CN116875967A - Method for directly plating nickel on aluminum substrate surface after copper activation - Google Patents
Method for directly plating nickel on aluminum substrate surface after copper activation Download PDFInfo
- Publication number
- CN116875967A CN116875967A CN202310805973.1A CN202310805973A CN116875967A CN 116875967 A CN116875967 A CN 116875967A CN 202310805973 A CN202310805973 A CN 202310805973A CN 116875967 A CN116875967 A CN 116875967A
- Authority
- CN
- China
- Prior art keywords
- activation
- copper
- plating
- nickel
- aluminum substrate
- Prior art date
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 99
- 238000007747 plating Methods 0.000 title claims abstract description 75
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 49
- 239000010949 copper Substances 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 47
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 46
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 230000004913 activation Effects 0.000 title claims abstract description 42
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 35
- 239000000758 substrate Substances 0.000 title claims abstract description 33
- 238000005530 etching Methods 0.000 claims abstract description 31
- 239000002253 acid Substances 0.000 claims abstract description 16
- 230000003213 activating effect Effects 0.000 claims abstract description 11
- 238000005238 degreasing Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 10
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 7
- 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 5
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-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
- 239000011780 sodium chloride Substances 0.000 claims description 4
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 4
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 4
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims description 3
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims description 3
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims description 3
- MCPLVIGCWWTHFH-UHFFFAOYSA-L methyl blue Chemical compound [Na+].[Na+].C1=CC(S(=O)(=O)[O-])=CC=C1NC1=CC=C(C(=C2C=CC(C=C2)=[NH+]C=2C=CC(=CC=2)S([O-])(=O)=O)C=2C=CC(NC=3C=CC(=CC=3)S([O-])(=O)=O)=CC=2)C=C1 MCPLVIGCWWTHFH-UHFFFAOYSA-L 0.000 claims description 3
- 239000001509 sodium citrate Substances 0.000 claims description 3
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 2
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims description 2
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 2
- OZECDDHOAMNMQI-UHFFFAOYSA-H cerium(3+);trisulfate Chemical compound [Ce+3].[Ce+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O OZECDDHOAMNMQI-UHFFFAOYSA-H 0.000 claims description 2
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000011790 ferrous sulphate Substances 0.000 claims description 2
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 2
- 239000000276 potassium ferrocyanide Substances 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 239000001488 sodium phosphate Substances 0.000 claims description 2
- 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 2
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 2
- 229910000406 trisodium phosphate Inorganic materials 0.000 claims 1
- 235000019801 trisodium phosphate Nutrition 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 16
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 abstract description 9
- OFNHPGDEEMZPFG-UHFFFAOYSA-N phosphanylidynenickel Chemical compound [P].[Ni] OFNHPGDEEMZPFG-UHFFFAOYSA-N 0.000 abstract description 7
- 229910045601 alloy Inorganic materials 0.000 abstract description 6
- 239000000956 alloy Substances 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 229910052763 palladium Inorganic materials 0.000 abstract description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052709 silver Inorganic materials 0.000 abstract description 4
- 239000004332 silver Substances 0.000 abstract description 4
- 229910001096 P alloy Inorganic materials 0.000 abstract description 2
- 238000002425 crystallisation Methods 0.000 abstract description 2
- 230000008025 crystallization Effects 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 238000001994 activation Methods 0.000 description 30
- 229910000838 Al alloy Inorganic materials 0.000 description 25
- 230000007797 corrosion Effects 0.000 description 17
- 238000005260 corrosion Methods 0.000 description 17
- 229910021641 deionized water Inorganic materials 0.000 description 12
- 239000011701 zinc Substances 0.000 description 10
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 9
- 229910052725 zinc Inorganic materials 0.000 description 8
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical group [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 239000003638 chemical reducing agent Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000003513 alkali Substances 0.000 description 5
- 230000007246 mechanism Effects 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- -1 Pd and Ni Chemical class 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 230000008021 deposition Effects 0.000 description 4
- 238000007772 electroless plating Methods 0.000 description 4
- 229910001453 nickel ion Inorganic materials 0.000 description 4
- 230000010287 polarization Effects 0.000 description 4
- 229910001008 7075 aluminium alloy Inorganic materials 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000008139 complexing agent Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 2
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- VREFGVBLTWBCJP-UHFFFAOYSA-N alprazolam Chemical compound C12=CC(Cl)=CC=C2N2C(C)=NN=C2CN=C1C1=CC=CC=C1 VREFGVBLTWBCJP-UHFFFAOYSA-N 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 229910001431 copper ion Inorganic materials 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000006479 redox reaction Methods 0.000 description 2
