制造方法、通过该制造方法制造的具有化学转化皮膜的金属材料。
背景技术
一直以来,进行着能够形成耐腐蚀性优异的化学转化皮膜的化学转化处理剂的开发。例如,专利文献1中公开了一种包含液体组合物的处理液,上述液体组合物含有(A)三价铬、(B)锆离子、(C)选自氯离子、硫酸根离子及硝酸根离子中的一种以上、(D)芳香族砜以及(E)氟离子。
现有技术文献
专利文献
专利文献1:日本特开2015-38255号公报。
发明内容
发明要解决的问题
本发明的目的在于提供能够在金属材料的表面或表面上形成耐腐蚀性优异、着色的化学转化皮膜的化学转化处理剂等。
用于解决问题的方案
本发明人为了解决上述问题而进行了深入研究,结果发现,含有离子(A)、离子(B)、包含氟的离子(C)及酸性染料(D)的、上述离子(C)的摩尔浓度相对于上述离子(A)的摩尔浓度为6倍以上的化学转化处理剂能够形成耐腐蚀性优异、着色的化学转化皮膜,上述离子(A)包含选自锆、钛及铪中的金属元素,上述离子(B)包含选自铬、铁、钴、钒及铜中的金属元素,以至完成了本发明。
本发明包含以下内容。
[1]一种化学转化处理剂,其含有离子(A)、离子(B)、包含氟的离子(C)及酸性染料(D),上述离子(A)包含选自锆、钛及铪中的金属元素,上述离子(B)包含选自铬、铁、钴、钒及铜中的金属元素,上述离子(C)的摩尔浓度相对于上述离子(A)的摩尔浓度为6倍以上。
[2]一种具有化学转化皮膜的金属材料的制造方法,其包括使上述[1]所述的化学转化处理剂接触金属材料的表面或表面上的工序。
[3]一种具有化学转化皮膜的金属材料,其是通过上述[2]所述的制造方法得到的。
发明效果
根据本发明,能够提供一种化学转化处理剂,其能够在金属材料的表面或表面上形成耐腐蚀性优异、着色的化学转化皮膜。此外,根据本发明还能够提供使用该化学转化处理剂在金属材料的表面或表面上形成化学转化皮膜来制造具有化学转化皮膜的金属材料的方法、通过该制造方法制造的具有化学转化皮膜的金属材料。
具体实施方式
本发明的实施方式的化学转化处理剂含有离子(A)、离子(B)、包含氟的离子(C)及酸性染料(D),上述离子(A)包含选自锆、钛及铪中的金属元素,上述离子(B)包含选自铬、铁、钴、钒及铜中的金属元素,上述离子(C)的摩尔浓度相对于上述离子(A)的摩尔浓度为6倍以上。通过使用这样的化学转化处理剂,能够在金属材料的表面或表面上制造耐腐蚀性优异、着色的化学转化皮膜。另外,本实施方式的化学转化处理剂可以是在水性介质中仅配合了离子(A)的供给源、离子(B)的供给源、离子(C)的供给源、酸性染料(D)的化学转化处理剂,也可以是进一步配合了其它成分而成的化学转化处理剂。本实施方式的化学转化处理剂可以包含含磷化合物,也可以不包含含磷化合物。
<离子(A)>
本实施方式的化学转化处理剂含有包含选自锆、钛及铪中的金属元素的离子(A)(以下也仅称为离子(A))。作为离子(A),能够举出例如:锆、钛或铪的金属离子;包含锆、钛或铪的络合物离子;锆、钛或铪的氧化物离子等。化学转化处理剂中可以包含这些离子中的一种或两种以上。
化学转化处理剂中的离子(A)的浓度没有特别限制,作为金属换算质量浓度(在包含两种以上的离子(A)的情况下,意为合计金属换算质量浓度。),通常为5mg/L以上,优选为20mg/L以上,此外,通常为2000mg/L以下,优选为1000mg/L以下。
