CN111910179A - Method for plating Ni-P film on surface of SiCp/Al composite material - Google Patents
Method for plating Ni-P film on surface of SiCp/Al composite material Download PDFInfo
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- CN111910179A CN111910179A CN202010730093.9A CN202010730093A CN111910179A CN 111910179 A CN111910179 A CN 111910179A CN 202010730093 A CN202010730093 A CN 202010730093A CN 111910179 A CN111910179 A CN 111910179A
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- zinc dipping
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- 238000007747 plating Methods 0.000 title claims abstract description 121
- 238000000034 method Methods 0.000 title claims abstract description 54
- 239000002131 composite material Substances 0.000 title claims abstract description 28
- 229910018104 Ni-P Inorganic materials 0.000 title claims abstract description 24
- 229910018536 Ni—P Inorganic materials 0.000 title claims abstract description 24
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 150
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 74
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 74
- 239000011701 zinc Substances 0.000 claims abstract description 74
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 73
- 238000007598 dipping method Methods 0.000 claims abstract description 61
- 239000000463 material Substances 0.000 claims abstract description 46
- 238000005530 etching Methods 0.000 claims abstract description 26
- 230000002378 acidificating effect Effects 0.000 claims abstract description 22
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 14
- 238000004140 cleaning Methods 0.000 claims abstract description 13
- 238000000605 extraction Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 71
- 229910001868 water Inorganic materials 0.000 claims description 51
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- 239000011159 matrix material Substances 0.000 claims description 35
- 238000006243 chemical reaction Methods 0.000 claims description 33
- 239000008367 deionised water Substances 0.000 claims description 20
- 229910021641 deionized water Inorganic materials 0.000 claims description 20
- 229910045601 alloy Inorganic materials 0.000 claims description 15
- 239000000956 alloy Substances 0.000 claims description 15
- 230000035484 reaction time Effects 0.000 claims description 14
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 13
- 229910017604 nitric acid Inorganic materials 0.000 claims description 13
- 239000008139 complexing agent Substances 0.000 claims description 11
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 11
- 229910021205 NaH2PO2 Inorganic materials 0.000 claims description 10
- 238000005282 brightening Methods 0.000 claims description 8
- 239000003638 chemical reducing agent Substances 0.000 claims description 8
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 7
- OFNHPGDEEMZPFG-UHFFFAOYSA-N phosphanylidynenickel Chemical compound [P].[Ni] OFNHPGDEEMZPFG-UHFFFAOYSA-N 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 5
- 238000011068 loading method Methods 0.000 claims description 5
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 claims description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 244000137852 Petrea volubilis Species 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- 238000003754 machining Methods 0.000 claims description 2
- 230000003287 optical effect Effects 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 2
- 239000001488 sodium phosphate Substances 0.000 claims description 2
- 239000002904 solvent Substances 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
- 239000000758 substrate Substances 0.000 abstract description 37
- 238000005498 polishing Methods 0.000 abstract description 13
- 239000002253 acid Substances 0.000 abstract description 11
- 238000000576 coating method Methods 0.000 abstract description 8
- 239000011248 coating agent Substances 0.000 abstract description 7
- 239000007788 liquid Substances 0.000 abstract description 5
- 238000001035 drying Methods 0.000 abstract description 4
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 4
- 150000002500 ions Chemical class 0.000 abstract description 4
- IJRVLVIFMRWJRQ-UHFFFAOYSA-N nitric acid zinc Chemical compound [Zn].O[N+]([O-])=O IJRVLVIFMRWJRQ-UHFFFAOYSA-N 0.000 abstract description 4
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 238000001994 activation Methods 0.000 abstract description 2
- 238000004065 wastewater treatment Methods 0.000 abstract description 2
- 239000003921 oil Substances 0.000 description 22
- 229910052782 aluminium Inorganic materials 0.000 description 21
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 21
- 239000002585 base Substances 0.000 description 21
- 239000000126 substance Substances 0.000 description 18
- 230000008569 process Effects 0.000 description 17
- 238000005406 washing Methods 0.000 description 14
- 229910000838 Al alloy Inorganic materials 0.000 description 12
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 10
- 239000003513 alkali Substances 0.000 description 10
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 10
- 239000001257 hydrogen Substances 0.000 description 9
- 229910052739 hydrogen Inorganic materials 0.000 description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 7
- 238000009713 electroplating Methods 0.000 description 7
- 239000012535 impurity Substances 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- 229910052593 corundum Inorganic materials 0.000 description 6
- 229910001845 yogo sapphire Inorganic materials 0.000 description 6
- 238000001755 magnetron sputter deposition Methods 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- -1 hydrogen ions Chemical class 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical compound [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 description 4
- 229910001096 P alloy Inorganic materials 0.000 description 3
- 239000003518 caustics Substances 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 238000007654 immersion Methods 0.000 description 3
- 229910001453 nickel ion Inorganic materials 0.000 description 3
- 229910052755 nonmetal Inorganic materials 0.000 description 3
- 239000003755 preservative agent Substances 0.000 description 3
- 230000002335 preservative effect Effects 0.000 description 3
- 238000010405 reoxidation reaction Methods 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 238000012876 topography Methods 0.000 description 3
- 229910000406 trisodium phosphate Inorganic materials 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 239000013077 target material Substances 0.000 description 2
