CN114107985A - Plating process of marine environment resistant composite material plating layer - Google Patents
Plating process of marine environment resistant composite material plating layer Download PDFInfo
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- CN114107985A CN114107985A CN202111342405.XA CN202111342405A CN114107985A CN 114107985 A CN114107985 A CN 114107985A CN 202111342405 A CN202111342405 A CN 202111342405A CN 114107985 A CN114107985 A CN 114107985A
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- nickel
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- 238000007747 plating Methods 0.000 title claims abstract description 139
- 239000002131 composite material Substances 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 46
- 230000008569 process Effects 0.000 title claims abstract description 34
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 247
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 119
- 239000000126 substance Substances 0.000 claims abstract description 89
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 60
- 239000011574 phosphorus Substances 0.000 claims abstract description 60
- 238000009713 electroplating Methods 0.000 claims abstract description 40
- PEVJCYPAFCUXEZ-UHFFFAOYSA-J dicopper;phosphonato phosphate Chemical compound [Cu+2].[Cu+2].[O-]P([O-])(=O)OP([O-])([O-])=O PEVJCYPAFCUXEZ-UHFFFAOYSA-J 0.000 claims abstract description 18
- 238000005498 polishing Methods 0.000 claims abstract description 13
- 238000006388 chemical passivation reaction Methods 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims description 62
- 239000003795 chemical substances by application Substances 0.000 claims description 61
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 54
- 238000005406 washing Methods 0.000 claims description 43
- 239000002253 acid Substances 0.000 claims description 24
- 150000003839 salts Chemical class 0.000 claims description 24
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 22
- 238000007788 roughening Methods 0.000 claims description 17
- 239000011248 coating agent Substances 0.000 claims description 16
- 238000000576 coating method Methods 0.000 claims description 16
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 12
- 239000008139 complexing agent Substances 0.000 claims description 12
- 230000004913 activation Effects 0.000 claims description 10
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 9
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 9
- 239000004606 Fillers/Extenders Substances 0.000 claims description 8
- 239000010949 copper Substances 0.000 claims description 7
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 claims description 7
- 239000004576 sand Substances 0.000 claims description 7
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- 230000003213 activating effect Effects 0.000 claims description 6
- 239000000654 additive Substances 0.000 claims description 6
- 230000000996 additive effect Effects 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 229910001453 nickel ion Inorganic materials 0.000 claims description 6
- 229910052763 palladium Inorganic materials 0.000 claims description 6
- 230000003750 conditioning effect Effects 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 239000012190 activator Substances 0.000 claims description 4
- 238000007664 blowing Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 3
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 claims description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 3
- 239000004327 boric acid Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 3
- 229910000069 nitrogen hydride Inorganic materials 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- RYCLIXPGLDDLTM-UHFFFAOYSA-J tetrapotassium;phosphonato phosphate Chemical compound [K+].[K+].[K+].[K+].[O-]P([O-])(=O)OP([O-])([O-])=O RYCLIXPGLDDLTM-UHFFFAOYSA-J 0.000 claims description 3
- 239000000080 wetting agent Substances 0.000 claims description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims 6
- 241000080590 Niso Species 0.000 claims 1
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical compound [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 claims 1
- 235000011180 diphosphates Nutrition 0.000 claims 1
- 239000010410 layer Substances 0.000 abstract description 24
- 239000004696 Poly ether ether ketone Substances 0.000 abstract description 17
- 229920002530 polyetherether ketone Polymers 0.000 abstract description 17
- 239000011247 coating layer Substances 0.000 abstract description 10
- 238000005260 corrosion Methods 0.000 abstract description 6
- 230000007797 corrosion Effects 0.000 abstract description 6
- 239000000047 product Substances 0.000 description 16
- 238000012360 testing method Methods 0.000 description 16
- 239000007921 spray Substances 0.000 description 11
- 238000001994 activation Methods 0.000 description 10
- 239000012298 atmosphere Substances 0.000 description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 7
- 229910052793 cadmium Inorganic materials 0.000 description 5
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 229910000838 Al alloy Inorganic materials 0.000 description 3
- 229920000049 Carbon (fiber) Polymers 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 3
- JUPQTSLXMOCDHR-UHFFFAOYSA-N benzene-1,4-diol;bis(4-fluorophenyl)methanone Chemical compound OC1=CC=C(O)C=C1.C1=CC(F)=CC=C1C(=O)C1=CC=C(F)C=C1 JUPQTSLXMOCDHR-UHFFFAOYSA-N 0.000 description 3
- 239000004917 carbon fiber Substances 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 239000011651 chromium Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- 238000006386 neutralization reaction Methods 0.000 description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 3
- 229910000881 Cu alloy Inorganic materials 0.000 description 2
- 238000010923 batch production Methods 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 2
- 238000005488 sandblasting Methods 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 208000034656 Contusions Diseases 0.000 description 1
- 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
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 229910021626 Tin(II) chloride Inorganic materials 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 150000008043 acidic salts Chemical class 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 208000034526 bruise Diseases 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000001119 stannous chloride Substances 0.000 description 1
- 235000011150 stannous chloride Nutrition 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
- KRAHLZAGPKKBSW-UHFFFAOYSA-N tetrasodium;dioxidophosphanyl phosphite Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])OP([O-])[O-] KRAHLZAGPKKBSW-UHFFFAOYSA-N 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
Images
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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
- C23C28/023—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material only coatings of metal elements only
-
- 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
- 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
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/10—Electroplating with more than one layer of the same or of different metals
- C25D5/12—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/48—After-treatment of electroplated surfaces
- C25D5/52—After-treatment of electroplated surfaces by brightening or burnishing
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Electrochemistry (AREA)
- Inorganic Chemistry (AREA)
- Electroplating Methods And Accessories (AREA)
- Electroplating And Plating Baths Therefor (AREA)
Abstract
The invention relates to a plating process of a marine environment resistant composite material plating layer, which comprises the steps of pretreatment, alkaline pre-nickel plating, high-phosphorus chemical nickel plating, copper pyrophosphate electroplating, chemical polishing, low-stress nickel electroplating, high-phosphorus chemical nickel plating and chemical passivation. The invention realizes the technical characteristics of high conductivity and high corrosion resistance of the coating layer of the polyetheretherketone composite material through the process design of the coating layer of the polyetheretherketone composite material, and meets the requirements of electronic components of shipborne equipment avionics systems and electromechanical systems, in particular to the service environment of a composite material connector.
