CN104451617A - Water-soluble nickel protective agent, preparation method thereof, chemical nickel plating method and surface nickel-plated workpiece - Google Patents
Water-soluble nickel protective agent, preparation method thereof, chemical nickel plating method and surface nickel-plated workpiece Download PDFInfo
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- CN104451617A CN104451617A CN201310438396.3A CN201310438396A CN104451617A CN 104451617 A CN104451617 A CN 104451617A CN 201310438396 A CN201310438396 A CN 201310438396A CN 104451617 A CN104451617 A CN 104451617A
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 408
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 204
- 239000003223 protective agent Substances 0.000 title claims abstract description 91
- 238000007747 plating Methods 0.000 title claims abstract description 78
- 239000000126 substance Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- FLGISLVJQPPAMV-UHFFFAOYSA-N 3-(2h-tetrazol-5-yl)aniline Chemical compound NC1=CC=CC(C2=NNN=N2)=C1 FLGISLVJQPPAMV-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000000080 wetting agent Substances 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- -1 benzo tetrazole Chemical class 0.000 claims description 19
- DBVJJBKOTRCVKF-UHFFFAOYSA-N Etidronic acid Chemical compound OP(=O)(O)C(O)(C)P(O)(O)=O DBVJJBKOTRCVKF-UHFFFAOYSA-N 0.000 claims description 14
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 14
- 239000000758 substrate Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 7
- 238000007772 electroless plating Methods 0.000 claims description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 230000004913 activation Effects 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- 238000002203 pretreatment Methods 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 238000005530 etching Methods 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 12
- 239000002184 metal Substances 0.000 abstract description 12
- 238000005260 corrosion Methods 0.000 abstract description 9
- 230000007797 corrosion Effects 0.000 abstract description 9
- 230000002209 hydrophobic effect Effects 0.000 abstract description 3
- 238000009736 wetting Methods 0.000 abstract description 3
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 230000002349 favourable effect Effects 0.000 abstract 2
- 230000001681 protective effect Effects 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 10
- 239000011248 coating agent Substances 0.000 description 9
- 238000000576 coating method Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- 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
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 101000608720 Helianthus annuus 10 kDa late embryogenesis abundant protein Proteins 0.000 description 1
- 206010023126 Jaundice Diseases 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 235000011194 food seasoning agent Nutrition 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000008233 hard water Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 150000002815 nickel Chemical class 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 229960004249 sodium acetate Drugs 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000011775 sodium fluoride Substances 0.000 description 1
- 235000013024 sodium fluoride Nutrition 0.000 description 1
- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000001384 succinic acid Substances 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—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
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/82—After-treatment
- C23C22/83—Chemical after-treatment
Landscapes
- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemically Coating (AREA)
- Preventing Corrosion Or Incrustation Of Metals (AREA)
Abstract
The invention provides a water-soluble nickel protective agent and a preparation method thereof. The water-soluble nickel protective agent is a water solution containing benzotetrazole, Dow wetting agent CF-10 and 5-(3-aminophenyl)tetrazole. The invention also provides a chemical nickel plating method and a surface nickel-plated workpiece obtained thereby. The chemical nickel plating method comprises the following steps: performing chemical nickel plating, and then performing nickel layer protective treatment by using the water-soluble nickel protective agent provided by the invention. The water-soluble nickel protective agent provided by the invention is environment-friendly, causes no pollution, can achieve a favorable adsorption and wetting hydrophobic effect on the surface of a metal nickel layer; a compact planar surface complex film is formed on the surface of the metal nickel layer, thus preventing the metal nickel layer from being directly exposed to air or other corrosion environments and preventing the nickel layer from being subjected to oxidation corrosion; and the metal nickel layer has better corrosion resistance and favorable electric conductivity at the same time.
Description
Technical field
The invention belongs to electroless plating field, the plating nickel on surface workpiece particularly relating to a kind of water-soluble nickel protective agent and preparation method thereof and a kind of chemical nickel plating method and obtained by this chemical nickel plating method.
Background technology
Nickel plating is a kind of metal protection method of a large amount of use, is divided into chemical nickel plating and electronickelling.Nickel is easy to form oxide compound and sulfide in an atmosphere, surface is jaundice easily, the nickel dam of variable color not only loses the metalluster of nickel, also can increase the contact resistance on surface, reduce nickel and other bonding force showing between coating, cause table plating exfoliation, simultaneously the oxide compound of nickel and sulfide also can reduce the welding property of nickel.
