CN114703456A - 一种铝及铝合金表面的新型耐腐蚀性超疏水涂层及其制备方法 - Google Patents
一种铝及铝合金表面的新型耐腐蚀性超疏水涂层及其制备方法 Download PDFInfo
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- CN114703456A CN114703456A CN202210348837.XA CN202210348837A CN114703456A CN 114703456 A CN114703456 A CN 114703456A CN 202210348837 A CN202210348837 A CN 202210348837A CN 114703456 A CN114703456 A CN 114703456A
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- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 95
- 238000000576 coating method Methods 0.000 title claims abstract description 69
- 239000011248 coating agent Substances 0.000 title claims abstract description 66
- 238000005260 corrosion Methods 0.000 title claims abstract description 65
- 230000007797 corrosion Effects 0.000 title claims abstract description 65
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 62
- 230000003075 superhydrophobic effect Effects 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 29
- 239000000126 substance Substances 0.000 claims abstract description 29
- 238000011065 in-situ storage Methods 0.000 claims abstract description 17
- 238000004140 cleaning Methods 0.000 claims abstract description 15
- 230000008569 process Effects 0.000 claims abstract description 11
- 239000002270 dispersing agent Substances 0.000 claims abstract description 9
- 238000003618 dip coating Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 44
- 238000006243 chemical reaction Methods 0.000 claims description 30
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- 238000005507 spraying Methods 0.000 claims description 23
- 238000005406 washing Methods 0.000 claims description 21
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 13
- 229910017604 nitric acid Inorganic materials 0.000 claims description 13
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- 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 claims description 10
- 238000002791 soaking Methods 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 8
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 8
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 7
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 7
- 238000000889 atomisation Methods 0.000 claims description 7
- 150000001844 chromium Chemical class 0.000 claims description 7