Description
Technical Field
The invention relates to a plating process of a marine environment resistant composite material plating layer.
Background
The ship-borne equipment takes off and lands on decks of ships and aircraft carriers in the whole service life, is parked on the decks most of time, cruises or resides along the ships and aircraft carriers, and mainly performs tasks over the ocean (patrol). The airborne equipment, the external craft pieces and the ground (ship) surface protection equipment which are arranged on the ground (ship) surface protection equipment are tested under special environmental conditions, and are subjected to stormy waves, sea fog, salt fog and temperature differences, illumination, rain and snow of different air areas and ship and carrier emissions (such as SO) of different air areas in the marine atmospheric environment with high temperature, high humidity and high salt fog for a long time2) And the corrosion effect of the comprehensive environment can generate serious corrosion effect on various metal and non-metal material equipment used on the carrier-based aircraft, particularly the connector, and the service life of the equipment is influenced. Common materials of the electric connector in the marine environment include aluminum alloy, copper alloy, stainless steel, titanium alloy, composite material PEI/PEEK and the like. When the composite material is used on a carrier-based aircraft, aluminum alloy or composite materials are generally adopted except for airtight products due to the weight reduction requirement.
The invention is mainly designed for a composite material plating process. At present, the marine environment resistant coating of the composite material at home and abroad is mainly chemical nickel plating, cadmium plating and Ni-PTFE. The composite material has no conductivity, and the composite material has certain conductivity after a metal coating is deposited on the surface of the composite material, but can not meet the conductivity requirement between the shells of the product only by chemical nickel plating, cadmium plating, Ni-PTFE and the like, namely within 3.0m omega; in addition, the cadmium plating layer of the composite material is not wear-resistant, and volatile matters (such as low molecular carboxylic acid, phenol, aldehyde, ammonia gas and the like) of the non-metallic material can corrode the cadmium plating layer under the condition of sealing or no air circulation, so that white frost is generated, and the service life of the product is shortened.
Disclosure of Invention
In order to solve the problems, the invention provides a plating process of a composite material plating layer resistant to marine environment, which realizes the technical characteristics of high conductivity and high corrosion resistance of the polyether-ether-ketone composite material plating layer through the process design of the polyether-ether-ketone composite material plating layer, and meets the requirements of electronic components of shipborne equipment avionics systems and electromechanical systems, particularly the service environment of a composite material connector.
The plating process of the marine environment resistant composite material plating layer comprises pretreatment, alkaline pre-nickel plating, high-phosphorus chemical nickel plating, copper pyrophosphate electroplating, chemical polishing, low-stress nickel electroplating, high-phosphorus chemical nickel plating and chemical passivation.