Because nickel coating is used to the protective layer of many outward appearance plating pieces; if do not carry out conservation treatment; nickel dam can react with oxygen or other etchant gases; affect plating piece outward appearance and performance, therefore seek that one does not change nickel dam outward appearance, do not affect conductivity, extends product work-ing life (salt fog performance), cheap nickel protective agent becomes the task of top priority.Now nickel protective agent is commercially oil soluble product substantially, and its essence is exactly that salt fog performance reaches requirement, but electroconductibility and welding property cannot realize, and expensive, market accepts difficulty to one deck paint on nickel dam.Some client also adopts sexavalent chrome passivation to protect, and not only effect is general, and hexavalent chromium polluted environment, does not meet European Union ROHS instruction, is prohibited use.
Summary of the invention
The invention solves the inadequate environmental protection of nickel protective agent in prior art, poor to nickel dam surface protection effect, cause the easily oxidation of nickel dam surface, reduce the technical problem of coating conductivity.
The invention provides a kind of water-soluble nickel protective agent, described water-soluble nickel protective agent is the aqueous solution containing benzo tetrazole, Tao Shi wetting agent CF-10 and 5-(3-aminophenyl) tetrazolium.
Present invention also offers the preparation method of described water-soluble nickel protective agent, comprise and benzo tetrazole, Tao Shi wetting agent CF-10 and 5-(3-aminophenyl) tetrazolium are dissolved in the water, namely obtain described water-soluble nickel protective agent.
Further, present invention also offers a kind of chemical nickel plating method, the method comprises workpiece to be plated to be placed in chemical nickel-plating liquid carries out electroless plating, obtains nickel plating part; And then nickel plating part is positioned in water-soluble nickel protective agent carries out nickel dam conservation treatment; Wherein, described water-soluble nickel protective agent is water-soluble nickel protective agent provided by the invention.
Finally, the invention provides a kind of plating nickel on surface workpiece, described plating nickel on surface workpiece comprises workpiece substrates to be plated and plating in the nickel layer on described workpiece substrates surface to be plated, and the surface of described nickel layer is also coated with nickel protection layer; Described plating nickel on surface workpiece is obtained by chemical nickel plating method provided by the invention.
Water-soluble nickel protective agent provided by the invention, by adopting the compound system of benzo tetrazole, Tao Shi wetting agent CF-10 and 5-(3-aminophenyl) tetrazolium, be chromium-free environment-friendly passivator, it has environmentally friendly, free of contamination advantage.Simultaneously; water-soluble nickel protective agent provided by the invention; good absorption and wetting hydrophobic interaction can be played on metal nickel dam surface; thus reach the object forming fine and close face type surface complexes film on metal nickel dam surface; metal nickel dam is avoided directly to be exposed in air or other corrosive environment; prevent the oxidized corrosion of nickel dam, there is better resistance to corrosion, there is good conductivity simultaneously.
Embodiment
The invention provides a kind of water-soluble nickel protective agent, described water-soluble nickel protective agent is the aqueous solution containing benzo tetrazole, Tao Shi wetting agent CF-10 and 5-(3-aminophenyl) tetrazolium.
Water-soluble nickel protective agent provided by the invention, by adopting the compound system of benzo tetrazole, Tao Shi wetting agent CF-10 and 5-(3-aminophenyl) tetrazolium, be chromium-free environment-friendly passivator, it has environmentally friendly, free of contamination advantage.
Simultaneously; water-soluble nickel protective agent provided by the invention; good absorption and wetting hydrophobic interaction can be played on metal nickel dam surface; thus reach the object forming fine and close face type surface complexes film on metal nickel dam surface; metal nickel dam is avoided directly to be exposed in air or other corrosive environment; prevent the oxidized corrosion of nickel dam, there is better resistance to corrosion, there is good conductivity simultaneously.
Particularly, in the present invention, described benzo tetrazole is organic inhibitor.Under preferable case, in described water-soluble nickel protective agent, the content of benzo tetrazole is 1-10g/L.
