CN104040035A - Plated Article And Manufacturing Method Therefor - Google Patents
Plated Article And Manufacturing Method Therefor Download PDFInfo
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- CN104040035A CN104040035A CN201280063675.XA CN201280063675A CN104040035A CN 104040035 A CN104040035 A CN 104040035A CN 201280063675 A CN201280063675 A CN 201280063675A CN 104040035 A CN104040035 A CN 104040035A
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- coating
- plating
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- plating product
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/10—Electroplating with more than one layer of the same or of different metals
- C25D5/12—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/60—Electroplating characterised by the structure or texture of the layers
- C25D5/623—Porosity of the layers
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/38—Electroplating: Baths therefor from solutions of copper
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/46—Electroplating: Baths therefor from solutions of silver
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/48—Electroplating: Baths therefor from solutions of gold
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/60—Electroplating characterised by the structure or texture of the layers
- C25D5/605—Surface topography of the layers, e.g. rough, dendritic or nodular layers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
- H01H1/00—Contacts
- H01H1/02—Contacts characterised by the material thereof
- H01H1/04—Co-operating contacts of different material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
- H01H11/00—Apparatus or processes specially adapted for the manufacture of electric switches
- H01H11/04—Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/22—Secondary treatment of printed circuits
- H05K3/24—Reinforcing the conductive pattern
- H05K3/244—Finish plating of conductors, especially of copper conductors, e.g. for pads or lands
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01R—ELECTRICALLY-CONDUCTIVE CONNECTIONS; STRUCTURAL ASSOCIATIONS OF A PLURALITY OF MUTUALLY-INSULATED ELECTRICAL CONNECTING ELEMENTS; COUPLING DEVICES; CURRENT COLLECTORS
- H01R13/00—Details of coupling devices of the kinds covered by groups H01R12/70 or H01R24/00 - H01R33/00
- H01R13/02—Contact members
- H01R13/03—Contact members characterised by the material, e.g. plating, or coating materials
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
- H05K2201/03—Conductive materials
- H05K2201/0332—Structure of the conductor
- H05K2201/0335—Layered conductors or foils
- H05K2201/0338—Layered conductor, e.g. layered metal substrate, layered finish layer, layered thin film adhesion layer
Abstract
A plated article comprising a multi-layer plating film formed on top of a conductive-metal substrate. Said plated article is characterized by having the following on top of the aforementioned substrate, in this order: a porous plating layer consisting primarily of nickel or copper; and a surface plating layer consisting primarily of gold or silver. This plated article is further characterized in that a large number of holes are formed in the surface of the multi-layer plating film. The plated article preferably also has an oxide layer comprising a nickel oxide or a copper oxide between the porous plating layer and the surface plating layer. It is also preferable that the surface plating layer is thinner where the aforementioned holes are than where bumps are. This makes it possible to provide a low-cost, highly corrosion-resistant plated article.
Description
Technical field
The present invention relates to be formed with the plating product of multicoating on the base material being formed by conductive metal.In addition, the present invention relates to manufacture method and the purposes of such plating product.
Background technology
At present, on the base material being made up of conductive metal, apply the plating product that obtain of plating uses in various fields.By apply plating on base material, can make the electricity such as contact resistance attenuating, wear resistant improvement, erosion resistance improvement, machinery, chemical property improve.Wherein, lower and the viewpoint of erosion resistance improvement from contact resistance, the coating of the precious metals such as Au, Ag is widely adopted in the contact of electric parts etc.For example, in the contact portion of web member, be generally at the substrate surface being formed by conductive metal, after forming the bottom coating such as Ni, Cu, form thinly the overlay coating (with reference to patent documentation 1) of the precious metals such as Au thereon.
But the precious metals such as known Au, Ag are when than its low-priced metallic contact, by potential difference generation electrolytic corrosion.Therefore,, from the viewpoint of erosion resistance, must avoid the pinprick in the overlay coating of precious metal to produce.For this reason, attempt or the thickness of thickening overlay coating or the method that overlay coating homogeneous is formed, but the manufacturing cost of any method all inevitably rises.Therefore the electroplating method of, strongly seeking to reduce the consumption of expensive precious metal and can improving electrical characteristic and chemical property.
Prior art document
Patent documentation
Patent documentation 1: TOHKEMY 2007-173224 communique
Summary of the invention
Invent problem to be solved
The present invention makes in order to solve above-mentioned problem, and object is to provide to be had excellent erosion resistance and plate cheaply product.In addition, object is also manufacture method and the purposes of the plating product that provide such.