The plating process of the marine environment resistant composite material plating layer comprises the following specific process steps:
step one, pretreatment: the pretreatment process comprises ultrasonic oil removal, chemical pre-roughening, physical roughening, stress removal, ultrasonic oil removal, secondary chemical roughening and activation surface conditioning; carrying out two flowing water washes on the pretreated workpiece, and washing the workpiece with pure water for later use;
step two, alkaline nickel preplating: putting the workpiece finished in the step one into a nickel plating solution at the temperature of 25-40 ℃ for treatment for 10-15 min to carry out alkaline pre-nickel plating, carrying out two-pass flowing water washing on the workpiece subjected to alkaline pre-nickel plating, and washing the workpiece with pure water for later use;
step three, high-phosphorus chemical nickel plating: carrying out high-phosphorus chemical nickel plating on the finished piece obtained in the second step, wherein the temperature is 85-90 ℃, and the electroplating time is 10-20 min; carrying out two-pass flowing water washing on the high-phosphorus chemical nickel-plated workpiece, and washing the workpiece with one-pass pure water for later use;
step four, electroplating copper pyrophosphate: electroplating copper pyrophosphate on the workpiece obtained in the third step at the temperature of 50-60 ℃; the thickness of the plating layer is required to be 25-35 mu m, the workpiece electroplated with copper pyrophosphate is subjected to two-pass flowing water washing, and one-pass pure water washing is carried out for later use;
step five, chemical polishing: chemically polishing the workpiece obtained in the fourth step at the temperature of 20-40 ℃ for 1-2 min; carrying out two flowing water washes on the chemically polished workpiece, and washing the workpiece with pure water for later use;
step six, electroplating low-stress nickel: electroplating low-stress nickel on the workpiece obtained in the fifth step at 50-60 ℃ for 1-3 min; carrying out two-pass flowing water washing on the workpiece electroplated with the low-stress nickel, and washing the workpiece with one-pass pure water for later use;
seventhly, high-phosphorus chemical nickel plating: performing high-phosphorus chemical nickel plating on the workpiece obtained in the sixth step again, wherein the temperature is 85-90 ℃, the time is 60-120 min, and the thickness is 12-18 mu m; carrying out two-pass flowing water washing on the high-phosphorus chemical nickel-plated workpiece, and washing the workpiece with one-pass pure water for later use;
step eight, chemical passivation:
chemically passivating the workpiece obtained in the seventh step at 40-70 ℃ for 5-10 min; and (4) carrying out two-time flowing washing on the chemically passivated workpiece, and drying after one-time pure water washing.
Further, in the ultrasonic oil removing step in the first step, the oil removing temperature is 60-70 ℃, and the time is 20-30 min; the content of the adopted oil removing powder in water is 30-45 g/L; the main component and content of the coarsening liquid used for chemical coarsening comprise chromic anhydride CrO3350-450 g/L and sulfuric acid H2SO4300-400 ml/L; the temperature of the chemical pre-roughening is 60-80 ℃, and the time is 5-8 min; the physical coarsening is to blow sand to the workpiece, the pressure of an air compressor is 0.3-0.4 MPa, and the sand blowing time is 0.5-2 min; the activating table adopts colloidal palladium activating solution.
Further, the main components and contents of the nickel plating solution adopted in the alkaline nickel preplating in the step two comprise 40ml/L of alkaline nickel preplating agent A, 40ml/L of alkaline nickel preplating agent B, 80ml/L of alkaline nickel preplating agent H and ammonia NH3·H2O10 ml/L; the pH of the nickel plating solution is 8.5-9.5, and Ni is2+The content is 4.0-6.0 g/L; wherein, the agent A is main salt, the agent B is complexing agent, and the agent H is acid replenisher.
Further, the main components and contents of the high-phosphorus chemical nickel plating solution in the third step comprise 60ml/L of high-phosphorus chemical nickel plating A agent and 150ml/L of high-phosphorus chemical nickel plating B agent; the pH value of the nickel plating solution is 4.5-4.8, and Ni2+The content is 5.5-6.5 g/L, and the pH value of the high-phosphorus chemical nickel plating solution is adjusted by using 50 mass percent of analytically pure ammonia water and 10 mass percent of sulfuric acid during production; adjusting the nickel ion content of the high-phosphorus chemical nickel plating solution by using a mixed solution of an agent A and an agent C in a volume ratio of 1: 1; wherein the agent A is main salt, the agent B is complexing agent, and the agent C isAn acid supplement.
Further, the plating solution for plating copper pyrophosphate in the fourth step mainly comprises copper pyrophosphate Cu2P2O7·3H270-85 g/L of O and potassium pyrophosphate K4P2O7260-340 g/L of ammonia water NH3·H2O3 ml/L, brightener 1ml/L, electroplating solution pH of 8.0-9.3, and cathode current density of 0.5-2A/dm2。
Further, the main components and contents of the electroplating solution used for the chemical polishing in the fifth step comprise additive A150ml/L, additive B75 ml/L and 50% hydrogen peroxide H by mass fraction2O2 100ml/L。
Further, the main components and contents of the electroplating solution for electroplating the low-stress nickel in the sixth step comprise NiSO4·6H2O 240～330g/L、NiCl2·6H220-30 g/L of O and H of boric acid3BO335-45 g/L of anode activator, 12ml/L of wetting agent and 12ml/L of extender; the pH of the electroplating solution is 3.8-4.8, and the cathode current density is 1-2A/dm2。
Further, the main components and contents of the high-phosphorus chemical nickel plating solution in the seventh step comprise 60ml/L of high-phosphorus chemical nickel plating agent A and 150ml/L of high-phosphorus chemical nickel plating agent B; the pH value of the nickel plating solution is 4.5-4.8, and Ni2+The content is 5.5-6.5 g/L, and the pH value of the high-phosphorus chemical nickel plating solution is adjusted by using 50 mass percent of analytically pure ammonia water and 10 mass percent of sulfuric acid during production; adjusting the nickel ion content of the high-phosphorus chemical nickel plating solution by using a mixed solution of an agent A and an agent C in a volume ratio of 1: 1; wherein, the agent A is main salt, the agent B is complexing agent, and the agent C is acid extender.