Described Tao Shi wetting agent CF-10 is the one low bubble class nonionogenic tenside that Dow Chemical is produced, and it has good emulsification, foaming and wet performance, and its resistance to hard water is strong, has excellent stable and dispersing property.Under preferable case, in described water-soluble nickel protective agent, the content of Tao Shi wetting agent CF-10 is 1.5-27g/L.
Described 5-(3-aminophenyl) tetrazolium is a kind of excellent tridentate ligand, its structural formula is as shown in the formula shown in I, two atom N contained by it and sulfydryl negative ion all can with the nickle atom coordination of nickel surface, form fine and close face type surface complexes film, can effectively suppress corrosive medium and nickel surface to react.Under preferable case, in described water-soluble nickel protective agent, the content of 5-(3-aminophenyl) tetrazolium is 0.5-9g/L.
In the water-soluble nickel protective agent provided of the present invention; by adopting the compound system of Tao Shi wetting agent CF-10 and 5-(3-aminophenyl) tetrazolium; contriver finds; it is more comprehensive, tight that Tao Shi wetting agent CF-10 can make 5-(3-aminophenyl) tetrazolium contact with nickle atom; namely the two is worked in coordination with and forms fine and close face type surface complexes film on nickel dam surface; namely the two has synergistic effect, is obviously better than effect when a certain component is used alone during its composite use to the protected effect of nickel.Further; contriver is by more preferably testing discovery; in described water-soluble nickel protective agent, the ratio of the weight content of described Tao Shi wetting agent CF-10 and 5-(3-aminophenyl) tetrazolium is (3 ~ 5): 1, and described water-soluble nickel protective agent is more excellent to nickel dam protected effect.
As a kind of preferred implementation of the present invention, also containing Sodium orthomolybdate in described water-soluble nickel protective agent, it act as inorganic complexing agent, can form inorganic chelate structure with the nickle atom on nickel dam surface.Under preferable case, in described water-soluble nickel protective agent, the content of Sodium orthomolybdate is 1-15g/L.
As another kind of preferred implementation of the present invention; also containing 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid in described water-soluble nickel protective agent; its structure is such as formula shown in II; its effect is similar with 5-(3-aminophenyl) tetrazolium; play coordination provide protection, but its successful is lower than 5-(3-aminophenyl) tetrazolium.Under preferable case, in described water-soluble nickel protective agent, the content of 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid is 1-8g/L.
Formula II present invention also offers the preparation method of described water-soluble nickel protective agent, comprises and benzo tetrazole, Tao Shi wetting agent CF-10 and 5-(3-aminophenyl) tetrazolium being dissolved in the water, namely obtain described water-soluble nickel protective agent.
As previously mentioned, in described water-soluble nickel protective agent, can also Sodium orthomolybdate and/or 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid being contained, therefore, when preparing described water-soluble nickel protective agent, correspondingly, also comprising step Sodium orthomolybdate and/or 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid are dissolved in the water.
Further, present invention also offers a kind of chemical nickel plating method, the method comprises workpiece to be plated to be placed in chemical nickel-plating liquid carries out electroless plating, obtains nickel plating part; And then nickel plating part is positioned in water-soluble nickel protective agent carries out nickel dam conservation treatment; Wherein, described water-soluble nickel protective agent is water-soluble nickel protective agent provided by the invention.Adopt the nickel layer after water-soluble nickel protective agent process provided by the invention to have good metalluster, and there is better resistance to corrosion.
Wherein, the chemical nickel-plating liquid adopted in plating process and chemical plating technology condition are well known to those skilled in the art, and be not particularly limited, repeat no more herein in the present invention.
The step of nickel plating part being carried out to nickel dam conservation treatment is then: directly contacted with water-soluble nickel protective agent provided by the invention by nickel plating part.Particularly, the condition of nickel dam conservation treatment comprises: the temperature of water-soluble nickel protective agent is 41-45 DEG C, and the treatment time is 1-3min.
As the common practise of those skilled in the art, in order to make the bonding force of nickel layer better, preferably, the method to carry out the step of pre-treatment to workpiece to be plated before being also included in electroless plating.Described pre-treatment comprises oil removing, acid etching and activation.Repeatedly wash respectively after oil removing, acid etching and activation.