作为离子(A)的供给源,只要是在混合到水性介质中时能够提供离子(A)的化合物,则没有特别限制。可举出例如六氟锆酸、硫酸锆、硫酸氧锆、硫酸锆铵、硝酸锆、硝酸氧锆、硝酸锆铵、乙酸氧锆、乳酸氧锆、四乙酰丙酮锆、三丁氧基乙酰丙酮锆、四正丙氧基锆、硝酸氧锆、碳酸锆、氢氧化锆、氧化锆、六氟钛酸、硝酸钛、硝酸氧钛、硝酸钛铵、硝酸氧钛、硫酸钛、硫酸氧钛、硫酸钛铵、氢氧化钛、氧化钛、氟化钛铵、六氟铪酸、硝酸铪、氧化铪等。在它们可以采取盐的形态的情况下,也可以是其盐。另外,这些供给源可以仅使用一种,也可以并用两种以上。
<酸性染料(D)>
本实施方式的化学转化处理剂含有酸性染料(D)。本说明书中的“酸性染料”意为具有酸性基团的水溶性染料和该酸性基能够反应构成盐的水溶性染料。作为该酸性基团,可举出例如磺基、羧基、酚性羟基、磷酸基等。酸性染料可以使用具有一种或两种以上的酸性基团的酸性染料。此外,作为盐,例如可举出:碱金属盐;碱土金属盐;铵盐;与铝、锡、铬、铜、钴、镍、铁等金属元素形成的盐等。另外,上述“水溶性染料”意为在20℃、100g的水中溶解0.01g以上的染料。此外,优选在20℃、100g的水中溶解0.02g以上的染料,更优选溶解0.2g以上的染料。酸性染料可以在水性介质中以任意形态溶解,例如可以为未离子化的形态、也可以为一部分或全部的官能团离子化的形态、也可以为络合物离子化的形态、也可以为其它形态。化学转化处理剂中可以包含这些酸性染料的一种或两种以上。
通过在化学转化处理剂中配合酸性染料(D),能够在金属材料的表面或表面上形成着色的化学转化皮膜。此外,该化学转化皮膜与利用不包含酸性染料(D)的化学转化处理剂形成的化学转化皮膜相比,具有优异的耐腐蚀性。
化学转化处理剂中的酸性染料(D)的配合量(浓度)没有特别限制,通常为200mg/L以上,此外,通常为30000mg/L以下,优选为10000mg/L以下,更优选为2000mg以下。
作为酸性染料(D),只要是公知的酸性染料,则没有特别限制。可举出例如偶氮酸性染料、三芳基甲烷酸性染料、靛青酸性染料、蒽醌酸性染料、呫吨酸性染料、喹啉酸性染料、硝基酸性染料、花青酸性染料等。这些能够使用一种或组合使用两种以上,在并用两种以上的情况下,能够任意地组合。作为酸性染料(D)的具体例子,可举出染料索引名为食品红1、食品红6、酸性红1、酸性红2、酸性红9、酸性红13、酸性红18、酸性红26、酸性红27、酸性红29、酸性红33、酸性红51、酸性红52、酸性红60、酸性红73、酸性红87、酸性红88、酸性红91、酸性红92、酸性红94、酸性红95、酸性红112、酸性红114、酸性红289、酸性紫9、酸性紫43、酸性橙7、酸性橙20、酸性橙24、酸性黄1、酸性黄3、酸性黄11、酸性黄23、酸性黄36、酸性黄40、酸性黄73、食品黄3、食品绿、酸性绿25、酸性绿5、酸性绿1、酸性绿3、食品蓝2、酸性蓝3、酸性蓝5、酸性蓝9、酸性蓝74、直接蓝1、直接蓝2、直接蓝6、直接蓝14、活性蓝21、酸性黑1等。
<离子(B)>
本实施方式的化学转化处理剂含有包含选自铬、铁、钴、钒及铜中的金属元素的离子(B)(以下也仅称为离子(B))。作为离子(B),可举出例如:铬、铁、钴、钒或铜的金属离子;包含铬、铁、钴、钒或铜的络合物离子;钒的氧化物离子等。化学转化处理剂中可以包含这些离子中的一种或两种以上。
化学转化处理剂中的离子(B)的浓度没有特别限制,作为金属换算质量浓度(在包含两种以上的离子(B)的情况下,意为合计金属换算质量浓度),通常为5mg/L以上,优选为20mg/L以上,此外,通常为2000mg/L以下,优选为1000mg/L以下。