Further, the chemical passivation reagent in the step eight mainly comprises potassium dichromate K2Cr2O740～50g/L。
The invention realizes the technical characteristics of high conductivity and high corrosion resistance of the coating layer of the polyetheretherketone composite material by the process design of the coating layer of the polyetheretherketone composite material. The requirements of electronic components of shipborne equipment avionics systems and electromechanical systems, particularly the service environment of a composite material connector are met, and the developed composite material marine environment-resistant coating layer meets the following index requirements:
acid salt spray with a pH value of 3.5 meets the 480h test requirement, and the standard GJB150.11A-2009 is executed;
acid atmosphere, pH value of 3.5, meeting the 56d test requirement, and executing the standard GJB 150.28A-2009;
and thirdly, the electrical continuity of the shell conforms to the GJB599B specification, and the requirement of the electrical continuity of the shell of the composite material connector is not more than 3m omega.
The connector shell with the composite material coating layer is qualified through various tests, various performance indexes meet requirements, and the product is verified through batch production and has stable and reliable structural performance.
Drawings
FIG. 1 shows the appearance of a carbon fiber polyetheretherketone composite material after copper plating;
FIG. 2 is the appearance of the carbon fiber polyetheretherketone composite after chemical nickel plating;
FIG. 3 is an appearance of a PEEK composite coating after an acid salt spray test;
FIG. 4 shows the appearance of the PEEK composite coating after acid atmosphere test.
Detailed Description
For a better understanding of the present invention, reference will now be made to the following examples taken in conjunction with the accompanying drawings. The following examples are given to illustrate the detailed embodiments and the operation steps based on the technology of the present invention, but the scope of the present invention is not limited to the following examples.
According to the invention, by analyzing the appearance and characteristics of the composite material chemical nickel plating, the composite material cadmium plating and the composite material electroplated Ni-PTFE coating, and combining the actual use working conditions of the product, the composite material chemical nickel plating is preferably selected as the appearance coating of the marine environment resistant composite material connector, and meanwhile, the process design and optimization are carried out on the combination design and thickness of the coating, so that the index requirements of electrical continuity between the shells of the product, acid salt mist resistance, acidic atmosphere resistance and the like are finally met.
The plating process of the plating layer is described in detail below by taking the polyetheretherketone composite material as an example:
the main process flow for preparing the coating layer of the polyetheretherketone composite material comprises the following steps:
pretreatment, alkaline nickel preplating, high-phosphorus chemical nickel plating, copper pyrophosphate electroplating, chemical polishing, low-stress nickel electroplating, high-phosphorus chemical nickel plating and chemical passivation.
Step one, pretreatment:
the method comprises the following steps of pretreating a workpiece, wherein the pretreatment process specifically comprises the working procedures of ultrasonic oil removal, chemical pre-roughening, physical roughening (sand blowing), stress removal, ultrasonic oil removal, secondary chemical roughening, activation surface conditioning and the like; carrying out two flowing water washes on the pretreated workpiece, and washing the workpiece with pure water for later use;
the pretreatment of the composite material is relatively complex compared with copper alloy, aluminum alloy and steel base, and the electroplating continuity between working procedures needs to be ensured. Of course, the usability and functionality of the obtained coating are different due to different process methods of the pretreatment of the composite material. The invention adopts the schemes of combining physical coarsening and chemical coarsening, activating and surface conditioning colloid palladium and the like.
The ultrasonic oil removing process is to put the carbon fiber reinforced polyether-ether-ketone composite material into an ultrasonic oil removing tank to remove oil, wherein the oil removing temperature is 60-70 ℃, and the oil removing time is 20-30 min. The ultrasonic oil removing process adopts oil removing powder, and the content of the oil removing powder in water is 30-45 g/L. After the oil of the workpiece is removed, the surface of the workpiece is uniform and consistent, the workpiece is not blackened, and the water film is not broken after the workpiece is washed and emptied for 30 s.
The chemical roughening is realized by putting a workpiece into roughening liquid and corroding the surface of the workpiece by the roughening liquid, wherein the main component and the content of the roughening liquid comprise industrial-grade chromic anhydride CrO3350-450 g/L and analytically pure sulfuric acid H2SO4300-400 ml/L. The temperature of the chemical pre-roughening is 60-80 ℃, and the time is 5-8 min. Before chemical pre-roughening, the bath solution containing the chemical reagent can be fully stirred for 2-5 min by using a stainless steel bar so as to fully oxidize trivalent chromium in the bath solution.
The physical coarsening is to blow sand to the workpiece, the pressure of an air compressor is 0.3-0.4 MPa, and the sand blowing time is 0.5-2 min. The sand blasting surface of the part after physical coarsening (sand blasting) is uniform and consistent, and the sprue gate is rough; the workpiece has no bruise, scratch, deformation and chipping; and ensuring that the size of the finished piece is qualified.