- 229910018104 Ni-P Inorganic materials 0.000 description 1
- 229910018536 Ni—P Inorganic materials 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000357 carcinogen Toxicity 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 description 1
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 description 1
- 229940112669 cuprous oxide Drugs 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical group O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- AVTYONGGKAJVTE-OLXYHTOASA-L potassium L-tartrate Chemical compound [K+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O AVTYONGGKAJVTE-OLXYHTOASA-L 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910000162 sodium phosphate Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 239000011787 zinc oxide Substances 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/38—Coating with copper
- C23C18/40—Coating with copper using reducing agents
-
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
- C23C18/1824—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
- C23C18/1837—Multistep pretreatment
- C23C18/1844—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
-
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
-
- 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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/32—Alkaline compositions
- C23F1/36—Alkaline compositions for etching aluminium or alloys thereof
-
- 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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
- C23G1/22—Light metals
Landscapes
- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemically Coating (AREA)
Abstract
The invention belongs to the technical field of alloy nickel plating, and particularly relates to a method for directly plating nickel on the surface of an aluminum substrate after copper activation. The method can successfully initiate the chemical nickel plating process on the aluminum by copper through the steps of degreasing, alkaline etching, acid etching, activating and the like, so that the nanocrystalline nickel-phosphorus alloy with uniform components and fine crystallization is prepared through copper activation. The invention solves the problems of complex process, environmental pollution, slow plating time, poor plating binding force and the like in the prior art, can reduce the production cost compared with silver activation and palladium activation, and is suitable for large-scale industrial production.
Description
Technical Field
The invention belongs to the technical field of alloy nickel plating, and particularly relates to a method for directly plating nickel on the surface of an aluminum substrate after copper activation.
Background
The aluminum alloy has wide application prospect in the industries of aerospace, aviation, computer manufacturing, automobile, rail train manufacturing and the like, and has become an increasingly important novel material. When the aluminum alloy is used as a structural member, hardness, wear resistance and corrosion resistance are necessary requirements, but the aluminum alloy has the problems of insufficient hardness, wear resistance and corrosion resistance due to inherent characteristics of aluminum phases in the aluminum alloy, so that the application of the aluminum alloy is limited.
Electroless nickel refers to a process of reducing metal ions to metal atoms by means of electron emission by catalytic reaction of a reducing agent in solution without power supply, which enables plating regardless of the shape of the product. The electroless plating is a process for plating an amorphous Ni-P alloy plating layer on a metal or nonmetal surface by a chemical method, and the nickel plating layer has the characteristics of excellent corrosion resistance, excellent wear resistance, high hardness, uniform thickness, better binding force than a plating layer, excellent smoothness and the like. The performance of the plating layer is closely related to the pretreatment of the aluminum substrate, and nickel plating layers with different binding force strength can be obtained by different activation modes. It is well known that initiation of electroless nickel plating on a substrate surface requires catalytically active sites, and that some transition metals, such as Pd and Ni, can initiate the electroless nickel plating process due to their catalytic activity on sodium hypophosphite. Other metals, such as Zn, fe, al, etc., are not catalytically active themselves, but can reduce nickel ions to elemental nickel, thereby acting as catalytically active sites. Copper is generally considered to be catalytically inactive in electroless nickel plating and cannot initiate electroless nickel plating.
At present, the pretreatment modes of the aluminum alloy mainly comprise: a secondary zinc leaching method, a direct plating method, a nickel leaching method, a silver activation method and a palladium activation method. The secondary zincating method has the main disadvantage that in a humid and corrosive environment, the zincating layer is anode relative to the nickel plating layer and will be subjected to transverse corrosion, and finally the nickel plating layer is peeled off. Zinc ions can cause pollution to plating solution during plating. The nickel pre-plating method can overcome the defects of the secondary zinc dipping method, but the mole ratio of the complexing agent to nickel ions and the PH value in the process are key process factors, and the activation degree and the plating solution stability are not high. The direct plating method has great difficulty, and is similar to the nickel dipping method, and parameters are difficult to control. Silver and palladium are noble metals, and silver activation and palladium activation are relatively costly and unsuitable for large-scale commercial applications.