As the common practise of those skilled in the art, be also included in after nickel dam conservation treatment is carried out to nickel plating part and dry step is carried out to plating piece.Wherein, drying can adopt natural air drying, also can adopt hot-air seasoning at 70-90 DEG C, but be not limited to this.
Finally, the invention provides a kind of plating nickel on surface workpiece, described plating nickel on surface workpiece comprises workpiece substrates to be plated and plating in the nickel layer on described workpiece substrates surface to be plated, and the surface of described nickel layer is also coated with nickel protection layer; Described plating nickel on surface workpiece is obtained by chemical nickel plating method provided by the invention.
In the present invention, particular requirement be there is no for workpiece to be plated, only need its surface energy to plate metal nickel dam.Under preferable case, described workpiece substrates to be plated is the workpiece to be plated that surface has copper plate.
In order to make technical problem solved by the invention, technical scheme and beneficial effect clearly understand, below in conjunction with specific embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.In embodiment and comparative example adopt raw material to be all commercially available, the present invention is not particularly limited.
Embodiment 1
(1) according to following proportioning by each components dissolved in water, preparation the present embodiment water-soluble nickel protective agent S1: Sodium orthomolybdate 1g/L; Benzo tetrazole 1g/L; Tao Shi wetting agent CF-101.5g/L; 5-(3-aminophenyl) tetrazolium 0.5g/L; 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid 1g/L;
(2) be that the workpiece to be plated of copper coating carries out ultrasonic oil removing by surface, the sulphuric acid soln of 5wt% is adopted to soak except oxide layer after washing, then proceed to palladium activation solution after putting into the preimpregnation of hydrochloric acid presoak after washing and activate 3min, put into chemical nickel-plating liquid after washing and carry out chemical nickel plating process, chemical nickel-plating liquid consists of: single nickel salt 20g/L, sodium hypophosphite 25g/L, sodium-acetate 18g/L, lactic acid 20g/L, oxysuccinic acid 5g/L, succinic acid 4.5g/L; Forming thickness on copper coating surface after nickel plating completes is the nickel layer of 3 microns, be impregnated in by nickel plating part in the water-soluble nickel protective agent S1 that step (1) prepares, process 3min at 45 DEG C after washing, then washing drying with whizzer, obtains plating piece S10.
Embodiment 2
Adopt the step identical with embodiment 1 to prepare water-soluble nickel protective agent S2, and carry out chemical nickel plating, difference is:
In step (1), water-soluble nickel protective agent S2 consists of: Sodium orthomolybdate 8g/L; Benzo tetrazole 6g/L; Tao Shi wetting agent CF-1015g/L; 5-(3-aminophenyl) tetrazolium 5g/L; 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid 5g/L;
In step (2), the condition of nickel dam conservation treatment comprises: the temperature of water-soluble nickel protective agent S2 is 43 DEG C, and the treatment time is 2min.
By above-mentioned steps, obtain the plating piece S20 of the present embodiment.
Embodiment 3
Adopt the step identical with embodiment 1 to prepare water-soluble nickel protective agent S3, and carry out chemical nickel plating, difference is:
In step (1), water-soluble nickel protective agent S3 consists of: Sodium orthomolybdate 15g/L; Benzo tetrazole 10g/L; Tao Shi wetting agent CF-1027g/L; 5-(3-aminophenyl) tetrazolium 9g/L; 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid 8g/L;
In step (2), the condition of nickel dam conservation treatment comprises: the temperature of water-soluble nickel protective agent S3 is 41 DEG C, and the treatment time is 1min.
By above-mentioned steps, obtain the plating piece S30 of the present embodiment.
Embodiment 4
Adopt the step identical with embodiment 1 to prepare water-soluble nickel protective agent 4, and carry out chemical nickel plating, difference is:
In step (1), water-soluble nickel protective agent S4 consists of: benzo tetrazole 6g/L; Tao Shi wetting agent CF-1015g/L; 5-(3-aminophenyl) tetrazolium 5g/L; 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid 5g/L;
In step (2), the condition of nickel dam conservation treatment comprises: the temperature of water-soluble nickel protective agent S4 is 43 DEG C, and the treatment time is 2min.
By above-mentioned steps, obtain the plating piece S40 of the present embodiment.