- 230000003749 cleanliness Effects 0.000 claims description 7
- 150000001879 copper Chemical class 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 238000005516 engineering process Methods 0.000 claims description 7
- 150000002815 nickel Chemical class 0.000 claims description 7
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 7
- 230000002378 acidificating effect Effects 0.000 claims description 6
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 6
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 6
- 239000003607 modifier Substances 0.000 claims description 6
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 5
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 4
- JXSRRBVHLUJJFC-UHFFFAOYSA-N 7-amino-2-methylsulfanyl-[1,2,4]triazolo[1,5-a]pyrimidine-6-carbonitrile Chemical compound N1=CC(C#N)=C(N)N2N=C(SC)N=C21 JXSRRBVHLUJJFC-UHFFFAOYSA-N 0.000 claims description 4
- 229910021555 Chromium Chloride Inorganic materials 0.000 claims description 4
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 4
- QSWDMMVNRMROPK-UHFFFAOYSA-K chromium(3+) trichloride Chemical compound [Cl-].[Cl-].[Cl-].[Cr+3] QSWDMMVNRMROPK-UHFFFAOYSA-K 0.000 claims description 4
- 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 claims description 4
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 4
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 4
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 4
- WKWOFMSUGVVZIV-UHFFFAOYSA-N n-bis(ethenyl)silyl-n-trimethylsilylmethanamine Chemical compound C[Si](C)(C)N(C)[SiH](C=C)C=C WKWOFMSUGVVZIV-UHFFFAOYSA-N 0.000 claims description 4
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 4
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 4
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 4
- 229920002401 polyacrylamide Polymers 0.000 claims description 4
- 239000000276 potassium ferrocyanide Substances 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 claims description 4
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 4
- 239000011775 sodium fluoride Substances 0.000 claims description 4
- 235000013024 sodium fluoride Nutrition 0.000 claims description 4
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 4
- 229940048086 sodium pyrophosphate Drugs 0.000 claims description 4