And (3) stress relief, namely, the workpieces are placed in order, the height of the workpieces is not more than 2 layers, other articles are not allowed to be stacked on the workpieces, the workpieces are placed in an oven with the actual temperature lower than 50 ℃, and the distance between the bottom layer workpieces and the bottom of the oven is not less than 15 cm. Starting a blower switch, starting a heating switch again, heating to 100 ℃, preserving heat for 0.5h, heating to 190 ℃, preserving heat for 4-4.5 h, cooling to below 50 ℃ along with a box after heat preservation or opening a gap of below 5cm of an oven door, cooling to below 50 ℃, and taking out a workpiece.
The activation surface conditioning comprises the processes of neutralization, promotion, presoaking, activation, acceleration and the like, and the activation adopts colloidal palladium activation solution.
The neutralization temperature is 25-35 ℃, the time is 3-4 min, and the neutralization solution is alkaline solution.
The promotion is to put the workpiece into a promotion solution to adjust the surface state of the workpiece so as to accelerate the reduction effect of palladium in the activation process, wherein the promotion temperature is 25-35 ℃, the time is 5-10 min, and the promotion solution contains 2-5 g/L of sodium pyrophosphite and 150-250 ml/L of analytically pure hydrochloric acid.
The presoaking is to adjust the pH value of the surface of the workpiece to match the pH condition of the activating solution, the presoaking temperature is 20-40 ℃, the presoaking time is 10-30 s, and the presoaking solution contains 180-220 ml/L of analytically pure hydrochloric acid.
The activation is to make the surface of the composite material adsorb a layer of metal particles with catalytic activity, necessary conditions are provided for subsequent metallization, the activation temperature is 25-35 ℃, the time is 5-10 min, and the adopted activation solution contains 0.2-0.4 g/L of palladium chloride, 150-250 ml/L of analytically pure hydrochloric acid, 40-60 g/L of analytically pure sodium chloride and 3-5 g/L of analytically pure stannous chloride.
The speeding-up is to further improve the reaction activity of the palladium adsorption layer on the surface of the workpiece, the speeding-up temperature is 50-60 ℃, the time is 5-10 min, and the speeding-up solution contains 20-30 g/L sodium hypophosphite.
After each procedure is finished, the workpiece is washed by two flowing water, and the next procedure is carried out after one pure water washing.
Step two, alkaline nickel preplating:
and (3) putting the workpiece finished in the step one into an alkaline nickel plating solution at the temperature of 25-40 ℃ for treatment for 10-15 min to carry out alkaline nickel preplating. Carrying out two-time flowing water washing on the workpiece subjected to the alkaline pre-nickel plating, and washing with one-time pure water for later use;
the alkaline nickel pre-plating solution adopts a finished product formula, and comprises the main components and contents of 40ml/L of alkaline nickel pre-plating agent A, 40ml/L of alkaline nickel pre-plating agent B, 80ml/L of alkaline nickel pre-plating agent H and ammonia NH3·H2O10 ml/L; the pH of the nickel plating solution is 8.5-9.5, and Ni is2+The content is 4.0-6.0 g/L. Wherein, the agent A is main salt, the agent B is complexing agent, and the agent H is acid replenisher. Wherein, the main salt, the complexing agent and the acid replenisher can adopt a commercially available finished product formula.
Step three, high-phosphorus chemical nickel plating:
and (4) carrying out high-phosphorus chemical nickel plating on the finished piece obtained in the second step at the temperature of 85-90 ℃ for 10-20 min. Carrying out two-pass flowing water washing on the high-phosphorus chemical nickel-plated workpiece, and washing the workpiece with one-pass pure water for later use;
the high-phosphorus chemical nickel plating solution adopts a finished product formula, and comprises the main components and the content of 60ml/L of high-phosphorus chemical nickel plating A agent and 150ml/L of high-phosphorus chemical nickel plating B agent; the pH value of the nickel plating solution is 4.5-4.8, and Ni2+The content is 5.5-6.5 g/L, and the pH value of the high-phosphorus chemical nickel plating solution is adjusted by using 50% of analytically pure ammonia water and 10% of analytically pure sulfuric acid during production. The nickel ion content of the high-phosphorus chemical nickel plating solution is adjusted by using a mixed solution of the agent A and the agent C in a volume ratio of 1: 1. Wherein, the agent A is main salt, the agent B is complexing agent, and the agent C is acid extender. Wherein, the main salt, the complexing agent and the acid replenisher can adopt a commercially available finished product formula.