Embodiment 5
Adopt the step identical with embodiment 1 to prepare water-soluble nickel protective agent 5, and carry out chemical nickel plating, difference is:
In step (1), water-soluble nickel protective agent S5 consists of: Sodium orthomolybdate 8g/L; Benzo tetrazole 6g/L; Tao Shi wetting agent CF-10 15g/L; 5-(3-aminophenyl) tetrazolium 5g/L;
In step (2), the condition of nickel dam conservation treatment comprises: the temperature of water-soluble nickel protective agent S5 is 43 DEG C, and the treatment time is 2min.
By above-mentioned steps, obtain the plating piece S50 of the present embodiment.
Embodiment 6
Adopt the step identical with embodiment 1 to prepare water-soluble nickel protective agent 6, and carry out chemical nickel plating, difference is:
In step (1), water-soluble nickel protective agent S6 consists of: benzo tetrazole 6g/L; Tao Shi wetting agent CF-10 15g/L; 5-(3-aminophenyl) tetrazolium 3g/L;
In step (2), the condition of nickel dam conservation treatment comprises: the temperature of water-soluble nickel protective agent S6 is 43 DEG C, and the treatment time is 2min.
By above-mentioned steps, obtain the plating piece S60 of the present embodiment.
Comparative example 1
Adopt the step identical with embodiment 1 to prepare water-soluble nickel protective agent DS1, and carry out chemical nickel plating, difference is:
In step (1), water-soluble nickel protective agent DS1 consists of: Sodium orthomolybdate 8g/L; Benzo tetrazole 6g/L; 5-(3-aminophenyl) tetrazolium 5g/L; 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid 5g/L;
In step (2), the condition of nickel dam conservation treatment comprises: the temperature of water-soluble nickel protective agent DS1 is 43 DEG C, and the treatment time is 2min.
By above-mentioned steps, obtain the plating piece DS10 of the present embodiment.
Comparative example 2
Adopt the step identical with embodiment 1 to prepare water-soluble nickel protective agent DS2, and carry out chemical nickel plating, difference is:
In step (1), water-soluble nickel protective agent DS2 consists of: Sodium orthomolybdate 8g/L; Benzo tetrazole 6g/L; Tao Shi wetting agent CF-10 15g/L; 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid 5g/L;
In step (2), the condition of nickel dam conservation treatment comprises: the temperature of water-soluble nickel protective agent DS2 is 43 DEG C, and the treatment time is 2min.
By above-mentioned steps, obtain the plating piece DS20 of the present embodiment.
Comparative example 3
Adopt the step identical with embodiment 1 to prepare water-soluble nickel protective agent DS3, and carry out chemical nickel plating, difference is:
In step (1), water-soluble nickel protective agent DS3 consists of: chromic oxide 6g/L, phosphoric acid 25ml/L, Sodium Fluoride 5g/L;
In step (2), the condition of nickel dam conservation treatment comprises: the temperature of water-soluble nickel protective agent DS3 is 43 DEG C, and the treatment time is 2min.
By above-mentioned steps, obtain the plating piece DS30 of the present embodiment.
Performance test
Neutral salt spray test condition: in salt-mist corrosion tester is the salts solution of 5 ± 1% with sodium chloride content: temperature is 35 DEG C time, and the collection liquid after spraying, pH value is 6.5 ~ 7.2.Dilute hydrochloric acid after permission dilution or sodium hydroxide adjusted to ph.Test space temperature 35 DEG C; Continuous spraying test period is 48H; Then in case, be returned to normal atmospheric condition, after stable, keep 2H.The outward appearance of each plating piece is detected.Standard: non-corroding, variable color, coating come off, and are designated as OK, otherwise are designated as NG.Test result is as shown in table 1.
Table 1
As can be seen from the test result of upper table 1 relatively, after adopting water-soluble nickel protective agent provided by the invention to carry out conservation treatment to nickel coating, plating piece appearance is good, and non-corroding, variable color, coating obscission, be obviously better than the plating piece sample in comparative example.
As can be seen from the test result of S10-S30 and S40-S60 relatively, time in water-soluble nickel protective agent provided by the invention preferably containing Sodium orthomolybdate and/or 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid, it is better to the protected effect of nickel coating.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (15)
1. a water-soluble nickel protective agent, is characterized in that, described water-soluble nickel protective agent is the aqueous solution containing benzo tetrazole, Tao Shi wetting agent CF-10 and 5-(3-aminophenyl) tetrazolium.