- QTZURURAKNSDHT-UHFFFAOYSA-K 2-hydroxypropane-1,2,3-tricarboxylate;nickel(3+) Chemical compound [Ni+3].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QTZURURAKNSDHT-UHFFFAOYSA-K 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- HZUJFPFEXQTAEL-UHFFFAOYSA-N azanylidynenickel Chemical compound [N].[Ni] HZUJFPFEXQTAEL-UHFFFAOYSA-N 0.000 description 1
- QDWJUBJKEHXSMT-UHFFFAOYSA-N boranylidynenickel Chemical compound [Ni]#B QDWJUBJKEHXSMT-UHFFFAOYSA-N 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000000724 energy-dispersive X-ray spectrum Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000002815 nickel Chemical class 0.000 description 1
- 229940078494 nickel acetate Drugs 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- DITXJPASYXFQAS-UHFFFAOYSA-N nickel;sulfamic acid Chemical compound [Ni].NS(O)(=O)=O DITXJPASYXFQAS-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- WWNBZGLDODTKEM-UHFFFAOYSA-N sulfanylidenenickel Chemical compound [Ni]=S WWNBZGLDODTKEM-UHFFFAOYSA-N 0.000 description 1
- 229910052717 sulfur Inorganic materials 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
- 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
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
-
- 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
- C23C18/52—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 using reducing agents for coating with metallic material not provided for in a single one of groups C23C18/32 - C23C18/50
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- 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)
- Electroplating Methods And Accessories (AREA)
- Chemically Coating (AREA)
Abstract
The invention relates to a method for plating a thick Ni-P film on the surface of a SiCp/Al composite material, which specifically comprises the following steps: conventional polishing of the SiCp/Al composite material → ultrasonic cleaning → oil removal, alkaline etching → light extraction → primary zinc dipping → nitric acid zinc removal → secondary zinc dipping → alkaline pre-plating → acid nickel plating → cleaning → drying. The invention aims to plate a thick amorphous Ni-P film on the surface of a SiCp/Al composite material so as to obtain high surface smoothness and improve the polishing property of the SiCp/Al composite material. After pretreatment, the substrate is subjected to secondary zinc dipping treatment in zinc dipping liquid with small concentration, so that the SiCp/Al substrate material and the coating can be better combined, and Pb is not used+、Hg2+、Ti+、Cd+And the activation process containing heavy metal ions reduces the pollution of waste water treatment to the environment. The zinc dipping solution used in the invention,Compared with other plating solutions, the alkaline nickel pre-plating solution and the acidic nickel plating solution have the advantages of less reagent, low concentration, less environmental pollution, faster plating speed, uniform plating layer, good density and ideal thickness.
Description
Technical Field
The invention belongs to the technical field of preparation of composite material coating films, and particularly relates to a method for plating a Ni-P film on the surface of a SiCp/Al composite material.
Background
The silicon carbide particle reinforced aluminum matrix (SiCp/Al) composite material has excellent performances of high compactness, high electric and thermal conductivity, low expansibility, light weight, low thermal expansion coefficient and the like, and has wide application prospect in the field of space light reflectors. However, the aluminum matrix composite has a polycrystalline structure, and the high surface smoothness obtained by the aluminum matrix composite is influenced by the anisotropy of crystals, grain boundaries and impurities in the processing process, so that the specular reflection capability is reduced. An effective method is to form a layer of amorphous substance on the surface of SiCp/Al composite material, the amorphous substance can eliminate the influence of the polycrystalline structure, obtain high surface smoothness, improve the polishing performance, and lay the foundation for completing silver plating or copper film of the reflector in the next step.
At present, there are various methods for plating Ni-P film, including electroplating method, magnetron sputtering method, chemical plating method, etc. The electroplating method is a process of depositing metal nickel on a base material at a cathode by utilizing an electrochemical principle and carrying out electrochemical reaction between a cathode and an anode in an electrolytic cell.
At the anode, hypophosphite is oxidized to release electrons, and hypophosphite and hydrogen ions are generated:
H2PO2 -+H2O→H2PO3 -+2H++2e Ea 0＝-0.5V
at the cathode, nickel ions get electrons to be reduced into metallic nickel, and hydrogen ions and hypophosphite get electrons to be reduced into hydrogen and phosphorus:
Ni2++2e→Ni Ea 0＝-0.25V
2H++2e→H2 Ea 0＝0V
H2PO2 -+2H++e→2H2O+P Ea 0＝-0.25V
the electroplating process comprises watt nickel, citrate nickel plating, sulfamic acid nickel plating, full gloss nickel plating, high sulfur nickel plating and the like. The electroplating method has high reaction speed, but has the defects that the nickel plating layer belongs to a cathode plating layer, the porosity is high, and the pH, the temperature, the current density, the electrolyte component, the current efficiency and the like of the electroplating solution can have great influence on the performance of the plating layer. In addition, the uniformity of the plating layer is poor, the internal stress is unstable, and the change is large, so that the service performance of the product is influenced.
The magnetron sputtering method belongs to a physical vapor deposition method, which is characterized in that a pre-deposited material is made into a plate-target and fixed on a cathode, a substrate material is placed on an anode opposite to a target surface, a certain distance is reserved between the plate-target and the target material, the system is filled with 1-10 Pa inert gas argon as a carrier of gas discharge in a high vacuum environment, a voltage of thousands of volts is added between the cathode and the anode, plasma glow discharge is generated between the cathode and the anode, the argon is ionized into argon ions by the discharge, the argon ions fly to the cathode under the action of a strong electric field and bombard atoms on the surface of the target, the atoms on the surface of the target material are sputtered from the target surface by collision to deposit on the surface of the substrate to form a film, and the energy of the film is in the range of one to tens. The magnetron sputtering method has high sputtering rate, good film-base binding force and uniform and compact plating layer. But the cost is high, and the method is only suitable for film deposition and surface coating preparation and is not suitable for preparing thick coatings.