- XOGGUFAVLNCTRS-UHFFFAOYSA-N tetrapotassium;iron(2+);hexacyanide Chemical compound [K+].[K+].[K+].[K+].[Fe+2].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] XOGGUFAVLNCTRS-UHFFFAOYSA-N 0.000 claims description 4
- 235000019818 tetrasodium diphosphate Nutrition 0.000 claims description 4
- NESLVXDUKMNMOG-UHFFFAOYSA-N triethoxy-(propyltetrasulfanyl)silane Chemical compound CCCSSSS[Si](OCC)(OCC)OCC NESLVXDUKMNMOG-UHFFFAOYSA-N 0.000 claims description 4
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 3
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 3
- PMQIWLWDLURJOE-UHFFFAOYSA-N triethoxy(1,1,2,2,3,3,4,4,5,5,6,6,7,7,10,10,10-heptadecafluorodecyl)silane Chemical compound CCO[Si](OCC)(OCC)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)CCC(F)(F)F PMQIWLWDLURJOE-UHFFFAOYSA-N 0.000 claims description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract description 8
- 230000002209 hydrophobic effect Effects 0.000 abstract description 6
- 229910052759 nickel Inorganic materials 0.000 abstract description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 abstract description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052804 chromium Inorganic materials 0.000 abstract description 3
- 239000011651 chromium Substances 0.000 abstract description 3
- 229910052802 copper Inorganic materials 0.000 abstract description 3
- 239000010949 copper Substances 0.000 abstract description 3
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- 238000004381 surface treatment Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- UMRSVAKGZBVPKD-UHFFFAOYSA-N acetic acid;copper Chemical compound [Cu].CC(O)=O UMRSVAKGZBVPKD-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
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- 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
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- XPBBUZJBQWWFFJ-UHFFFAOYSA-N fluorosilane Chemical compound [SiH3]F XPBBUZJBQWWFFJ-UHFFFAOYSA-N 0.000 description 1
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- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
-
- 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
- C23C22/24—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 hexavalent chromium compounds