In summary, although the above-mentioned methods can electroless nickel plating on the surface of aluminum alloy, various problems and complicated process and high cost occur in the pretreatment process, and the requirements of the current enterprises cannot be met. Therefore, developing an electroless nickel plating technique for aluminum alloy surfaces, which is suitable for industrial mass production, simple in process, environment-friendly, low in cost and the like, becomes a research difficulty in the field.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and provides a method for preparing nanocrystalline nickel-phosphorus alloy with uniform components and fine crystallization by copper activation.
The invention provides a method for directly plating nickel on the surface of an aluminum substrate after copper activation, which is shown in figure 1 and comprises the following steps:
alkaline degreasing: removing dirt on the surface of the aluminum substrate to enable the surface of the aluminum to be in a clean and pollution-free state;
alkali etching: removing the oxide film and various alloy elements and impurities on the surface of the aluminum substrate to further expose the aluminum substrate, and providing an aluminum-rich surface for subsequent plating.
Acid etching: after alkali etching, the surface of the aluminum substrate is black gray, and is an etching product generated by alkali etching, and the product is unfavorable for the combination of a coating, so that acid etching removal is required. The acid etching makes the surface of the substrate bright, and can improve the binding force of the plating layer while activating the substrate.
Copper activation: through the pretreatment of the steps, the surface of the aluminum substrate has a catalytic active center. Oxidation-reduction reactions occur in the copper activation solution, allowing copper to be deposited on the surface of the aluminum substrate.
Chemical nickel plating: after the copper-activated aluminum alloy is placed in a nickel plating solution, electrons are released by aluminum corrosion for nickel ion deposition, and the electroless plating process is continuously carried out according to an autocatalytic mechanism after nickel deposition.
Wherein, the de-ionized water washing process is carried out for one time or a plurality of times among the oil removal, alkali etching, acid washing, copper activation and chemical nickel plating processes.
1. Components of the oil removal liquid: 25g/L sodium carbonate, 25g/L sodium phosphate, 2g/L sodium dodecyl benzene sulfonate.
2. The alkaline etching solution comprises the following components: 50g/L sodium hydroxide, 2g/L sodium dodecyl benzene sulfonate.
3. The components of the acid etching solution are as follows: 10% nitric acid
4. Copper activating solution comprises the following components: 15g/L copper sulfate, 15g/L sodium citrate, 20g/L disodium ethylenediamine tetraacetate, 30g/L sodium hypophosphite, 30mg/L anhydrous potassium ferrocyanide, 20mg/L2,2' -bipyridine, 10g/L sodium chloride, 2g/L nickel sulfate, 0.8g/L cerium sulfate, 1.5g/L ferrous sulfate, 2g/L polyethylene glycol, 0.5g/L ammonium persulfate, 0.2g/L methyl blue, 0.2g/L thiourea, 30mg/L polyvinylpyrrolidone, and ph of 9.
The invention provides a method for activating electroless nickel-plated copper of an aluminum alloy, which comprises the following steps:
(1) The cut area was 2x2cm 2 The 7075 aluminum substrate is placed in alkaline degreasing liquid for degreasing for 5min at the temperature of 70 ℃, and then deionized water is used for washing.
(2) The deoiled substrate is etched in an alkaline etching solution for 30s at 25 ℃, and then washed with deionized water.
(3) The base etched substrate was placed in an acid etching solution for etching for 30s at 25 c, followed by washing with deionized water.
(4) The acid etched substrate was placed in copper activation solution for 5min at 70 c and then washed with deionized water.
(5) And (3) placing the copper-activated substrate in a nickel plating solution for 60min at the temperature of 85 ℃, taking out, washing with water, and drying.
In the invention, a layer of copper particles is deposited on the surface of the aluminum alloy after the activation of the aluminum alloy copper, the copper particles do not completely cover the surface of the aluminum alloy, and micropore channels exist between the copper layer and the aluminum layer. After the nickel plating solution is put into the plating solution, copper and aluminum form a corrosion primary cell, copper serves as a cathode, aluminum serves as an anode, electrons are released by corrosion of the aluminum for nickel ion deposition, and the electroless plating process is continuously carried out according to an autocatalytic mechanism after the nickel deposition. The solution according to the invention therefore has the following advantages:
1) The copper activation solution disclosed by the invention takes sodium hypophosphite as a reducing agent to be alkalescent, and has a ph of 9, so that an aluminum substrate is not easy to corrode under the condition of the ph value. The pH value of the traditional electroless copper plating solution using formaldehyde as a reducing agent is more than 12, the concentration of sodium hydroxide is generally more than 8g/L, and the electroless copper plating solution is easy to attack an aluminum substrate, so that a plating layer is transversely peeled off.