The electroless nickel plating method is a process of reducing nickel ions in a nickel salt (nickel sulfate, nickel acetate, nickel chloride) solution to metallic nickel by using a strong reducing agent (hypophosphite, hydrazine, borohydride and derivatives thereof), and simultaneously, phosphorus, nitrogen, boron and the like in the strong reducing agent are simultaneously separated out from the nickel, so that alloy plating layers of nickel-phosphorus, nickel-nitrogen, nickel-boron and the like are obtained. Wherein the reduction reaction formula of the nickel ions is as follows:
Ni·Cm 2++R→Ni+mC+O
in the reaction formula, C is a complex, m is the amount of a complexing agent, R is a reducing agent, and O is an oxide.
The chemical nickel plating method has simple equipment requirement, low cost and no need of power supplyEquipment, the plating layer tissue is uniform. However, the chemical plating often results in poor binding force between the substrate and the plating layer, unstable plating solution and S, Pb in the plating solution+、Hg2+、Ti+、Cd+The heavy metal ions bring difficulty to the sewage treatment.
With the improvement of the industrialization degree in the 21 st century, the environmental problems become more serious, the sustainable development of human beings is restricted, and the focus of attention of people is formed. Against this background, reducing the pollution source of chemical production is the leading research direction of green chemistry today.
Disclosure of Invention
The invention aims to provide a method for plating a thick Ni-P film on the surface of a SiCp/Al composite material, which aims to solve the problems of more plating solution components, high concentration, instability, easy environmental pollution of heavy metal ions and poor binding force in the prior art.
In order to achieve the aim of the invention, the invention provides a method for plating a thick Ni-P film on the surface of a SiCp/Al composite material, which comprises the following steps:
step one, pretreating a SiCp/Al matrix material: including sanding, ultrasonic cleaning, degreasing and alkaline etching.
Step two, using HNO for SiCp/Al matrix material3、HF、H2And (4) performing light extraction treatment on the solution prepared from the O.
Step three, carrying out primary zinc dipping treatment on the SiCp/Al base material, wherein the primary zinc dipping solution is prepared from the following components in percentage by weight: 20-30 g/L ZnO, 100-120 g/L NaOH, 50-60 g/L KNaC4H4O6·4H2O, 1-2 g/L FeCl3。
Step four, using HNO for SiCp/Al base material3、H2And (4) carrying out zinc removing treatment on the solution prepared from the O.
Step five, using ZnO, NaOH and KNaC as the SiCp/Al matrix material4H4O6·4H2O、FeCl3The solution is subjected to secondary zinc dipping treatment.
Sixthly, carrying out alkaline nickel preplating treatment on the SiCp/Al base material, wherein the solution ratio of the alkaline nickel preplating is as follows: NiSO4Is 25 &30g/L，NaH2PO225 to 30g/L of Na4P2O7·10H2O is 50-60 g/L and NH is used3·H2Adjusting the pH value to 9-11 by O, controlling the reaction temperature to 45 ℃ and controlling the reaction time to 5 min.
Seventhly, carrying out acidic nickel pre-plating treatment on the SiCp/Al base material, wherein the solution ratio of acidic nickel plating is as follows: NiSO420 to 30g/L, a reducing agent NaH2PO225-35 g/L of complexing agent C3H6O310-20 mL/L of complexing agent C6H8O7·H2O is 10-20 g/L, and a buffer CH3COONa is 10-20 g/L, an accelerator NaF is 1-2 g/L, the pH value is adjusted to 4.5-4.6 by NH3 & H2O, the loading capacity is about 1dm2/L, the reaction temperature is 88 ℃, the reaction time is 6-12H, the plating solution is changed every 1H, alloy nickel-phosphorus is deposited on the surface of a plated part, and the plating layer is gradually thickened along with the time extension so as to obtain the thick Ni-P alloy plating layer which meets the optical precision machining requirement and is between 80 and 140 mu m.
In the first step, the types of the used sand paper are as follows: 120#, 240#, 600#, 1000#, 1500 #; the solvents for ultrasonic cleaning were: absolute ethyl alcohol, and the cleaning time is 10 min; solution proportioning for oil removal and alkaline etching: 20g/L of sodium carbonate, 30g/L of sodium phosphate, 5g/L of sodium hydroxide, 50 ℃ of reaction temperature and 3-5 min of reaction time.
In the second step, the used brightening liquid is HNO3:HF:H2O is 3:1:1, and the reaction time is 3-5 s.
In the third step, the first zinc dipping solution is carried out at room temperature, and the reaction time is 50-60 s.
In the fourth step, the dezincification liquid is HNO3:H2O is 1:1, and the reaction time is 3-5 s.
In the fifth step, the concentration of the secondary zinc dipping solution is the same as that of the primary zinc dipping solution, and the reaction time is 20-30 s at room temperature.
Cleaning steps are added among the steps, and the cleaning step is to clean the SiCp/Al matrix material by adopting deionized water and then carry out the next step operation.