Step four, electroplating copper pyrophosphate:
and (4) electroplating copper pyrophosphate on the workpiece obtained in the third step at the temperature of 50-60 ℃. The thickness of the plating layer is required to be 25-35 mu m, the workpiece electroplated with copper pyrophosphate is subjected to two-pass flowing water washing, and one-pass pure water washing is carried out for later use;
electroplating solution for electroplating copper pyrophosphateComprises copper pyrophosphate Cu as main component2P2O7.3H2O70-85 g/L, potassium pyrophosphate K4P2O7260-340 g/L of ammonia water NH3·H2O3 ml/L, brightener 1ml/L, electroplating solution pH of 8.0-9.3, and cathode current density of 0.5-2A/dm2。
Step five, chemical polishing:
and (4) chemically polishing the workpiece obtained in the fourth step at the temperature of 20-40 ℃ for 1-2 min. Carrying out two flowing water washes on the chemically polished workpiece, and washing the workpiece with pure water for later use;
the electroplating solution for chemical polishing can adopt the existing finished product formula, and comprises the main components and contents of additive A150ml/L, additive B75 ml/L, and 50% hydrogen peroxide H by mass fraction2O2 100ml/L。
Step six, electroplating low-stress nickel:
and electroplating the part obtained in the fifth step with low-stress nickel at the temperature of 50-60 ℃ for 1-3 min. Carrying out two-pass flowing water washing on the workpiece electroplated with the low-stress nickel, and washing the workpiece with one-pass pure water for later use;
the main components and contents of the electroplating solution for electroplating low-stress nickel comprise NiSO4·6H2O 240～330g/L、NiCl2·6H220-30 g/L of O and H of boric acid3BO335-45 g/L of anode activator, 12ml/L of anode activator, 10ml/L of wetting agent and 12ml/L of extender. The pH of the electroplating solution is 3.8-4.8, and the cathode current density is 1-2A/dm2。
Seventhly, high-phosphorus chemical nickel plating:
and (4) carrying out high-phosphorus chemical nickel plating on the workpiece obtained in the sixth step again, wherein the temperature is 85-90 ℃, the thickness is 12-18 mu m, and the time is 60-120 min. Carrying out two-pass flowing water washing on the high-phosphorus chemical nickel-plated workpiece, and washing the workpiece with one-pass pure water for later use;
the high-phosphorus chemical nickel plating solution adopts a finished product formula, and comprises the main components and the content of 60ml/L of high-phosphorus chemical nickel plating A agent and 150ml/L of high-phosphorus chemical nickel plating B agent; the pH of the high-phosphorus chemical nickel plating solution is 4.5-4.8, and Ni2+The content is 5.5 to 6.5g/L, and the productionWhile the pH value of the high-phosphorus chemical nickel plating solution is adjusted by using analytically pure ammonia water with the mass fraction of 50 percent and analytically pure sulfuric acid with the mass fraction of 10 percent. The nickel ion content of the high-phosphorus chemical nickel plating solution is adjusted by using a mixed solution of the agent A and the agent C in a volume ratio of 1: 1. Wherein, the agent A is main salt, the agent B is complexing agent, and the agent C is acid extender. Wherein, the main salt, the complexing agent and the acid replenisher can adopt a commercially available finished product formula.
Step eight, chemical passivation:
and (4) chemically passivating the workpiece obtained in the step seven, wherein the temperature is 40-70 ℃, and the time is 5-10 min. And (4) carrying out two-time flowing washing on the chemically passivated workpiece, and drying after one-time pure water washing.
The chemical passivation reagent mainly comprises potassium dichromate K2Cr2O740-50 g/L. After the parts are passivated, high-temperature purified water is used for carefully cleaning, so that the phenomenon that the parts are not cleaned cleanly after heat treatment is avoided.
The product of the coating layer of the polyether-ether-ketone composite material prepared by the process is bright in appearance and has metallic luster, and meets the requirements of the GJB150.11A-2009 acid salt spray 480h test; GJB150.28A-2009 acidic atmosphere, 56d test requirements; the housing electrical continuity complies with the GJB599B specification (the connector housing electrical continuity requirement is no more than 3m Ω).
The method for testing the electrical continuity and the environment among the shells comprises the following steps:
(1) testing the electrical continuity between the shells:
the plugged connectors were tested as specified by method 3007 in GJB1217A-2009, and the following specifications were met:
a. the connector is not wired;
b. under the maximum direct current voltage of 1.5V, connecting a proper resistor in a circuit to limit the current to be (1 +/-0.1) A;
c. the dc resistance from any point on the tail of the plug to any point on the flange of the receptacle should be measured.
(2) Acid salt spray test:
at 35 deg.C, salt spray is prepared from (5 + -1)% NaCl solution (pH 3.5 + -0.5 by oxidizing with chemically pure dilute sulfuric acid or chemically pure hydrogenpH value adjusted by sodium), salt spray precipitation rate is (1.0-3.0) ml/80cm2H. Single cycle period 48h (24h continuous spray and 24 dry), 10 cycles total trial period, for a total of 480h, performing criteria GJB150.11A-2009. The method comprises the following steps: the coating was allowed to darken slightly and the coating did not flake, blister or flake off.