作为离子(B)的供给源,只要是在混合到水性介质中时,能够提供离子(B)的化合物,则没有特别限制。可举出例如:氟化铬(III)、磷酸铬(III)、硝酸铬(III)、硫酸铬(III)、氯化铬(III)、乙酸铬(III)、草酸铬(III)、琥珀酸铬(III);氟化亚铁(II)、氟化铁(III)、氢氧化亚铁(II)、氢氧化铁(III)、硝酸亚铁(II)、硝酸铁(III)、乙酰丙酮铁(III)、氯化亚铁(II)、氯化铁(III)、柠檬酸铁(III)、氧化亚铁(II)、氧化铁(III)、六氰合亚铁(II)、六氰合铁(III)、六氰合亚铁(II)酸、六氰合铁(III)酸钾、硫酸亚铁(II)铵、硫酸铁(III)铵、磷酸亚铁(II);氟化钴、硫酸钴、硝酸钴、乙酸钴、碳酸钴、磷酸钴、氯化钴;氧化钒(II)、氧化钒(IV)、氧化钒(V)、偏钒酸钠、偏钒酸钾、偏钒酸铵、双乙酰丙酮钒、二乙酰丙酮氧钒、氟化钒、磷酸钒、硫酸氧钒、硫化钒、草酸氧钒、三异丙氧基氧化钒、三丁氧基氧化钒、三乙氧基氧化钒、三异丁氧基氧化钒、三乙醇胺氧化钒、柠檬酸氧化钒铵、硬脂酸三丁氧基钒、乙酰丙酮氧钒、四丙氧基钒、四丁氧基钒;硝酸铜、硫酸铜、氯化铜、氧化铜、氟化铜等。在它们能够采取盐的形态的情况下,也可以是其盐。另外,这些供给源可以仅使用一种,也可以并用两种以上。其中,离子(B)的供给源是与酸性染料(D)不同的化合物。
<包含氟的离子(C)>
本实施方式的化学转化处理剂含有包含氟的离子(C)(以下也仅称为离子(C))。作为离子(C),可举出例如:氟化物离子;与化学转化处理剂中存在的金属离子键合或配位的离子等。化学转化处理剂中可以包含这些离子中的一种或两种以上。
关于化学转化处理剂中的离子(C)的浓度,以氟换算摩尔浓度计,只要为锆、钛及铪的合计金属换算摩尔浓度的6倍以上即可,上限值优选为200倍以下。
作为离子(C)的供给源,只要是在混合到水性介质中时,能够提供离子(C)的化合物,则没有特别限制。可举出例如:氢氟酸、氟化铵、氟化氢铵、氟化锗、氟化铝、氟化钾、氟化氢钾、氟化钠、氟化氢钠等含氟化合物。此外,可以仅由六氟锆酸、六氟钛酸、六氟铪酸等离子(A)的供给源(也属于含氟化合物)供给,也可以仅由氟化铬(III)、氟化亚铁(II)、氟化铁(III)、氟化钴、氟化钒、氟化铜等离子(B)的供给源(也属于含氟化合物)供给,可以通过离子(A)的供给源和离子(B)的供给源供给,也可以通过除了离子(A)的供给源和离子(B)的供给源以外的含氟化合物供给,也可以通过配合离子(A)的供给源和/或离子(B)的供给源与除它们以外的含氟化合物供给。另外,在使用六氟锆酸、六氟钛酸、六氟铪酸等含有锆、钛或铪、和氟的化合物制备化学转化处理剂的情况下,能够供给离子(A)和离子(C)。此外,在使用氟化铬(III)、氟化亚铁(II)、氟化铁(III)、氟化钴、氟化钒、氟化铜等含有铬、铁、钴、钒、或铜、和氟的化合物制备化学转化处理剂的情况下,能够供给离子(B)和离子(C)。另外,各种含氟化合物可以仅使用一种,也可以并用两种以上。
<水性介质>
作为水性介质,只要是水或水与水混溶性有机溶剂的混合物(以水性介质的体积为基准,含有50体积%以上的水的混合物),则没有特别限制。作为水混溶性有机溶剂,只要是与水混溶的有机溶剂,则没有特别限制,可举出例如:丙酮、甲乙酮等酮系溶剂;N,N’-二甲基甲酰胺、二甲基乙酰胺等酰胺系溶剂;甲醇、乙醇、异丙醇等醇系溶剂;乙二醇单丁基醚、乙二醇单己基醚等醚系溶剂;1-甲基-2-吡咯烷酮、1-乙基-2-吡咯烷酮等吡咯烷酮系溶剂等。这些水混溶性有机溶剂可以一种与水混合,也可以两种以上与水混合。