Compared with the prior art, the invention has the advantages that:
the invention aims to plate a thick amorphous Ni-P film on the surface of the SiCp/Al composite material to obtain high surface smoothness and improve the polishing property of the SiCp/Al composite material, and lays a foundation for finishing the silver plating or copper film of a reflector in the next step. After pretreatment, the substrate is subjected to secondary zinc dipping treatment in zinc dipping liquid with small concentration, so that the SiCp/Al substrate material and the coating can be better combined, and Pb is not used+、Hg2+、Ti+、Cd+And the activation process containing heavy metal ions reduces the pollution of waste water treatment to the environment. Compared with other plating solutions, the zinc dipping solution, the alkaline pre-plating nickel solution and the acidic nickel plating solution used in the invention have the advantages of less reagent, low concentration, less environmental pollution, faster plating speed, uniform plating layer, good density and ideal thickness.
Drawings
FIG. 1 is a schematic view of an electroplating process.
FIG. 2 is a schematic view of a magnetron sputtering method.
FIG. 3 is a schematic diagram of an electroless acidic nickel plating process.
FIG. 4 is an SEM image of the thickness of the electroless nickel 12hNi-P film after pretreatment by zincing, wherein a and b are the thickness of the film of example 1, c and d are the thickness of the film of example 2, and e and f are the thickness of the film of example 3, and the lower right corner of the image is a 100 μm scale.
FIG. 5 is an SEM image of the surface of the electroless nickel 12hNi-P film after pretreatment by zincing, wherein a and b are surface topography images of the substrate of example 1, c and d are surface topography images of the substrate of example 2, and the lower right corner of the images is a 100 μm scale.
Figure 6 is an XRD diffractogram of the electroless acidic nickel plated 12hNi-P film layer after pretreatment by zincing.
Figure 7 is an EDS energy spectrum of an electroless acidic nickel plated 12hNi-P film layer after pretreatment by zincing.
Detailed Description
The present invention will be described in further detail with reference to the following detailed description and accompanying drawings.
The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
Example 1:
a method for plating a thick Ni-P film on the surface of a SiCp/Al composite material specifically comprises the following steps:
conventional polishing of the SiCp/Al composite material → ultrasonic cleaning → oil removal, alkaline etching → light extraction → primary zinc dipping → nitric acid zinc removal → secondary zinc dipping → alkaline pre-plating → acid nickel plating → cleaning → drying.
(1) Matrix pretreatment: polishing, ultrasonic cleaning, oil removal and alkaline etching. Aluminum alloy No. 120, No. 240, No. 600, No. 1000 and No. 1500 which are 10mm multiplied by 3mm are sanded, and then are put into absolute ethyl alcohol solution for ultrasonic cleaning for 10min, so that impurities, oil stains and the like carried by the surface of the material due to polishing are removed. According to NaCO3Is 20g/L, Na3PO430g/L and 5g/L NaOH, preparing an alkali etching and oil removing solution, and reacting at 50 ℃ for 5 min. Further removing various alloy elements and inclusions on the surface of the SiCp/Al composite material to form an aluminum-rich surface, wherein the chemical reaction generated in the alkaline etching process is as follows:
Al2O3+2NaOH＝2NaAlO2+H2O
2Al+2NaOH+2H2O＝2NaAlO2+3H2↑
hydrogen is generated in the reaction process, the reaction is violent, and the hydrogen can promote non-soluble substances to leave the surface of the aluminum alloy, so that the base material is purified. And (3) taking out the substrate material by using tweezers after the reaction is finished, washing the surface of the substrate material to be black, and cleaning the alkaline etching solution by using deionized water.
(2) Light emission: preparation of HNO3:HF:H2O is 3:1: 1. Clamping the base material subjected to oil removal and alkaline etching by using tweezers, quickly putting the base material into a brightening solution for brightening, immediately taking out the base material after the surface of the base material is whitened for about 3s, and then taking out the base material by using the tweezers and then washing the base material by using deionized water. The light emission can remove certain metal or non-metal impurities which can not be removed in the oil removal and alkali corrosion processes on the surface of the aluminum alloy, and simultaneously remove black corrosive substances generated in the alkali corrosion and oil removal processes, so that the matrix is brighter and activeThe matrix is changed to improve the binding force.
(3) Primary zinc dipping: according to 20g/L ZnO, 120g/L NaOH and KNaC4H4O6·4H2O is 50g/L, FeCl3Preparing zinc dipping solution with the concentration ratio of 2 g/L. The prepared zinc dipping solution is divided into two parts, one part is used as the primary zinc dipping solution, and the other part is used as the secondary zinc dipping solution. And (3) quickly putting the bright substrate into a primary zinc dipping solution, reacting for 50s at room temperature, taking out the substrate by using tweezers, and washing the substrate by using deionized water, wherein the surface of the substrate is gray. Because the aluminum in the aluminum alloy matrix can immediately form an oxide film after encountering oxygen, the alloy can effectively remove the oxide film on the surface in the zinc dipping solution, and can deposit a zinc layer to prevent the reoxidation of the aluminum, thereby improving the binding force of a subsequent coating and the aluminum matrix.
(4) Zinc stripping by nitric acid: with HNO3:H2And (3) carrying out dezincification treatment on the matrix after the zinc is immersed by the dezincification solution with the ratio of O to 1:1 for about 3s, forming a black film on the surface of the matrix material, taking out the black film by using tweezers, and then washing the black film by using deionized water.