(3) Acid atmosphere test:
at 35 ℃, 11.9mg (6uL) of sulfuric acid (95-98% concentration) and 8.8mg (6uL) of nitric acid (68-71% concentration) were added to 4L of distilled or deionized water, respectively, and the pH of the test solution was adjusted to 3.5 with dilute hydrochloric acid or sodium hydroxide solution for the total duration: 56d, perform standard GJB 150.28-2009. Spraying salt spray on a sample to be tested for 2 hours, wherein the sedimentation rate of the salt solution is controlled to be 1-3 mL/(80 cm) during spraying2H), taking out the tested sample, and drying the tested sample for 7d under the conditions that the temperature is 15-35 ℃ and the relative humidity is not higher than 50%, wherein the cycle period is one cycle period and the total number is 8. The method comprises the following steps: the coating was allowed to darken slightly and the coating did not flake, blister or flake off.
Table 1 shows the orthogonal design combination scheme of copper layer and electroless nickel layer, wherein the bottom layer nickel refers to alkaline pre-nickel plating and high-phosphorous electroless nickel plating; table 2 shows the results of the electrical continuity between the housings tested according to the design combinations of table 1. Table 3 shows the results of the acid salt spray and acid atmosphere tests according to the design combination scheme of table 1.
TABLE 1 coating orthogonal design combination test protocol
TABLE 2 results of electrical continuity test between plated cases
TABLE 3 contents and results of acidic salt spray and acidic atmosphere tests on the coating
The invention mainly aims at the polyether-ether-ketone composite material, the plating process adopts the combined design of alkaline pre-plating nickel, high-phosphorus chemical nickel plating, electroplating copper pyrophosphate, electroplating low-stress nickel, high-phosphorus chemical nickel plating and other plating layers after pretreatment, and when the thickness of the high-phosphorus chemical nickel plating of the surface plating layer reaches more than 8 mu m, the marine environment resistance of the plating layer can completely reach the standard requirement. The product conductivity is combined, the copper layer thickness needs to meet more than 25um, and the electrical continuity between the shells of the composite material connector can meet the requirement within 3m omega. The combined design of the polyetheretherketone composite coating layer meets the requirements of relevant standards such as MIL-38999, GJB599, GJB1217, ASTM-B733, ASTMB117 and the like, the metal coating layer has the characteristics of high conductivity (the electrical continuity between the shells is less than or equal to 3m omega) and high corrosion resistance (acid salt spray 480h and acid atmosphere 56d), the connector shell is qualified through various tests, various performance indexes meet the requirements, and the product is verified through batch production, so that the structural performance is stable and reliable.
The above description is only an embodiment of the present invention, and is not intended to limit the present invention in any way, and the present invention may also have other embodiments according to the above structures and functions, and is not listed again. Therefore, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention by those skilled in the art can be made within the technical scope of the present invention.
Claims (10)
1. A plating process of a marine environment resistant composite material plating layer is characterized by comprising the steps of pretreatment, alkaline pre-nickel plating, high-phosphorus chemical nickel plating, copper pyrophosphate electroplating, chemical polishing, low-stress nickel electroplating, high-phosphorus chemical nickel plating and chemical passivation.
2. The plating process of the marine environment resistant composite material plating layer according to claim 1, characterized in that the specific process steps are operated as follows:
step one, pretreatment: the pretreatment process comprises ultrasonic oil removal, chemical pre-roughening, physical roughening, stress removal, ultrasonic oil removal, secondary chemical roughening and activation surface conditioning; carrying out two flowing water washes on the pretreated workpiece, and washing the workpiece with pure water for later use;
step two, alkaline nickel preplating: putting the workpiece finished in the step one into a nickel plating solution at the temperature of 25-40 ℃ for treatment for 10-15 min to carry out alkaline pre-nickel plating, carrying out two-pass flowing water washing on the workpiece subjected to alkaline pre-nickel plating, and washing the workpiece with pure water for later use;
step three, high-phosphorus chemical nickel plating: carrying out high-phosphorus chemical nickel plating on the finished piece obtained in the second step, wherein the temperature is 85-90 ℃, and the electroplating time is 10-20 min; carrying out two-pass flowing water washing on the high-phosphorus chemical nickel-plated workpiece, and washing the workpiece with one-pass pure water for later use;
step four, electroplating copper pyrophosphate: electroplating copper pyrophosphate on the workpiece obtained in the third step at the temperature of 50-60 ℃; the thickness of the plating layer is required to be 25-35 mu m, the workpiece electroplated with copper pyrophosphate is subjected to two-pass flowing water washing, and one-pass pure water washing is carried out for later use;
step five, chemical polishing: chemically polishing the workpiece obtained in the fourth step at the temperature of 20-40 ℃ for 1-2 min; carrying out two flowing water washes on the chemically polished workpiece, and washing the workpiece with pure water for later use;
step six, electroplating low-stress nickel: electroplating low-stress nickel on the workpiece obtained in the fifth step at 50-60 ℃ for 1-3 min; carrying out two-pass flowing water washing on the workpiece electroplated with the low-stress nickel, and washing the workpiece with one-pass pure water for later use;
seventhly, high-phosphorus chemical nickel plating: performing high-phosphorus chemical nickel plating on the workpiece obtained in the sixth step again, wherein the temperature is 85-90 ℃, the time is 60-120 min, and the thickness is 12-18 mu m; carrying out two-pass flowing water washing on the high-phosphorus chemical nickel-plated workpiece, and washing the workpiece with one-pass pure water for later use;
step eight, chemical passivation:
chemically passivating the workpiece obtained in the seventh step at 40-70 ℃ for 5-10 min; and (4) carrying out two-time flowing washing on the chemically passivated workpiece, and drying after one-time pure water washing.