- C23C22/26—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 hexavalent chromium compounds containing also organic compounds
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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
- C23C22/24—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 hexavalent chromium compounds
- C23C22/26—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 hexavalent chromium compounds containing also organic compounds
- C23C22/27—Acids
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- 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
- C23C22/24—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 hexavalent chromium compounds
- C23C22/26—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 hexavalent chromium compounds containing also organic compounds
- C23C22/28—Macromolecular compounds
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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
- C23C22/24—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 hexavalent chromium compounds
- C23C22/33—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 hexavalent chromium compounds containing also phosphates
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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
- C23C22/78—Pretreatment of the material to be coated
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Abstract
本发明公开了一种铝及铝合金表面的新型耐腐蚀性超疏水涂层及其制备方法，具体为：将铝或铝合金依次经清洁预处理、浸渍提拉镀膜、原位化学固化处理后实现了涂层的均匀附着和有效增强二者界面的结合力，从而获得了超强稳定性的新型耐腐蚀性超疏水涂层。本发明利用浸渍提拉法快速将铜、铬、镍等化学结合在铝及铝合金表面，有效增强二者界面的结合力；同时采用促进剂和分散剂有效改变了铝及铝合金表面官能团，并通过原位化学固化处理进一步颗粒增强耐腐蚀涂层的疏水性能，在后续使用过程中超疏水性更好，耐久性更强，从而实现超强稳定性的新型耐腐蚀性超疏水涂层的制备，在航空航天、电子电气、船舶建筑等领域有广阔的应用前景。
Description
技术领域
本发明属于金属表面功能涂层技术领域，具体涉及一种铝及铝合金表面的新型耐腐蚀性超疏水涂层及其制备方法。
背景技术
铝及铝合金是广泛应用于航空航天、电子电气、船舶建筑等领域的重要材料，具有密度小、价格便宜、力学性能好和可加工性能优异的优点。然而，未经过表面处理的铝及铝合金在湿润的环境下会发生不同程度的腐蚀现象，并且还容易生成氧化膜，严重影响其正常使用性。因此，通常需要对铝及铝合金进行表面处理，制备出耐腐蚀的涂层以保证长时间的正常使用。
此外，铝及铝合金在潮湿环境中使用时腐蚀速率明显大于干燥环境，然而并不能保证铝及铝合金一定在干燥环境中使用。超疏水通常指水滴与基体表面的接触角大于150°且滚动角小于10°，此时基体表面基本不会受到水滴的影响。如果能够使得铝及铝合金制品的表面具有超疏水特性，这将能够有效降低潮湿环境中水汽对铝及铝合金的腐蚀效果。然而目前兼具耐腐蚀和超疏水的多功能涂层制备步骤繁多，工艺复杂，并且部分涂层结合力较弱，使用稳定性还有待提升。因此通过简单的技术手段获得铝及铝合金表面超强稳定性的新型耐腐蚀性超疏水涂层将是一种减少材料失效事故发生、降低企业生产成本、促进产业快速发展的有效方法。