(5) Secondary zinc dipping: the same immersion zinc solution is reacted for 20s at room temperature, and the surface of the substrate is gray. The secondary zinc dipping layer is thinner, more compact and more uniform than the primary zinc dipping layer and is in a fine honeycomb net shape, so that a compact and uniform plating layer is deposited on the aluminum substrate by the subsequent chemical nickel-phosphorus alloy plating. The chemical reactions that occur during zincing are as follows:
2NaOH+ZnO＝Na2ZnO2+H2O
2NaOH+Al2O3＝2NaAlO2+H2O
3Na2ZnO2+2Al+2H2O＝3Zn↓+2NaAlO2+4NaOH
2Al+2NaOH+2H2O＝2NaAlO2+3H2↑
(6) alkaline nickel preplating: according to NiSO4Is 25g/L, NaH2PO2Is 25g/L, Na4P2O7·10H2And O is in a concentration ratio of 50g/L, and alkaline nickel pre-plating solution is prepared. By NH3·H2Blend of oxygen and sulfurAnd (3) setting the pH value of the nickel pre-plating solution to be 10, putting the substrate material subjected to secondary zinc dipping into a beaker filled with the nickel pre-plating solution, putting the beaker into a constant-temperature water bath kettle at 45 ℃, carrying out alkaline nickel pre-plating treatment for 5min, taking out the beaker with tweezers, and then washing the beaker with deionized water. The purpose of the nickel preplating is to improve the bonding force between the chemical nickel plating layer and the aluminum matrix alloy. The chemical reactions that take place in the alkaline pre-nickel plating solution are as follows:
Ni2++H2PO2 -+2OH-→Ni+H2PO3 -+H2O
H2PO2 -+H2O→H2PO3 -+H2↑
H2PO2 -+H+→P+H2O+H2PO3 -
(7) acid chemical nickel plating: according to the main salt NiSO425g/L, reducing agent NaH2PO230g/L of complexing agent C3H6O320mL/L, complexing agent C6H8O7·H2O is 10g/L, buffer CH3COONa 15g/L, accelerator NaF 1g/L, and prepared with a loading (ratio of surface area of workpiece immersed in plating solution to volume of plating solution) of about 1dm2Acid nickel plating solution of/L, using NH3·H2O adjusted pH 4.5. The basic material which is subjected to alkaline pre-nickel plating is washed clean by deionized water and then is quickly placed into a small beaker filled with acidic nickel plating solution, the opening of the beaker is wrapped by a preservative film and is placed into a constant-temperature water bath kettle at 88 ℃ for reaction for 12 hours, and the acidic plating solution is changed once every 1 hour by the same method. The chemical reactions that take place in the acidic nickel plating solution are as follows:
Ni2++H2PO2 -+H2O→Ni+H2PO3 -+2H+
H2PO2 -+H2O→H2PO3 -+H2↑
H2PO2 -+H+→P+H2O+H2PO3 -
after the reaction of the acidic nickel plating solution for 12 hours, a silvery white Ni-P plating layer with the thickness of about 140 mu m can be finally obtained. The average plating rate was about 12 μm/h.
Example 2:
a method for plating a thick Ni-P film on the surface of a SiCp/Al composite material specifically comprises the following steps:
conventional polishing of the SiCp/Al composite material → ultrasonic cleaning → oil removal, alkaline etching → light extraction → primary zinc dipping → nitric acid zinc removal → secondary zinc dipping → alkaline pre-plating → acid nickel plating → cleaning → drying.
(1) Matrix pretreatment: polishing, ultrasonic cleaning, oil removal and alkaline etching. Aluminum alloy No. 120, No. 240, No. 600, No. 1000 and No. 1500 which are 10mm multiplied by 3mm are sanded, and then are put into absolute ethyl alcohol solution for ultrasonic cleaning for 10min, so that impurities, oil stains and the like carried by the surface of the material due to polishing are removed. According to NaCO3Is 20g/L, Na3PO430g/L and 5g/L NaOH, preparing an alkali etching and oil removing solution, and reacting at 50 ℃ for 5 min. Further removing various alloy elements and inclusions on the surface of the SiCp/Al composite material to form an aluminum-rich surface, wherein the chemical reaction generated in the alkaline etching process is as follows:
Al2O3+2NaOH＝2NaAlO2+H2O
2Al+2NaOH+2H2O＝2NaAlO2+3H2↑
hydrogen is generated in the reaction process, the reaction is violent, and the hydrogen can promote non-soluble substances to leave the surface of the aluminum alloy, so that the base material is purified. And (3) taking out the substrate material by using tweezers after the reaction is finished, washing the surface of the substrate material to be black, and cleaning the alkaline etching solution by using deionized water.
(2) Light emission: preparation of HNO3:HF:H2O is 3:1: 1. Clamping the base material subjected to oil removal and alkaline etching by using tweezers, quickly putting the base material into a brightening solution for brightening, immediately taking out the base material after the surface of the base material is whitened for about 3s, and then taking out the base material by using the tweezers and then washing the base material by using deionized water. Aluminum alloy can be removed by light extractionThe method has the advantages that certain metal or nonmetal impurities which cannot be removed in the oil removing and alkali etching processes on the gold surface are removed, black corrosive substances generated in the alkali etching and oil removing processes are removed, a matrix is brighter, and the matrix is activated to improve the binding force.