<其它成分>
作为其它成分,可举出例如:含有选自铝、镁及锌中的金属的离子的供给源(E)、硝酸离子的供给源(F)、调节被处理物的润湿性的表面活性剂、被称作消泡剂的表面活性剂等添加剂、pH调节剂等用于化学转化处理剂的公知的添加剂;丙烯酸系树脂、聚酯系树脂、环氧系树脂、聚烯烃系树脂、酚醛系树脂、聚乙烯基系树脂、聚氨酯系树脂、聚酰亚胺系树脂、聚酰胺系树脂等公知的水溶性树脂、水分散性树脂等,但并不限定于此。另外,可以在不损害本发明的效果的范围包含这些其它成分。
<化学转化处理剂的pH>
本实施方式的化学转化处理剂的pH没有特别限制,通常处于酸性~中性的区域,具体而言,pH优选处于1.0~7.0的范围内,更优选处于1.5~6.0的范围内,特别优选处于2.0~5.5的范围内。在此,本说明书中的化学转化处理剂的pH值意为使用pH计在50℃测定的值。
化学转化处理剂的pH可以使用例如:盐酸、硫酸、硝酸、氢氟酸、硼酸、有机酸等酸成分;氢氧化锂、氢氧化钾、氢氧化钠、氢氧化钙、氢氧化镁、氢氧化钡、碱金属盐、氨、铵盐、胺类等碱成分等的pH调节剂进行调节,但并不限定于这些成分。另外,pH调节剂可以使用一种或两种以上。
<化学转化处理剂的制造方法>
本实施方式的化学转化处理剂能够通过将离子(A)的供给源、离子(B)的供给源、离子(C)的供给源及酸性染料(D)作为原料在水性介质中配合规定量来制造。通过将上述各原料例如按照上述顺序配合在水性介质中,能够制造本实施方式的化学转化处理剂。另外,在配合其它成分的情况下,例如能够将上述各原料配合到水性介质,然后配合其它成分来制造。
<化学转化皮膜的制造方法>
本实施方式的化学转化皮膜的制造方法包括使本实施方式的化学转化处理剂接触金属材料的表面或表面上的接触工序。由此在金属材料的表面或表面上形成化学转化皮膜。作为化学转化处理剂与金属材料的接触方法,可举出现有的接触方法,例如,浸渍处理法、或者喷雾处理法、冲洗处理法等处理法、或这些的组合等方法,但并不限定于此。
上述接触工序优选在规定的温度范围内进行一定时间。接触温度优选处于10℃以上且90℃以下的范围内,更优选处于20℃以上且85℃以下的范围内,但并不限于这些温度范围内。此外,接触时间优选处于20~700秒的范围内,更优选处于30~600秒的范围内,但并不限于这些时间内。
此外,可以在接触工序前进行前处理工序。作为前处理工序,可以举出例如:酸洗工序;脱脂工序;碱清洗工序;铬酸盐化学转化处理;使用磷酸锌、磷酸铁等磷酸盐的磷酸盐化学转化处理工序;铋置换镀覆工序、锆化学转化处理工序、钛化学转化处理工序、铪化学转化处理工序、钒化学转化处理工序等。这些之中优选至少进行脱脂工序。另外,这些前处理工序可以进行一个工序,也可以组合两个以上的工序依次进行。作为两个以上的工序的组合,能够举出磷酸盐化学转化处理工序、与铬酸盐化学转化处理、铋置换镀覆工序、锆化学转化处理工序、钛化学转化处理工序、铪化学转化处理工序或钒化学转化处理工序的组合。作为前处理工序实施的锆化学转化处理工序可以使用本实施方式的化学转化处理剂,也可以使用与本实施方式的化学转化处理剂不同的化学转化处理剂。另外,在进行上述各种前处理工序的情况下,可以在各种前处理工序后进行水洗处理工序。在进行多种各种前处理工序的情况下,可以在各工序后、或者在一部分工序后进行水洗处理工序。此外,在进行水洗处理工序的情况下,可以在其后进行使金属材料的表面干燥的干燥工序。