中国专利《在铝合金表面制备耐腐蚀超疏水膜层的方法》(申请号：CN201910929771.1，授权号：CN110724992B，公告日：2021.07.09)公开了一种在铝合金表面制备耐腐蚀超疏水膜层的方法，通过对预磨的铝合金基体进行清洗后，依次进行电解抛光、阳极氧化、扩孔处理以及电化学镀镍、镀钴处理，构建花瓣状微纳米粗糙结构，最后放入氟硅烷乙醇溶液中浸泡获得耐腐蚀超疏水膜层，有效的提高了铝合金的耐蚀性。然而该方法生产步骤繁多、工艺复杂，成本较高，并且不适用于大型铝基材料。
中国专利《一种铝合金表面耐磨超疏微纳复合结构的制备方法及系统》(申请号：CN201911336345.3，授权号：CN110938860B，公告日：2021.08.20)公开了一种铝合金表面耐磨超疏微纳复合结构的制备方法及系统，通过超声清洗、电化学刻蚀以及后处理清洗等步骤对铝合金板材进行了处理，提高了铝合金表面的超疏水性以及耐磨耐腐蚀性。该方法虽然效率较高，但对于设备的要求较大，并且并未在铝合金表面形成保护膜，使用稳定性较差。
中国专利《一种铝合金板带用石墨烯/烷烃复合涂层及其制备方法》(申请号：CN202010768026.6，授权号：CN111849225B，公告日：2021.11.05)公开了一种铝合金板带用石墨烯/烷烃复合涂层。通过添加含有烷烃或环烷烃、石墨烯及其衍生物等的涂料在铝合金板带表面，实现耐腐蚀性、疏水性、长使用寿命的涂层制备。该方法环保、低成本、工艺简单、可连续生产，适合于铝合金的表面处理，然而有机复合涂层不耐高温，膜基结合力较弱导致使用稳定性较差，并且添加的石墨烯材料价格昂贵，并不适用于企业生产。
中国专利《一种疏水、水下疏油性能好的铝合金表面处理工艺》(申请号：CN202111125663.2，授权号：CN113564596B，公告日：2022.02.11)公开了一种疏水、水下疏油性能好的铝合金表面处理工艺，通过在铝合金材料表面激光雕刻鱼鳞图案，随后经过分步化学蚀刻和硬脂酸修饰后获得疏水、水下疏油效果好的铝合金表面。该方法同样对于设备要求较高、工艺复杂，经过处理后的表面并不能有效提升其耐腐蚀性能，使用稳定性较差。
发明内容
本发明的目的是提供一种铝及铝合金表面的新型耐腐蚀性超疏水涂层及其制备方法，解决了现有技术步骤繁多、工艺复杂并且膜基结合力较弱而导致生产成本高、使用稳定性较差的问题。
本发明是通过以下技术方案实现的：
一种铝及铝合金表面的新型耐腐蚀性超疏水涂层的制备方法，包括如下步骤：
(1)清洁预处理：
将铝或铝合金放入氢氧化钠溶液中浸泡一定时间后采用流动水清洗，随后经硝酸溶液洗涤并采用流动水清洗干净，获得表面光亮、清洁度高的铝或铝合金；
(2)浸渍提拉镀膜：
将步骤(1)经清洁预处理的铝或铝合金浸入预先制备好的反应溶液1中，通过均匀的速度将其平稳提拉出来，调节溶液温度、提拉速度等获得耐腐蚀性涂层；
(3)原位化学固化：
将步骤(2)中所得的铝或铝合金进行原位化学固化处理，选择合适的喷涂流量、压力、固化温度、时长以及环境湿度等，通过雾化喷涂技术将反应溶液2喷涂在铝或铝合金表面，在出口处60℃烘干处理后获得新型耐腐蚀性超疏水涂层。
进一步地，步骤(1)中所述的氢氧化钠溶液质量分数为3％～6％，浸泡时间为60s～120s，流动水清洗时间为30s～60s，硝酸溶液质量分数为8％～15％，洗涤时间为40s～100s，流动水清洗时间为120s～240s。
进一步地，步骤(2)中所述的反应液1按照质量百分比由以下物质组成：水溶性铜盐为0.5％～1.5％，水溶性铬盐为0.05％～0.3％，水溶性镍盐为1％～2.5％，促进剂为0.02％～0.1％，分散剂为0.03％～0.2％，水为95.4％～98.4％，以上组分总和为100％；此外还需添加酸性物质维持溶液pH为4.2～5.2。
进一步地，所述水溶性铜盐为氯化铜、硫酸铜、硝酸铜等中的一种或多种，水溶性铬盐为氯化铬、硫酸铬、硝酸铬等中的一种或多种，水溶性镍盐为氯化镍、硫酸镍、硝酸镍等中的一种或多种，促进剂为次磷酸钠、氟化钠、氟锆酸钠、亚铁氰化钾等中的一种或多种，分散剂为十二烷基苯磺酸钠、六偏磷酸钠、焦磷酸钠、硅烷偶联剂KH570、聚丙烯酰胺、硬脂酸铜等中的一种或多种，酸性物质为盐酸、乙酸、硫酸、硝酸等中的一种或多种。
进一步地，步骤(2)中所述的溶液温度为60℃～85℃，提拉速度为3cm/min～5cm/min。
进一步地，步骤(3)中所述的原位化学固化处理的工艺参数为：选择喷涂流量5mL/min～20mL/min，压力0.2MPa～1.0MPa，固化温度80℃～90℃，时长20s～40s，环境湿度30％～40％。
进一步地，步骤(3)中所述的反应溶液2按照质量百分比由以下物质组成：正硅酸四乙酯15％～25％，改性剂3％～8％，水67％～82％，以上组分总和为100％。其中改性剂为六甲基二硅氮烷，十七氟癸基三乙氧基硅烷，二乙烯基四甲基二硅氮烷，硅烷偶联剂KH570，三乙氧基硅基丙基四硫化物等中的一种或多种。
本发明相比现有技术具有以下优点：
1、本发明选择控制水溶性铜盐、铬盐、镍盐的含量，实现铝及铝合金表面涂层成分的调控，并通过调节促进剂来充分控制在铝及铝合金表面的化学反应速率，实现涂层的均匀附着和有效增强二者界面的结合力，改变分散剂的含量来调节铝及铝合金的表面官能团，增强耐腐蚀性能；并控制原位化学固化处理的工艺参数，进一步固化增强涂层结合，且实现了颗粒增强耐腐蚀涂层疏水性能的目的，使其在使用过程中耐久性更强，从而获得了超强稳定性的新型耐腐蚀性超疏水涂层。