For solving the method for problem
Above-mentioned problem is by providing the plating product that a kind of feature is following to solve: on the base material being made up of conductive metal, be formed with multicoating, on above-mentioned base material, have successively taking Ni or Cu as the Porous coating of main component and taking Au or Ag as the overlay coating of main component, be formed with a large amount of holes on the surface of above-mentioned multicoating.Now, the mean diameter in above-mentioned hole, in area loading mean value, is preferably 0.2～20 μ m.Also the thickness of preferred above-mentioned Porous coating is that the thickness of 0.1～20 μ m and above-mentioned overlay coating is 0.001～3 μ m.Also preferably between above-mentioned Porous coating and above-mentioned overlay coating, there is the oxide skin being formed by oxidation Ni or oxidation Cu.The also overlay coating thin thickness of the overlay coating Thickness Ratio protuberance in preferred above-mentioned hole.
In addition, also preferably between base material and Porous coating, be also formed with the bottom coating taking the metal identical with this Porous coating as main component.Now, the thickness of above-mentioned bottom coating is preferably 0.1～20 μ m.
Above-mentioned problem also solves by the manufacture method that above-mentioned plating product are provided, the manufacture method of these plating product is characterised in that, possess in the plating bath that contains Ni ion or Cu ion, form the first plating operation of Porous coating and containing Au ion or the plating bath of Ag ion in form the second plating operation of overlay coating.
Now, preferably, between above-mentioned the first plating operation and above-mentioned the second plating operation, also possesses the operation of Porous coating surface being carried out to oxide treatment.Also preferably plate after operation above-mentioned first, after Porous coating surface is carried out to oxide treatment, activation is carried out in this surface.Also preferably plate after operation above-mentioned second, oxide treatment is carried out in the surface of multicoating.
Above-mentioned problem is also by providing the electric parts being made up of above-mentioned plating product to solve, and this electric parts is characterised in that, the part that is formed with above-mentioned multicoating is electric terminal.Now, preferred above-mentioned electric parts is web member terminal or the switch terminal with contact portion and portion of terminal, in this contact portion, forms above-mentioned multicoating.In addition, also preferred above-mentioned electric parts is printed-wiring board (PWB).
The effect of invention
By the present invention, can provide and there is excellent anticorrosive and plate cheaply product.Manufacture method and the purposes of such plating product can be provided in addition.
Brief description of the drawings
Fig. 1 is the scanning ion microscope image of the Porous Ni coating section in embodiment 1.
Fig. 2 is the surperficial secondary electron image of the plating product of embodiment 1.
Fig. 3 is the friction wear test-results of the plating product of embodiment 1.
Fig. 4 is the secondary electron image after the friction wear of the plating product of embodiment 1 is tested.
Fig. 5 is the surperficial secondary electron image of the plating product of comparative example 1.
Fig. 6 is the friction wear test-results of the plating product of comparative example 1.
Fig. 7 is the secondary electron image after the friction wear of the plating product of comparative example 1 is tested.
Fig. 8 is the surperficial secondary electron image of the plating product of embodiment 7.
Embodiment
The present invention relates to be formed with the plating product of multicoating on the base material being formed by conductive metal.Here importantly on base material, have successively taking Ni or Cu as the Porous coating of main component, and taking Au or Ag as the overlay coating of main component, be formed with a large amount of holes on the surface of multicoating.There is excellent erosion resistance and plate cheaply product by forming such layer structure, can providing.
The base material of the base material that used in the present invention as long as being made up of conductive metal, its material is not particularly limited.Wherein, from viewpoints such as conductivities, use suitably copper or the alloy taking copper as main component.Here, more than " for main component " refers to and contains 50 % by weight.
Porous coating is in the present invention the coating taking Ni or Cu as main component.Here, more than " for main component " refers to and contains 50 % by weight.From contact resistance aspect, the Ni in Porous coating or the content of Cu more preferably 60 % by weight above, be more preferably 80 % by weight more than.In addition, in the present invention, " Porous " refers on the surface of coating a large amount of holes, and surface-area is large.More specifically, refer to have and enter a large amount of recesses for concavity towards base material low-lying area.
In the present invention, the thickness of Porous coating is preferably 0.1～20 μ m.When the thickness of Porous coating is less than 0.1 μ m, the worry that has erosion resistance, wear characteristic to reduce.The thickness of Porous coating more preferably 0.2 μ m above, be more preferably 0.5 μ m more than.When the thickness of Porous coating exceedes 20 μ m, the worry that has the manufacturing cost of causing to rise.The thickness of Porous coating more preferably 10 μ m following, be more preferably below 5 μ m.Here, the thickness of Porous coating refers to the thickness of the protuberance from this substrate surface to Porous coating form Porous coating on base material time.