此外,在本实施方式的化学转化皮膜的制造方法中,在接触工序之后,可以进行例如碱清洗工序、水洗工序、铬酸盐化学转化处理、磷酸锌化学转化处理工序、铋置换镀覆工序、磷铁化学转化处理工序、锆化学转化处理工序、钛化学转化处理工序、铪化学转化处理工序、干燥工序等后处理工序。作为这些后处理工序,可以单独进行一个工序,也可以组合两个以上的工序依次进行。作为后处理工序实施的锆化学转化处理工序可以使用本实施方式的化学转化处理剂,也可以使用与本实施方式的化学转化处理剂不同的化学转化处理剂。另外,在进行上述各种后处理工序的情况下,可以在各种后处理工序后进行水洗处理工序。在进行多种各种后处理工序的情况下,可以在各工序后、或者在一部分工序后进行水洗处理工序。此外,在进行水洗处理工序的情况下,可以在其后进行使金属材料的表面干燥的干燥工序。干燥工序通常在50~180℃、优选在80~150℃下进行,通常进行5~20分钟,优选进行10~15分钟。
作为金属材料,可举出例如:钢铁材料(例如,冷轧钢板、热轧钢板、高张力钢板、工具钢、合金工具钢、球状石墨铸铁、灰铸铁等);镀覆材料、例如镀锌材料(例如,电镀锌、熔融镀锌等)、镀锌合金材料(例如,合金化熔融镀锌、镀Zn-Al合金、镀Zn-Al-Mg合金、电镀锌合金等)、镀铝材料等;铝材料或铝合金材料(例如,1000系、2000系、3000系、4000系、5000系、6000系、7000系、铝铸件、铝合金铸件、压铸材料等);镁材料或镁合金材料;锌材料或锌合金材料;铜材料或铜合金材料;铬材料或铬合金材料;镍材料或镍合金材料;锡材料或锡合金材料等。
本实施方式的具有化学转化皮膜的金属材料是在金属材料的表面或表面上接触本实施方式的化学转化处理剂,在金属材料的表面或表面上制造化学转化皮膜而得到的。制造的化学转化皮膜中,该化学转化皮膜所含有的锆、钛、铪、铬、铁、钴、钒及铜的每单位面积的全部合计质量优选为5mg/m2以上,更优选为10mg/m2以上,特别优选为20mg/m2以上。另外,作为上限值,没有特别限制,优选为200mg/m2以下。另外,该化学转化皮膜中的锆、钛、铪、铬、铁、钴、钒及铜的质量能够通过使用例如荧光X射线分析装置来测定。
制造的化学转化皮膜中,该化学转化皮膜所含有的酸性染料的每单位面积的合计碳换算质量(以下也仅称染料附着量)优选为10mg/m2以上,更优选为20mg/m2以上,特别优选为50mg/m2以上。另外,作为上限值,没有特别限制,优选为200mg/m2以下。另外,该化学转化皮膜中的酸性染料的质量能够通过使用例如TOC(总有机碳分析仪)来测定。
本实施方式的具有化学转化皮膜的金属材料在通过接触本实施方式的化学转化处理剂得到的化学转化皮膜之上或之下可以具有一个或两个以上的上述各种皮膜(例如,铬酸盐化学转化皮膜、磷酸盐化学转化皮膜、铋置换镀覆皮膜等)。