2、本发明简单方便的制备出超强稳定性的新型耐腐蚀性超疏水涂层，充分利用浸渍提拉法快速将铜、铬、镍等化学结合在铝及铝合金表面，有效增强二者界面的结合力；同时采用促进剂和分散剂有效改变了铝及铝合金表面官能团，并通过原位化学固化处理进一步颗粒增强耐腐蚀涂层的疏水性能，在后续使用过程中超疏水性更好，耐久性更强，从而实现超强稳定性的新型耐腐蚀性超疏水涂层的制备，在航空航天、电子电气、船舶建筑等领域有广阔的应用前景。
附图说明
图1为本申请实施例1制备的耐腐蚀性超疏水涂层的水接触角。
具体实施方式
下面结合附图和具体实施方式对本发明进行详细说明。
本发明所采用的技术方案是，一种铝及铝合金表面的新型耐腐蚀性超疏水涂层及其制备方法，具体按以下步骤实施：
(1)清洁预处理：
将铝或铝合金放入质量分数为3％～6％的氢氧化钠溶液中浸泡60s～120s后采用流动水清洗30s～60s，随后经质量分数为8％～15％硝酸溶液洗涤40s～100s并采用流动水清洗120s～240s，获得表面光亮、清洁度高的铝或铝合金。
(2)浸渍提拉镀膜：
将步骤(1)经清洁预处理的铝或铝合金浸入预先制备好的反应溶液1中，通过均匀的速度将其平稳提拉出来，调节溶液温度为60℃～85℃，提拉速度为3cm/min～5cm/min获得耐腐蚀性涂层。
其中步骤(2)中反应溶液1按照质量百分比由以下物质组成：水溶性铜盐为0.5％～1.5％，水溶性铬盐为0.05％～0.3％，水溶性镍盐为1％～2.5％，促进剂为0.02％～0.1％，分散剂为0.03％～0.2％，水为95.4％～98.4％，以上组分总和为100％。此外还需添加酸性物质维持溶液pH为4.2～5.2之间。
其中水溶性铜盐为氯化铜、硫酸铜、硝酸铜等中的一种或多种，水溶性铬盐为氯化铬、硫酸铬、硝酸铬等中的一种或多种，水溶性镍盐为氯化镍、硫酸镍、硝酸镍等中的一种或多种，促进剂为次磷酸钠、氟化钠、氟锆酸钠、亚铁氰化钾等中的一种或多种，分散剂为十二烷基苯磺酸钠、六偏磷酸钠、焦磷酸钠、硅烷偶联剂KH570、聚丙烯酰胺、硬脂酸铜等中的一种或多种，酸性物质为盐酸、乙酸、硫酸、硝酸等中的一种或多种。
(3)原位化学固化：
将步骤(2)所得铝或铝合金进行原位化学固化处理，选择喷涂流量5mL/min～20mL/min，压力0.2MPa～1.0MPa，固化温度80℃～90℃，时长20s～40s，环境湿度30％～40％，通过雾化喷涂技术将反应溶液2喷涂在铝或铝合金表面，在出口处60℃烘干处理后获得新型耐腐蚀性超疏水涂层。
其中反应溶液2按照质量百分比由以下物质组成：正硅酸四乙酯15％～25％，改性剂3％～8％，水67％～82％，以上组分总和为100％。其中改性剂为六甲基二硅氮烷，十七氟癸基三乙氧基硅烷，二乙烯基四甲基二硅氮烷，硅烷偶联剂KH570，三乙氧基硅基丙基四硫化物等中的一种或多种。
实施例1
将铝合金放入质量分数为5％的氢氧化钠溶液中浸泡80s后采用流动水清洗40s，随后经质量分数为10％硝酸溶液洗涤60s并采用流动水清洗180s，获得表面光亮、清洁度高的铝合金。
随后浸入预先制备好的反应溶液1中，反应溶液1由硫酸铜为1.0％，氯化铬0.2％，硝酸镍1.5％，亚铁氰化钾0.05％，焦磷酸钠0.1％，水97.15％组成，并添加乙酸维持溶液pH为4.2～5.2之间。通过均匀的速度将其平稳提拉出来，调节溶液温度为75℃，提拉速度为4cm/min获得耐腐蚀性涂层。
选择喷涂流量8mL/min，压力0.8MPa，固化温度85℃，时长30s，环境湿度35％，通过雾化喷涂技术将反应溶液2喷涂在铝合金表面进行原位化学固化处理，反应溶液2由正硅酸四乙酯20％，5％硅烷偶联剂KH570，水75％组成，在出口处60℃烘干后获得新型耐腐蚀性超疏水涂层。
实施例2
将铝放入质量分数为3％的氢氧化钠溶液中浸泡120s后采用流动水清洗30s，随后经质量分数为15％硝酸溶液洗涤40s并采用流动水清洗240s，获得表面光亮、清洁度高的铝。
随后浸入预先制备好的反应溶液1中，反应溶液1由氯化铜0.5％，硝酸铬0.05％，硝酸镍1％，氟化钠0.02％，十二烷基苯磺酸钠0.03％，水98.4％组成，并添加硝酸维持溶液pH为4.2～5.2之间。通过均匀的速度将其平稳提拉出来，调节溶液温度为85℃，提拉速度为3cm/min获得耐腐蚀性涂层。
选择喷涂流量5mL/min，压力1.0MPa，固化温度80℃，时长40s，环境湿度30％，通过雾化喷涂技术将反应溶液2喷涂在铝表面进行原位化学固化处理，反应溶液2由正硅酸四乙酯15％，六甲基二硅氮烷3％，水82％组成，在出口处60℃烘干后获得新型耐腐蚀性超疏水涂层。
实施例3
将铝合金放入质量分数为4％的氢氧化钠溶液中浸泡100s后采用流动水清洗45s，随后经质量分数为12％硝酸溶液洗涤60s并采用流动水清洗200s，获得表面光亮、清洁度高的铝或铝合金。
随后浸入预先制备好的反应溶液1中，反应溶液1由硝酸铜1.2％，硝酸铬0.25％，氯化镍1.8％，次磷酸钠0.06％，聚丙烯酰胺0.08％，水为95.89％组成，并添加盐酸维持溶液pH为4.2～5.2之间。通过均匀的速度将其平稳提拉出来，调节溶液温度为65℃，提拉速度为3cm/min获得耐腐蚀性涂层。
选择喷涂流量12mL/min，压力0.7MPa，固化温度82℃，时长25s，环境湿度33％，通过雾化喷涂技术将反应溶液2喷涂在铝或铝合金表面进行原位化学固化处理，反应溶液2由正硅酸四乙酯18％，三乙氧基硅基丙基四硫化物4％，水78％组成，在出口处60℃烘干后获得新型耐腐蚀性超疏水涂层。