2) The reducing agent adopted by the copper activating solution is sodium hypophosphite. The traditional electroless copper plating reducing agent is formaldehyde, the reducibility of the formaldehyde is weak, and the formaldehyde is a high-risk carcinogen, and is harmful to the environment and operators.
3) According to the copper activating solution, sodium citrate and disodium ethylenediamine tetraacetate are used as complexing agents, and copper ions are easy to react with a reducing agent under the action of the complexing agents to form cuprous ions. Meanwhile, ammonia persulfate is used as a surfactant, cuprous oxide particles can be oxidized into soluble copper ions, so that the stability of the plating solution is improved, the service life of the plating solution is prolonged (more than one and half years), and the scrapped old solution can be reused after being reprocessed, so that the production cost of enterprises is greatly reduced.
4) The copper activating solution can reduce the temperature of the plating solution, reduce the energy consumption and reduce the cost.
5) The copper activating solution contains the methyl blue corrosion inhibitor, so that the substitution attack of copper to aluminum can be further reduced.
Drawings
FIG. 1 is a flow chart of an experimental process;
FIG. 2 shows the average hardness of the aluminum matrix, zinc activation, example 1, example 2;
FIG. 3 is a schematic diagram of the electroless nickel plating mechanism on copper activated aluminum;
FIG. 4 shows Tafil polarization curves of nickel plating in 3.5% NaCl solution for two activation modes;
FIG. 5 is an SEM image of copper-activated electroless nickel plating of example 1;
FIG. 6 is an SEM image of copper-activated electroless nickel plating of example 2;
fig. 7 is an SEM image of zinc-activated electroless nickel plating in comparative example 1.
Detailed Description
The technical solutions provided by the present invention are described in detail below in conjunction with examples for further illustrating the present invention, but they should not be construed as limiting the scope of the present invention.
Example 1
Taking a piece with an area of 2x2cm 2 The 7075 aluminum alloy is put into degreasing liquid at 70 ℃ to remove surface oil stains for 5min, and the aluminum alloy is taken out and washed by deionized water for a plurality of times. And (3) placing the deoiled aluminum alloy into alkaline etching solution, wherein the temperature is room temperature and the time is 30s. And taking out the aluminum alloy, cleaning the aluminum alloy by deionized water for a plurality of times, and putting the aluminum alloy into acid etching solution at room temperature for 15 seconds. Taking out, washing with deionized water for several times, placing into copper activating solution, the temperature was 70℃and the time was 2min. And taking out, washing with deionized water for multiple times, and putting into nickel plating solution, wherein the plating time is 60min, so that a uniform, complete and strong-binding-force nickel-phosphorus plating layer can be obtained.
Example 2
Taking a piece with an area of 2x2cm 2 The 7075 aluminum alloy is put into degreasing liquid at 60 ℃ to remove surface oil stains for 10min, and the aluminum alloy is taken out and washed by deionized water for a plurality of times. And (3) placing the deoiled aluminum alloy into alkaline etching solution, wherein the temperature is room temperature and the time is 45s. And taking out the aluminum alloy, cleaning the aluminum alloy by deionized water for many times, and putting the aluminum alloy into acid etching solution at room temperature for 30 seconds. Taking out, washing with deionized water for several times, placing into copper activating solution, the temperature was 65℃and the time was 5min. And after being taken out, the nickel-phosphorus plating solution is cleaned by deionized water for a plurality of times and is put into the nickel-plating solution, and the plating time is 60 minutes, so that the uniform, complete and strong-binding-force nickel-phosphorus plating layer can be obtained.
Comparative example 1
To demonstrate the feasibility of copper activation, a comparative set of test Zn activations was set up, with the exception of the activation solution, the procedure being exactly as in example 1. The formulation of comparative example 1 was: 2g/L zinc oxide, 45g/L sodium hydroxide, 40g/L ferric trichloride and 20g/L potassium tartrate. After plating for 60min, a uniform, complete nickel-phosphorus plating layer with strong binding force is obtained
According to GB/T5270-2005 (review of methods for experiments of adhesion strength of electrodeposited and chemically deposited layers of a metal coating on a metal substrate), the nickel-plated part of an aluminum substrate obtained by the above process is subjected to three tests including bending test, adhesive tape scribing and cross-hatch test and thermal shock test (the plated part is heated to 220 ℃ for 1h and then taken out and immediately quenched in room temperature water), and the results are shown in the following Table 1.