通过在本实施方式的具有化学转化皮膜的金属材料的表面上使用涂料进行涂装来形成涂膜,从而能够制造具有化学转化皮膜和涂膜的涂装金属材料。作为涂料,没有特别限制,可以使用有色的涂料,为了不改变由酸性染料(D)赋予的颜色,也可以使用透明的涂料。作为涂装方法,没有特别限制,能够应用辊涂法、流动浸渍涂装法、静电粉末涂装法、电沉积涂装法、溶剂涂装法等公知方法。此外,也可以通过干式层压法、挤出层压法等来粘贴层压膜。涂装金属材料可以在本实施方式的具有化学转化皮膜的金属材料的表面上具有涂膜,也可以在该化学转化皮膜上进一步形成的一个或两个以上的上述各种皮膜(例如,铬酸盐化学转化皮膜、磷酸盐化学转化皮膜、铋置换镀覆皮膜、钒化学转化皮膜等)的表面上具有涂膜。另外,涂膜可以由1层构成,也可以由2层以上构成。涂膜的厚度没有特别限制,可根据涂装金属材料的使用用途适当设定。
实施例
以下通过实施例详细说明本发明的效果,但本发明并不受以下的实施例限制。
<金属材料>
作为金属材料,将JIS H 4000:2014中规定的铝板(A1050:厚度:0.8mm)、JIS G3302:2010中规定的熔融镀锌钢板(GI:厚度:0.6mm、镀覆附着量:单面50g/m2)、JIS G3321:2012中规定的熔融镀铝-锌钢板(GL:厚度:0.4mm、镀覆附着量:单面75g/m2)、JISG3313:2010中规定的电镀锌钢板(EG:厚度0.8mm、镀覆附着量:单面45g/m2)分别切断为长150mm×宽70mm的尺寸。
<用于化学转化处理剂的制备的各成分>
在化学转化处理剂的制备中,作为离子(A)的供给源,使用A1:六氟锆酸(森田化学工业株式会社)、A2:硫酸锆(日本轻金属株式会社)、或A3:氟化钛铵(森田化学工业株式会社);作为离子(B)的供给源,使用B1:硝酸铬(日本化学工业株式会社)、B2:硫酸铬(日本化学工业株式会社)、B3:硝酸铁(富士胶片和光纯药株式会社)、B4:硫酸铜(富士胶片和光纯药株式会社);作为离子(C)的供给源,使用C1:氢氟酸(森田化学工业株式会社)、C2:氟化铝(森田化学工业株式会社);作为染料(D),使用D1:食品黄No.5(东京化成工业株式会社;食品黄3)、D2:酸性黄23(东京化成工业株式会社)、D3:酸性红27(东京化成工业株式会社)、D4:酸性蓝74(东京化成工业株式会社)、D5:酸性蓝9(东京化成工业株式会社)、D6:活性翠蓝G(N)(住友化学株式会社;活性蓝21)的酸性染料、D7:碱性蓝9(富士胶片和光纯药株式会社)、D8:碱性紫10(富士胶片和光纯药株式会社)、D9:碱性紫3(富士胶片和光纯药株式会社)的碱性染料。另外,上述A1和A3也用作离子(C)的供给源。
<化学转化处理剂的制备>
如表1所示,将规定量的各成分在水中配合,然后用氨调节至规定的pH来制备实施例1~21和比较例1~8的化学转化处理剂。
<具有化学转化皮膜的金属材料的制造>
将各种金属材料(A1050、GI、GL及EG)在调节至50℃的脱脂剂(FC-4424;日本帕卡濑精株式会社;使用在水中溶解成20g/L的浓度的水溶液)中浸渍120秒来进行脱脂。其后,进行30秒喷雾水洗。接着,在表1所示条件下在各种化学转化处理剂(实施例1~21和比较例1~8的化学转化处理剂)中浸渍金属材料,在金属材料的表面或表面上制造化学转化皮膜。得到的具有化学转化皮膜的金属材料的表面上依次用自来水、去离子水进行清洗,在150℃下干燥10分钟,得到试验板。
[表1]
<性能评价>
使用制作的试验板进行以下性能评价。结果示于表2。
(1)附着量
对于制作的试验板的化学转化皮膜的附着量(全部金属合计附着量),使用Rigaku株式会社制造的扫描型荧光X射线分析装置ZSX primusII测定化学转化皮膜所包含的锆、钛、铬、铁及铜的全部合计质量。此外,使用岛津制作所株式会社制造的总有机碳分析仪TOC-LCSH测定的总有机碳量换算求出染料附着量。