实施例4
将铝合金放入质量分数为6％的氢氧化钠溶液中浸泡60s后采用流动水清洗60s，随后经质量分数为8％硝酸溶液洗涤100s并采用流动水清洗120s，获得表面光亮、清洁度高的铝合金。
随后浸入预先制备好的反应溶液1中，反应溶液1由硫酸铜1.5％，硫酸铬0.3％，硫酸镍2.5％，氟锆酸钠0.1％，硬脂酸铜0.2％，水95.4％组成，并添加硫酸维持溶液pH为4.2～5.2之间。通过均匀的速度将其平稳提拉出来，调节溶液温度为60℃，提拉速度为5cm/min获得耐腐蚀性涂层。
选择喷涂流量20mL/min，压力0.2MPa，固化温度90℃，时长20s，环境湿度40％，通过雾化喷涂技术将反应溶液2喷涂在铝合金表面进行原位化学固化处理，反应溶液2由正硅酸四乙酯25％，二乙烯基四甲基二硅氮烷8％，水67％组成，在出口处60℃烘干后获得新型耐腐蚀性超疏水涂层。
表1是实施例1中具有新型耐腐蚀性超疏水涂层的铝合金与未进行涂层修饰铝合金的耐腐蚀性及水接触角对比。
表1具有新型耐腐蚀性超疏水涂层的铝合金与未进行涂层修饰的铝合金的耐腐蚀性及水接触角
从表1中可以看出，未进行涂层修饰的铝合金耐腐蚀性较差，在铜乙酸加速实验6h后出现鼓泡现象，表面凹凸不平。而具有新型耐腐蚀性超疏水涂层的铝合金表面没有任何变化，依然光洁如新。对比它们的水接触角发现，未进行涂层修饰的铝合金水接触角约为85°，具有新型耐腐蚀性超疏水涂层的铝合金的水接触角达到了163°，这表明通过浸渍提拉结合原位化学固化处理充分将铜、铬、镍等化学结合在铝及铝合金表面，还通过颗粒增强耐腐蚀涂层的疏水性能，从而实现了铝合金表面耐久性更强的新型耐腐蚀性超疏水涂层的制备。
图1是本发明实施例1制备的耐腐蚀性超疏水涂层的水接触角。从图1可以看出，水滴在铝合金表面基本保持球形结构，没有出现扁平化粘附现象，其与涂层的水接触角达到了163°，表明所制备的涂层是超疏水性的。
Claims (8)
1.一种铝及铝合金表面的新型耐腐蚀性超疏水涂层的制备方法，其特征在于，包括如下步骤：
(1)清洁预处理：
将铝或铝合金放入氢氧化钠溶液中浸泡后采用流动水清洗，随后经硝酸溶液洗涤并采用流动水清洗干净，获得表面光亮、清洁度高的铝或铝合金；
(2)浸渍提拉镀膜：
将步骤(1)经清洁预处理的铝或铝合金浸入预先制备好的反应溶液1中，通过均匀的速度将其平稳提拉出来，调节溶液温度、提拉速度等获得耐腐蚀性涂层；
(3)原位化学固化：
将步骤(2)中所得的铝或铝合金进行原位化学固化处理，选择合适的喷涂流量、压力、固化温度、时长以及环境湿度等，通过雾化喷涂技术将反应溶液2喷涂在铝或铝合金表面，在出口处60℃烘干处理后获得新型耐腐蚀性超疏水涂层。
2.根据权利要求1所述一种铝及铝合金表面的新型耐腐蚀性超疏水涂层的制备方法，其特征在于，步骤(1)中所述的氢氧化钠溶液质量分数为3％～6％，浸泡时间为60s～120s，流动水清洗时间为30s～60s，硝酸溶液质量分数为8％～15％，洗涤时间为40s～100s，流动水清洗时间为120s～240s。
3.根据权利要求1所述一种铝及铝合金表面的新型耐腐蚀性超疏水涂层的制备方法，其特征在于，步骤(2)中所述的反应液1按照质量百分比由以下物质组成：水溶性铜盐为0.5％～1.5％，水溶性铬盐为0.05％～0.3％，水溶性镍盐为1％～2.5％，促进剂为0.02％～0.1％，分散剂为0.03％～0.2％，水为95.4％～98.4％，以上组分总和为100％；此外还需添加酸性物质维持溶液pH为4.2～5.2。
4.根据权利要求3所述一种铝及铝合金表面的新型耐腐蚀性超疏水涂层的制备方法，其特征在于，所述水溶性铜盐为氯化铜、硫酸铜、硝酸铜等中的一种或多种，水溶性铬盐为氯化铬、硫酸铬、硝酸铬等中的一种或多种，水溶性镍盐为氯化镍、硫酸镍、硝酸镍等中的一种或多种，促进剂为次磷酸钠、氟化钠、氟锆酸钠、亚铁氰化钾等中的一种或多种，分散剂为十二烷基苯磺酸钠、六偏磷酸钠、焦磷酸钠、硅烷偶联剂KH570、聚丙烯酰胺、硬脂酸铜等中的一种或多种，酸性物质为盐酸、乙酸、硫酸、硝酸等中的一种或多种。
5.根据权利要求1所述一种铝及铝合金表面的新型耐腐蚀性超疏水涂层的制备方法，其特征在于，步骤(2)中所述的溶液温度为60℃～85℃，提拉速度为3cm/min～5cm/min。
6.根据权利要求1所述一种铝及铝合金表面的新型耐腐蚀性超疏水涂层的制备方法，其特征在于，步骤(3)中所述的原位化学固化处理的工艺参数为：选择喷涂流量5mL/min～20mL/min，压力0.2MPa～1.0MPa，固化温度80℃～90℃，时长20s～40s，环境湿度30％～40％。
7.根据权利要求6所述一种铝及铝合金表面的新型耐腐蚀性超疏水涂层的制备方法，其特征在于，步骤(3)中所述的反应溶液2按照质量百分比由以下物质组成：正硅酸四乙酯15％～25％，改性剂3％～8％，水67％～82％，以上组分总和为100％。其中改性剂为六甲基二硅氮烷，十七氟癸基三乙氧基硅烷，二乙烯基四甲基二硅氮烷，硅烷偶联剂KH570，三乙氧基硅基丙基四硫化物等中的一种或多种。
8.一种铝及铝合金表面的新型耐腐蚀性超疏水涂层，其特征在于，按照权利要求1～7任意一项方法制备而成。
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