Table 1 performance test of aluminum substrates of examples 1 and 2 after nickel plating
Because the hardness and the wear resistance of the aluminum alloy are poor, the hardness of the nickel plating layer can be greatly improved after chemical nickel-phosphorus plating. To demonstrate this, the following comparative experiments were performed with hardness at the top and center five points of the four pieces of aluminum matrix, zinc activated, example 1, example 2, respectively. As shown in FIG. 2, the hardness of the plating piece after copper activation is 2-2.5 times that of pure aluminum, and is slightly higher than that of zinc activation in a conventional activation mode.
The chemical nickel plating mechanism on the copper activated aluminum is shown in figure 3, the aluminum substrate is pretreated by degreasing, alkali etching, acid etching and the like, the surface of the aluminum substrate is provided with a catalytic active center, and oxidation-reduction reaction is carried out after the copper activated liquid is put into the aluminum substrate, so that nickel and phosphorus can be deposited on the surface of the aluminum substrate.
Tafil polarization curves of the nickel plating layers of the two activation modes in 3.5% NaCl solution are shown in FIG. 4. The polarization curve represents a relationship curve in which the electrode potential changes with the current density, and electroless plating is usually performed with the electrode potential on the abscissa and the current density on the ordinate. The polarization curve is one of the basic rules for explaining metal corrosion, revealing metal corrosion mechanism and discussing corrosion path control, the positive electrode potential shows that the plated part is more corrosion-resistant, and the small corrosion current density shows that the corrosion rate is slow. From fig. 4 it can be seen that the Cu activation is more positive than the Zn activated plating, and the current density is smaller, thus indicating that the Cu activated plating is better corrosion resistant.
SEM pictures of electroless nickel plating in example 1, example 2, and comparative example 1 are shown in fig. 5, 6, and 7, respectively. The shape of the coating determines the properties of the coating, such as hardness, wear resistance, corrosion resistance and the like. In addition, the electroless nickel plating process of the aluminum alloy is influenced by an activation mode and a nucleation mode, and the shapes of plated parts obtained by different activation modes are different. It can therefore be explained from a morphological aspect that copper activation is better than zinc activation in terms of hardness and corrosion resistance.
Although the foregoing embodiments have been described in some, but not all, embodiments of the invention, it should be understood that other embodiments may be devised in accordance with the present embodiments without departing from the spirit and scope of the invention.
Claims (10)
1. A method for plating nickel directly after copper activation on the surface of an aluminum substrate, comprising the steps of:
sequentially carrying out alkaline degreasing, alkaline etching and acid etching on the surface of the aluminum substrate, and then placing the aluminum substrate into copper activation liquid for activation, wherein the activation temperature is 70 ℃ and the activation time is 2-5 min.
2. The method of claim 1 wherein the alkaline oil removal liquid comprises 25g/L sodium carbonate, 25g/L trisodium phosphate, 2g/L sodium dodecyl benzene sulfonate.
3. The method according to claim 1 or 2, wherein the degreasing is carried out at a temperature of 70 ℃ for a period of 5min.
4. The method according to claim 1, wherein the alkaline etching solution used for the alkaline etching comprises 50g/L sodium hydroxide and 2g/L sodium dodecyl benzene sulfonate;
the acid etching solution used for the acid etching comprises 10% nitric acid.
5. The method according to claim 4, wherein the alkaline etching is performed at a temperature of 25 ℃ for 30s;
the temperature of the acid etching is 25 ℃ and the time is 30s.
6. The method of claim 1, wherein the copper activation solution comprises the components: 15g/L copper sulfate, 15g/L sodium citrate, 20g/L disodium ethylenediamine tetraacetate, 30g/L sodium hypophosphite, 30mg/L anhydrous potassium ferrocyanide, 20mg/L2,2' -bipyridine, 10g/L sodium chloride, 2g/L nickel sulfate, 0.8g/L cerium sulfate, 1.5g/L ferrous sulfate, 2g/L polyethylene glycol, 0.5g/L ammonium persulfate, 0.2g/L methyl blue, 0.2g/L thiourea, 30mg/L polyvinylpyrrolidone, and ph of 9.
7. The method according to claim 1 or 6, wherein the activation temperature is 70 ℃ for a period of 2 to 5 minutes.
8. The method of claim 1, wherein the nickel plating is performed by placing the activated aluminum substrate in a nickel plating solution for 60 minutes at a temperature of 85 ℃.
9. The method of claim 1, wherein the degreasing, alkaline etching, acid etching, activating and nickel plating are performed one or more times between the de-ionized water washing steps.
10. The method of claim 1, wherein the nickel plating further comprises water washing and drying after removal.
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