(2)着色性
目视判定制作的试验板的着色。
<判定基准>
Y···观察到着色。
N···未观察到着色。
(3)耐腐蚀性
各试验板的耐腐蚀性按照JIS Z 2371:2015进行中性盐水喷雾试验,对具有化学转化皮膜的评价面,测定产生的锈面积达到10%为止的时间。另外,具有化学转化皮膜的评价面中的锈面积是测定目视确认锈处的合计面积。
(4)耐酸性
将各试验板在pH调节至2的硝酸水溶液(25℃)中浸渍5分钟,目视化学转化皮膜是否掉色,按照以下评价基准评价耐酸性(硝酸水溶液)。
<评价基准>
Y···不掉色
N···掉色
此外,将使用实施例4或15的化学转化处理剂如上所述形成化学转化皮膜的各试验板在5%或者10%的乙酸水溶液、或5%或者10%的柠檬酸水溶液(各25℃)中浸渍5分钟,目视观察化学转化皮膜是否掉色,按照同样的评价基准进行评价。其结果表明,在任一种水溶液中都没有掉色。另外,使用乙酸和柠檬酸的耐酸性评价结果未示于表2。
(5)耐碱性
将各试验板在pH调节至12的氢氧化钠水溶液(25℃)中浸渍5分钟,目视观察化学转化皮膜是否掉色来进行评价。
<评价基准>
Y···不掉色
N···掉色
[表2]
如表2所示,在使用实施例(实施例1~21)的化学转化处理剂的情况下,与使用比较例(比较例1~8)的化学转化处理剂的情况相比,能够在金属材料的表面或表面上形成具有更优异的耐腐蚀性的、着色的化学转化皮膜。此外,该化学转化皮膜的耐酸性和耐碱性优异。进而,在使用本实施方式的化学转化处理剂的情况下,化学转化皮膜的色调(形成化学转化皮膜前的金属材料的色调与形成化学转化皮膜后的金属材料的色调之差:色差)与该化学转化皮膜的附着量显示相关性。即,通过目视确认化学转化皮膜的色调,能够管理该化学转化皮膜的附着量。此外,能够在金属材料的表面或表面上形成没有颜色不均、附着量均匀的化学转化皮膜。
另外,虽然参照具体的实施例对本发明进行了详细地说明,但对本领域的技术人员来说,能够在不脱离本发明的宗旨和范围内实施各种变更、改变是显而易见的。
Claims (3)
1.一种化学转化处理剂,其含有离子(A)、离子(B)、包含氟的离子(C)及酸性染料(D),
所述离子(A)包含选自锆、钛及铪中的金属元素,所述离子(B)包含选自铬、铁、钴、钒及铜中的金属元素,
所述离子(C)的摩尔浓度相对于所述离子(A)的摩尔浓度为6倍以上。
2.一种具有化学转化皮膜的金属材料的制造方法,其包括使权利要求1所述的化学转化处理剂接触金属材料的表面或表面上的工序。
3.一种具有化学转化皮膜的金属材料,其是通过权利要求2所述的制造方法得到的。
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WO2018123842A1 (ja) * | 2016-12-28 | 2018-07-05 | 日本パーカライジング株式会社 | 化成処理剤、化成皮膜の製造方法、化成皮膜付き金属材料、及び塗装金属材料 |
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CN104145046A (zh) * | 2012-03-09 | 2014-11-12 | 日本油漆株式会社 | 化学转化处理剂及化学转化处理皮膜 |
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