3. The plating process of the marine environment resistant composite material plating layer according to claim 2, characterized in that in the first step, the ultrasonic oil removing process has an oil removing temperature of 60-70 ℃ for 20-30 min; the content of the adopted oil removing powder in water is 30-45 g/L; the main component and content of the coarsening liquid used for chemical coarsening comprise chromic anhydride CrO3350-450 g/L and sulfuric acid H2SO4300-400 ml/L; the temperature of the chemical pre-roughening is 60-80 ℃, and the time is 5-8 min; the physical coarsening is to blow sand to the workpiece, the pressure of an air compressor is 0.3-0.4 MPa, and the sand blowing time is 0.5-2 min; the activating table adopts colloidal palladium activating solution.
4. The plating process of the marine environment resistant composite material plating layer according to claim 2, characterized in that the main components and contents of the nickel plating solution adopted in the alkaline nickel preplating in the second step comprise 40ml/L of alkaline nickel preplating agent A, 40ml/L of alkaline nickel preplating agent B, 80ml/L of alkaline nickel preplating agent H, and ammonia NH3·H2O10 ml/L; the pH of the nickel plating solution is 8.5-9.5, and Ni is2+The content is 4.0-6.0 g/L; wherein, the agent A is main salt, the agent B is complexing agent, and the agent H is acid replenisher.
5. The plating process of the marine environment resistant composite material plating layer according to claim 2, characterized in that the main components and contents of the high phosphorus chemical nickel plating solution in the third step comprise 60ml/L high phosphorus chemical nickel plating agent A and 150ml/L high phosphorus chemical nickel plating agent B; the pH value of the nickel plating solution is 4.5-4.8, and Ni2+The content is 5.5-6.5 g/L, and the pH value of the high-phosphorus chemical nickel plating solution is adjusted by using 50 mass percent of analytically pure ammonia water and 10 mass percent of sulfuric acid during production; adjusting the nickel ion content of the high-phosphorus chemical nickel plating solution by using a mixed solution of an agent A and an agent C in a volume ratio of 1: 1; wherein, the agent A is main salt, the agent B is complexing agent, and the agent C is acid extender.
6. The process of claim 2, wherein the plating solution for the copper pyrophosphate electroplating of the fourth step comprises Cu pyrophosphate as a main component2P2O7·3H270-85 g/L of O and potassium pyrophosphate K4P2O7260-340 g/L of ammonia water NH3·H2O3 ml/L, brightener 1ml/L, electroplating solution pH of 8.0-9.3, and cathode current density of 0.5-2A/dm2。
7. The plating process of the marine environment resistant composite material plating layer as claimed in claim 2, wherein the main components and contents of the plating solution used in the chemical polishing in the fifth step include additive A150ml/L, additive B75 ml/L, and hydrogen peroxide H with the mass fraction of 50%2O2 100ml/L。
8. The process according to claim 2, wherein the plating solution for plating the low-stress nickel in the sixth step comprises NiSO as a main component4·6H2O 240～330g/L、NiCl2·6H220-30 g/L of O and H of boric acid3BO335-45 g/L of anode activator, 12ml/L of wetting agent and 12ml/L of extender; the pH of the electroplating solution is 3.8-4.8, and the cathode current density is 1-2A/dm2。
9. The plating process of the marine environment resistant composite material plating layer according to claim 2, characterized in that the main components and contents of the high phosphorus chemical nickel plating solution in the seventh step include 60ml/L of high phosphorus chemical nickel plating A agent and 150ml/L of high phosphorus chemical nickel plating B agent; the pH value of the nickel plating solution is 4.5-4.8, and Ni2+The content is 5.5-6.5 g/L, and the pH value of the high-phosphorus chemical nickel plating solution is adjusted by using 50 mass percent of analytically pure ammonia water and 10 mass percent of sulfuric acid during production; adjusting the nickel ion content of the high-phosphorus chemical nickel plating solution by using a mixed solution of an agent A and an agent C in a volume ratio of 1: 1; wherein, the agent A is main salt, the agent B is complexing agent, and the agent C is acid extender.
10. A process for coating a marine environment resistant composite coating according to claim 2, wherein the chemical passivation in step eight comprises the following agents in amounts and concentrations including potassium dichromate K2Cr2O7 40～50g/L。
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| CN116462531A (en) * | 2023-03-21 | 2023-07-21 | 沈阳富创精密设备股份有限公司 | Ceramic surface treatment method |
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