2. water-soluble nickel protective agent according to claim 1; it is characterized in that, in described water-soluble nickel protective agent, the content of benzo tetrazole is 1-10g/L; the content of Tao Shi wetting agent CF-10 is the content of 1.5-27g/L, 5-(3-aminophenyl) tetrazolium is 0.5-9g/L.
3. water-soluble nickel protective agent according to claim 1 and 2, is characterized in that, in described water-soluble nickel protective agent, the ratio of the weight content of described Tao Shi wetting agent CF-10 and 5-(3-aminophenyl) tetrazolium is (3 ~ 5): 1.
4. water-soluble nickel protective agent according to claim 1, is characterized in that, also containing Sodium orthomolybdate in described water-soluble nickel protective agent.
5. water-soluble nickel protective agent according to claim 4, is characterized in that, in described water-soluble nickel protective agent, the content of Sodium orthomolybdate is 1-15g/L.
6. water-soluble nickel protective agent according to claim 1, is characterized in that, also containing 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid in described water-soluble nickel protective agent.
7. water-soluble nickel protective agent according to claim 6, is characterized in that, in described water-soluble nickel protective agent, the content of 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid is 1-8g/L.
8. the preparation method of water-soluble nickel protective agent according to claim 1, is characterized in that, comprises and benzo tetrazole, Tao Shi wetting agent CF-10 and 5-(3-aminophenyl) tetrazolium being dissolved in the water, namely obtain described water-soluble nickel protective agent.
9. the preparation method stated according to Claim 8, is characterized in that, also comprises step Sodium orthomolybdate and/or 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid are dissolved in the water.
10. a chemical nickel plating method, is characterized in that, the method comprises workpiece to be plated to be placed in chemical nickel-plating liquid carries out electroless plating, obtains nickel plating part; And then nickel plating part is positioned in water-soluble nickel protective agent carries out nickel dam conservation treatment; It is characterized in that, described water-soluble nickel protective agent is the water-soluble nickel protective agent described in any one of claim 1-7.
11. chemical nickel plating methods according to claim 10, is characterized in that, the condition of nickel dam conservation treatment comprises: the temperature of water-soluble nickel protective agent is 41-45 DEG C, and the treatment time is 1-3min.
12. chemical nickel plating methods according to claim 10, is characterized in that, the method to carry out the step of pre-treatment to workpiece to be plated before being also included in chemical nickel plating.
13. chemical nickel plating methods according to claim 12, is characterized in that, described pre-treatment comprises oil removing, acid etching and activation.
14. 1 kinds of plating nickel on surface workpiece, described plating nickel on surface workpiece comprises workpiece substrates to be plated and plating in the nickel layer on described workpiece substrates surface to be plated, and the surface of described nickel layer is also coated with nickel protection layer; It is characterized in that, described plating nickel on surface workpiece is obtained by the chemical nickel plating method described in any one of claim 10-13.
15. plating nickel on surface workpiece according to claim 14, is characterized in that, described workpiece substrates to be plated is the workpiece to be plated that surface has copper plate.
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| CN112410838A (en) * | 2020-04-08 | 2021-02-26 | 上海昕沐化学科技有限公司 | Water-based electroplated nickel sealing agent and preparation method thereof |
| CN112647103A (en) * | 2020-12-18 | 2021-04-13 | 成都宏明双新科技股份有限公司 | Iron part broken section salt spray test lifting method |
| CN113621952A (en) * | 2020-05-08 | 2021-11-09 | 广州天至环保科技有限公司 | Aqueous protective agent for improving corrosion resistance and surface wettability of coating |
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| CN112410838B (en) * | 2020-04-08 | 2022-07-01 | 上海昕沐化学科技有限公司 | Water-based electroplated nickel sealing agent and preparation method thereof |
| CN113621952A (en) * | 2020-05-08 | 2021-11-09 | 广州天至环保科技有限公司 | Aqueous protective agent for improving corrosion resistance and surface wettability of coating |
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| CN104451617B (en) | 2017-04-05 |
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