(3) Primary zinc dipping: according to 20g/L ZnO, 120g/L NaOH and KNaC4H4O6·4H2O is 50g/L, FeCl3Preparing zinc dipping solution with the concentration ratio of 2 g/L. The prepared zinc dipping solution is divided into two parts, one part is used as the primary zinc dipping solution, and the other part is used as the secondary zinc dipping solution. And (3) quickly putting the bright substrate into a primary zinc dipping solution, reacting for 60s at room temperature, taking out the substrate by using tweezers, and washing the substrate by using deionized water, wherein the surface of the substrate is gray. Because the aluminum in the aluminum alloy matrix can immediately form an oxide film after encountering oxygen, the alloy can effectively remove the oxide film on the surface in the zinc dipping solution, and can deposit a zinc layer to prevent the reoxidation of the aluminum, thereby improving the binding force of a subsequent coating and the aluminum matrix.
(4) Zinc stripping by nitric acid: with HNO3:H2And (3) carrying out dezincification treatment on the matrix after the zinc is immersed by the dezincification solution with the ratio of O to 1:1 for about 5s, forming a black film on the surface of the matrix material, taking out the black film by using tweezers, and then washing the black film by using deionized water.
(5) Secondary zinc dipping: the same immersion zinc solution is reacted for 30s at room temperature, and the surface of the substrate is gray. The secondary zinc dipping layer is thinner, more compact and more uniform than the primary zinc dipping layer and is in a fine honeycomb net shape, so that a compact and uniform plating layer is deposited on the aluminum substrate by the subsequent chemical nickel-phosphorus alloy plating. The chemical reactions that occur during zincing are as follows:
2NaOH+ZnO＝Na2ZnO2+H2O
2NaOH+Al2O3＝2NaAlO2+H2O
3Na2ZnO2+2Al+2H2O＝3Zn↓+2NaAlO2+4NaOH
2Al+2NaOH+2H2O＝2NaAlO2+3H2↑
(6) alkaline nickel preplating: according to NiSO430g/L of NaH2PO2Is 30g/L, Na4P2O7·10H2And O is in a concentration ratio of 60g/L, and alkaline nickel pre-plating solution is prepared. By NH3·H2Adjusting the pH value of the nickel pre-plating solution to be about 10 by O, putting the substrate material subjected to secondary zinc dipping into a beaker filled with the nickel pre-plating solution, putting the beaker into a constant-temperature water bath kettle at 45 ℃, carrying out alkaline nickel pre-plating treatment for 5min, taking out the beaker by using tweezers, and then washing the beaker by using deionized water. The purpose of the nickel preplating is to improve the bonding force between the chemical nickel plating layer and the aluminum matrix alloy. The chemical reactions that take place in the alkaline pre-nickel plating solution are as follows:
Ni2++H2PO2 -+2OH-→Ni+H2PO3 -+H2O
H2PO2 -+H2O→H2PO3 -+H2↑
H2PO2 -+H+→P+H2O+H2PO3 -
(7) acid chemical nickel plating: according to the main salt NiSO420g/L, reducing agent NaH2PO225g/L of complexing agent C3H6O325mL/L of complexing agent C6H8O7·H2O is 10g/L, buffer CH3COONa 15g/L, accelerator NaF 1g/L, and prepared with a loading (ratio of surface area of workpiece immersed in plating solution to volume of plating solution) of about 1dm2Acid nickel plating solution of/L, using NH3·H2O adjusted pH 4.6. The basic material which is subjected to alkaline pre-nickel plating is washed clean by deionized water and then is quickly placed into a small beaker filled with acidic nickel plating solution, the opening of the beaker is wrapped by a preservative film and is placed into a constant-temperature water bath kettle at 88 ℃ for reaction for 12 hours, and the acidic plating solution is changed once every 1 hour by the same method. The chemical reactions that take place in the acidic nickel plating solution are as follows:
Ni2++H2PO2 -+H2O→Ni+H2PO3 -+2H+
H2PO2 -+H2O→H2PO3 -+H2↑
H2PO2 -+H+→P+H2O+H2PO3 -
after the reaction of the acidic nickel plating solution for 12 hours, a silvery white Ni-P plating layer with the thickness of about 130 mu m can be finally obtained. The average plating rate was 11 μm/h.
Example 3:
a method for plating a thick Ni-P film on the surface of a SiCp/Al composite material specifically comprises the following steps:
conventional polishing of the SiCp/Al composite material → ultrasonic cleaning → oil removal, alkaline etching → light extraction → primary zinc dipping → nitric acid zinc removal → secondary zinc dipping → alkaline pre-plating → acid nickel plating → cleaning → drying.
(1) Matrix pretreatment: polishing, ultrasonic cleaning, oil removal and alkaline etching. Aluminum alloy No. 120, No. 240, No. 600, No. 1000 and No. 1500 which are 10mm multiplied by 3mm are sanded, and then are put into absolute ethyl alcohol solution for ultrasonic cleaning for 10min, so that impurities, oil stains and the like carried by the surface of the material due to polishing are removed. According to NaCO3Is 20g/L, Na3PO430g/L and 5g/L NaOH, preparing an alkali etching and oil removing solution, and reacting at 50 ℃ for 5 min. Further removing various alloy elements and inclusions on the surface of the SiCp/Al composite material to form an aluminum-rich surface, wherein the chemical reaction generated in the alkaline etching process is as follows:
Al2O3+2NaOH＝2NaAlO2+H2O
2Al+2NaOH+2H2O＝2NaAlO2+3H2↑
hydrogen is generated in the reaction process, the reaction is violent, and the hydrogen can promote non-soluble substances to leave the surface of the aluminum alloy, so that the base material is purified. And (3) taking out the substrate material by using tweezers after the reaction is finished, washing the surface of the substrate material to be black, and cleaning the alkaline etching solution by using deionized water.