In plating product of the present invention, on above-mentioned Porous coating, form the overlay coating taking Au or Ag as main component.Here, more than " for main component " refers to and contains 50 % by weight.From contact resistance aspect, the Au in overlay coating or Ag content more preferably 55 % by weight above, be more preferably 70 % by weight more than.
In the present invention, the thickness of overlay coating is preferably 0.001～3 μ m.When the thickness of overlay coating is less than 0.001 μ m, there is the worry that can not obtain desirable contact resistance use plating product of the present invention in electric terminal time.The thickness of overlay coating more preferably 0.005 μ m above, be more preferably 0.01 μ m more than.On the other hand, when the thickness of overlay coating is thick, manufacturing cost uprises.The thickness of overlay coating is more preferably below 1 μ m.Multicoating in the present invention, though the thickness of overlay coating than common when thin, erosion resistance is also excellent.Thickness from the viewpoint, particularly overlay coating of usage quantity that reduce precious metal during taking Au as main component more preferably below 0.1 μ m, be more preferably below 0.04 μ m, be particularly preferably below 0.025 μ m.Now, the thickness of overlay coating refers to the thickness adhesion weight with Au or Ag is long-pending divided by proportion and surfacing and that calculate.Here, surfacing is amassed and is not considered the concavo-convex of surface.
In addition, in the present invention, the preferably overlay coating thin thickness of the overlay coating Thickness Ratio protuberance in hole.Like this, contribute to the most overlay coating thickness of frictional coefficient, contact resistance or erosion resistance by thickening, can not make performance reduce the consumption that reduces Au or Ag.Particularly, because Au cost is high, therefore, its interests are large.More preferably below 0.8 times of overlay coating thickness that the overlay coating thickness in hole is protuberance.
By form overlay coating on Porous coating, form overlay coating in the concavo-convex mode along Porous coating, in overlay coating, also form hole.Protuberance at Porous coating surface easily forms overlay coating, is difficult to form overlay coating in bottom surface and the side in the hole that is formed at Porous coating surface.Its result, produces and does not form the part of overlay coating and the part of overlay coating thin thickness.In the present invention, this point is important, known to inhomogeneous as the overlay coating of main component taking Au or Ag, can prevent from causing that the corrosion current of electrolytic corrosion is concentrated, and erosion resistance improves.In the past, extensively carried out or thickeied overlay coating or carry out the trial that homogenizing improves erosion resistance, but having it is shocking specifically, by making, corrosion current is local to be disperseed, and has improved on the contrary erosion resistance.Owing to making noble metal dosage reduce and can effectively improve erosion resistance, therefore, from the viewpoint of saving resource, cost degradation, meaning is also large.
In area loading mean value, the mean diameter that is formed at the hole on multicoating surface is preferably 0.2～20 μ m.When mean diameter is less than 0.2 μ m, there is the worry that can not make corrosion current disperse, can not obtain excellent erosion resistance.The mean diameter in hole more preferably 0.5 μ m above, be more preferably 1 μ m more than.When the mean diameter in hole exceedes 20 μ m, plating product of the present invention when electric terminal uses, are had to the worry that contact resistance value increases, electrical conductivity declines.The mean diameter in hole more preferably 10 μ m following, be more preferably below 5 μ m.Here, the mean diameter in hole by selecting multiple holes from the scanning electron microscope photo (secondary electron image) on plating product surface, and the diameter of measuring these holes carries out area loading and on average obtains.When hole is not circle, to be equivalent to circular diameter as diameter.
The specific surface area of multicoating of the present invention is preferably more than 1.2 times, more preferably more than 1.4 times of specific surface area of the plated film that does not form hole.Large by specific surface area, corrosion current is dispersed, and can obtain excellent erosion resistance.
In the present invention, preferably, between base material and Porous coating, further form the bottom coating taking the metal identical with this Porous coating as main component.In the time that the hole of Porous coating connects base material from surface, by forming bottom coating, can prevent exposing of base material.In addition, by making Porous coating and bottom coating taking same metal as main component, eliminate the potential difference of Porous coating and bottom coating, can prevent the electrolytic corrosion being caused by potential difference.
The thickness of bottom coating is preferably 0.1～20 μ m.When the thickness of bottom coating is less than 0.1 μ m, there is the worry that can not fully be prevented the effect that base material exposes.The thickness of bottom coating more preferably 0.2 μ m above, be more preferably 0.5 μ m more than.When thickness is greater than 20 μ m, manufacturing cost uprises.The thickness of bottom coating more preferably 10 μ m following, be more preferably below 5 μ m.