(2) Light emission: preparation of HNO3:HF:H2O is 3:1: 1. Removing oil and alkali corrosion on the base materialThe material is clamped by tweezers and is rapidly put into the brightening liquid for brightening, the material is taken out immediately after the surface of the substrate becomes white, the time is about 3s, and the material is taken out by the tweezers and is washed clean by deionized water. The bright dipping can remove some metal or non-metal impurities on the surface of the aluminum alloy which can not be removed in the oil and alkali etching processes, and simultaneously remove black corrosive substances generated in the alkali etching and oil removing processes, so that the matrix is brighter, and simultaneously, the matrix is activated to improve the binding force.
(3) Primary zinc dipping: according to 20g/L ZnO, 120g/L NaOH and KNaC4H4O6·4H2O is 50g/L, FeCl3Preparing zinc dipping solution with the concentration ratio of 2 g/L. The prepared zinc dipping solution is divided into two parts, one part is used as the primary zinc dipping solution, and the other part is used as the secondary zinc dipping solution. And (3) quickly putting the bright substrate into a primary zinc dipping solution, reacting for 50s at room temperature, taking out the substrate by using tweezers, and washing the substrate by using deionized water, wherein the surface of the substrate is gray. Because the aluminum in the aluminum alloy matrix can immediately form an oxide film after encountering oxygen, the alloy can effectively remove the oxide film on the surface in the zinc dipping solution, and can deposit a zinc layer to prevent the reoxidation of the aluminum, thereby improving the binding force of a subsequent coating and the aluminum matrix.
(4) Zinc stripping by nitric acid: with HNO3:H2And (3) carrying out dezincification treatment on the matrix after the zinc is immersed by the dezincification solution with the ratio of O to 1:1 for about 3s, forming a black film on the surface of the matrix material, taking out the black film by using tweezers, and then washing the black film by using deionized water.
(5) Secondary zinc dipping: the same immersion zinc solution is reacted for 20s at room temperature, and the surface of the substrate is gray. The secondary zinc dipping layer is thinner, more compact and more uniform than the primary zinc dipping layer and is in a fine honeycomb net shape, so that a compact and uniform plating layer is deposited on the aluminum substrate by the subsequent chemical nickel-phosphorus alloy plating. The chemical reactions that occur during zincing are as follows:
2NaOH+ZnO＝Na2ZnO2+H2O
2NaOH+Al2O3＝2NaAlO2+H2O
3Na2ZnO2+2Al+2H2O＝3Zn↓+2NaAlO2+4NaOH
2Al+2NaOH+2H2O＝2NaAlO2+3H2↑
(6) alkaline nickel preplating: according to NiSO4Is 25g/L, NaH2PO2Is 25g/L, Na4P2O7·10H2And O is in a concentration ratio of 50g/L, and alkaline nickel pre-plating solution is prepared. By NH3·H2Adjusting the pH value of the nickel pre-plating solution to be about 10 by O, putting the substrate material subjected to secondary zinc dipping into a beaker filled with the nickel pre-plating solution, putting the beaker into a constant-temperature water bath kettle at 45 ℃, carrying out alkaline nickel pre-plating treatment for 5min, taking out the beaker by using tweezers, and then washing the beaker by using deionized water. The purpose of the nickel preplating is to improve the bonding force between the chemical nickel plating layer and the aluminum matrix alloy. The chemical reactions that take place in the alkaline pre-nickel plating solution are as follows:
Ni2++H2PO2 -+2OH-→Ni+H2PO3 -+H2O
H2PO2 -+H2O→H2PO3 -+H2↑
H2PO2 -+H+→P+H2O+H2PO3 -
(7) acid chemical nickel plating: according to the main salt NiSO425g/L, reducing agent NaH2PO230g/L of complexing agent C3H6O320mL/L, complexing agent C6H8O7·H2O is 10g/L, buffer CH3COONa 15g/L, accelerator NaF 1g/L, and prepared with a loading (ratio of surface area of workpiece immersed in plating solution to volume of plating solution) of about 1dm2Acid nickel plating solution of/L, using NH3·H2O adjusted pH 4.5. The basic material which is subjected to alkaline pre-nickel plating is washed clean by deionized water and then is quickly placed into a small beaker filled with acidic nickel plating solution, the opening of the beaker is wrapped by a preservative film and is placed into a constant-temperature water bath kettle at 88 ℃ for reaction for 12 hours, and the acidic plating solution is changed once every 1 hour by the same method. The chemical reactions that take place in the acidic nickel plating solution are as follows:
Ni2++H2PO2 -+H2O→Ni+H2PO3 -+2H+
H2PO2 -+H2O→H2PO3 -+H2↑
H2PO2 -+H+→P+H2O+H2PO3 -
and reacting for 6 hours by using an acidic nickel plating solution to finally obtain a silvery white Ni-P plating layer with the thickness of about 75-87 microns. The average plating rate was about 13 μm/h.
And (4) analyzing results: as can be seen from the process diagram of FIG. 3, the chemical acidic nickel plating experimental apparatus of FIG. 3 is compared with the electroplating method of FIG. 1 and the magnetron sputtering method of FIG. 2.
And (4) analyzing results: as can be seen from the SEM image of the Ni-P film thickness in FIG. 4, after the SiCp/Al composite material is treated by the processes of secondary zinc dipping, alkaline nickel preplating, acid nickel plating and the like for 12 hours and 6 hours, the thickness of the nickel-phosphorus film on the surface of the SiCp/Al composite material can reach 80-140 μm, the average plating speed is about 10-13 μm/h, and the film is uniformly distributed.
And (4) analyzing results: as can be seen from the SEM of the surface topography of the Ni-P film layer in FIG. 5, the film layer is tightly bonded and dense.
And (4) analyzing results: as can be seen from the XRD diffraction pattern of the surface morphology of the Ni-P film layer in FIG. 6, a very obvious broadened diffraction peak appears when the diffraction angle 2 theta is about 44-45 degrees, and the position of the amorphous Ni-P diffraction peak is analyzed, which shows that the main component of the surface of the film layer is Ni-P alloy.
And (4) analyzing results: as can be seen from the EDS spectra of the Ni-P film of fig. 7, the Ni content of the film was about 84.54% and the P content was 15.46% over the selected regions.
It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the invention and these are intended to be within the scope of the invention.
Claims (7)
1. A method for plating a Ni-P film on the surface of a SiCp/Al composite material is characterized by comprising the following steps:
step one, pretreating a SiCp/Al matrix material: the method comprises the steps of sanding with sand paper, ultrasonic cleaning, oil removal and alkaline etching;
step two, using HNO for SiCp/Al matrix material3、HF、H2Performing light extraction treatment on the solution prepared by the step O;
step three, carrying out primary zinc dipping treatment on the SiCp/Al base material, wherein the primary zinc dipping solution is prepared from the following components in percentage by weight: 20-30 g/L ZnO, 100-120 g/L NaOH, 50-60 g/L KNaC4H4O6·4H2O, 1-2 g/L FeCl3；
Step four, using HNO for SiCp/Al base material3、H2B, performing zinc removal treatment on the solution prepared from the O;
step five, using ZnO, NaOH and KNaC as the SiCp/Al matrix material4H4O6·4H2O、FeCl3Carrying out secondary zinc dipping treatment on the solution;
sixthly, carrying out alkaline nickel preplating treatment on the SiCp/Al base material, wherein the solution ratio of the alkaline nickel preplating is as follows: NiSO425 to 30g/L of NaH2PO225 to 30g/L of Na4P2O7·10H2O is 50-60 g/L and NH is used3·H2Adjusting the pH value to 9-11 by O, controlling the reaction temperature to 45 ℃ and controlling the reaction time to 5 min;
seventhly, carrying out acidic nickel pre-plating treatment on the SiCp/Al base material, wherein the solution ratio of acidic nickel plating is as follows: NiSO420 to 30g/L, a reducing agent NaH2PO225-35 g/L of complexing agent C3H6O310-20 mL/L of complexing agent C6H8O7·H2O is 10-20 g/L, and a buffer CH3COONa is 10-20 g/L, an accelerator NaF is 1-2 g/L, the pH value is adjusted to 4.5-4.6 by NH3 & H2O, the loading capacity is about 1dm2/L, the reaction temperature is 88 ℃, the reaction time is 6-12H, the plating solution is changed every 1H, alloy nickel-phosphorus is deposited on the surface of a plated part, and the plating layer is gradually thickened along with the time extension so as to obtain the thick Ni-P alloy plating layer which meets the optical precision machining requirement and is between 80 and 140 mu m.
2. The method of claim 1, wherein in step one, the sandpaper type used is: 120#, 240#, 600#, 1000#, 1500 #; the solvents for ultrasonic cleaning were: absolute ethyl alcohol, and the cleaning time is 10 min; solution proportioning for oil removal and alkaline etching: 20g/L of sodium carbonate, 30g/L of sodium phosphate, 5g/L of sodium hydroxide, 50 ℃ of reaction temperature and 3-5 min of reaction time.
3. The method according to claim 1 or 2, wherein in the second step, the brightening solution is HNO3:HF:H2O is 3:1:1, and the reaction time is 3-5 s.
4. The method as claimed in claim 3, wherein in the third step, the first zinc dipping solution is carried out at room temperature, and the reaction time is 50-60 s.
5. The method according to claim 4, wherein in the fourth step, the dezincification solution used is HNO3:H2O is 1:1, and the reaction time is 3-5 s.
6. The method as claimed in claim 5, wherein in the fifth step, the concentration of the secondary zinc dipping solution is the same as that of the primary zinc dipping solution, and the reaction time is 20-30 s at room temperature.
7. The method as claimed in claim 6, wherein a cleaning step is added between each step, and the cleaning step is performed after the SiCp/Al matrix material is cleaned by deionized water.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112663031A (en) * | 2020-12-17 | 2021-04-16 | 陕西宝成航空仪表有限责任公司 | Ultra-thick high-phosphorus chemical nickel plating and stabilizing treatment process for aluminum-based silicon carbide composite material |
| CN114150297A (en) * | 2021-10-29 | 2022-03-08 | 北京卫星制造厂有限公司 | Chemical nickel plating method for surface of high-volume aluminum-based silicon carbide composite material |
| CN114150297B (en) * | 2021-10-29 | 2023-12-12 | 北京卫星制造厂有限公司 | Surface chemical nickel plating method for high-volume aluminum-based silicon carbide composite material |
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