Multicoating of the present invention preferably further has the oxide skin being made up of oxidation Ni or oxidation Cu between Porous coating and overlay coating.By have this oxide skin between Porous coating and overlay coating, the erosion resistance of plating product improves more.,, by have the oxide skin as insulation layer between Porous coating and overlay coating, Porous coating does not directly contact with overlay coating, can suppress the generation of corrosion current.
The applicable manufacture method of plating product of the present invention, possess in the plating bath that contains Ni ion or Cu ion, form Porous coating first plating operation and containing Au ion or the plating bath of Ag ion in form overlay coating second plating operation.
First, as the first plating operation, in the plating bath that contains Ni ion or Cu ion, skimming treatment as required, the base material washed are applied to plating, form the Porous coating taking Ni or Cu as main component.As long as form Porous coating, electroplating method is not particularly limited.Can be illustrated in electric plating method etc. in the plating bath that contains Ni ion or Cu ion and be added with the soluble quaternary ammonium with hydrophobicity base.Here,, as hydrophobicity base, carbonatoms is that more than 6 alkyl is applicable to.Now, quaternary ammonium salt can add in known Ni plating bath and Cu plating bath.The applicable addition of quaternary ammonium salt is 0.001～0.5mol/L.As known plating bath, for example, can illustrate a watt bath, Wood bath, thionamic acid Ni bath, organic acid Ni bath, cyaniding Cu bath, sulfuric acid Cu bath, tetra-sodium Cu bath etc.In the time electroplating, suitably set current density and time, making Porous coating is desirable thickness.
Then,, as the second plating operation, in the plating bath that contains Au ion or Ag ion, on Porous coating, form overlay coating.The plating bath kind that contains Au ion or Ag ion is not particularly limited, and can use known Au plating bath and Ag plating bath.For example, as Au plating bath, can illustrate cyaniding Au and bathe (acid bath, neutral bath, alkali bath), non-cyaniding bath (sulfurous acid bath), as Ag plating bath, can illustrate cyaniding Ag and bathe.Can form overlay coating by electroless plating, also can be used together electroless plating and plating.In addition, the condition of plating, suitably sets current density and time, and making overlay coating is desirable thickness.
In addition, in the manufacture method of plating product of the present invention, preferably, between the first plating operation and the second plating operation, oxide treatment is carried out in the surface of Porous coating.The method of oxide treatment is not particularly limited, as long as forming at Porous coating surface the method for oxide film thereon.For example, can be set forth in containing the method that heats Porous coating under oxygen atmosphere, make Porous coating be immersed in method in hot water, various medicine etc., be not particularly limited.In the time of heating Porous coating, Heating temperature is suitably set according to the oxygen concn of atmosphere etc., is generally 80～350 DEG C.In addition, above-mentioned oxide treatment, as long as importing at Porous coating surface the oxide treatment of Sauerstoffatom, comprises the processing that forms hydroxy.Therefore, on the surface of Porous coating, not only can form the oxide compound tunicle of oxidation Ni etc., and can form the oxyhydroxide tunicle of hydroxide Ni etc.
Then, implemented to above-mentioned the Porous coating surface that oxide treatment is crossed, in the second plating operation, formed overlay coating.Now, preferably, after oxide treatment, form before overlay coating, activation treatment is carried out in the surface of Porous coating.Thus, the surface of oxide film thereon, by appropriate etching, forms overlay coating and becomes easy in the second plating operation.In addition, the sticking power of overlay coating also improves.As operable liquid in activation treatment, as long as being etched in the liquid on the oxide compound tunicle surface that Porous coating surface forms, be not particularly limited, can use acidic aqueous solution, alkaline aqueous solution, the reductive agent aqueous solution, the coordination agent aqueous solution etc.As acidic aqueous solution, can illustrate the aqueous solution that contains hydrochloric acid, nitric acid, sulfuric acid, fluoric acid, Neutral ammonium fluoride, phosphoric acid, citric acid etc.As alkaline aqueous solution, can illustrate the aqueous solution that contains sodium hydroxide, potassium hydroxide, lithium hydroxide, ammonia etc.As the reductive agent aqueous solution, can illustrate the aqueous solution that contains ortho phosphorous acid, hydrazine, dimethylamine borane, Trimethylamine 99 borine, xitix, sodium borohydride, POTASSIUM BOROHYDRIDE etc.In addition, as the coordination agent aqueous solution, can illustrate the polycarboxylic acid that contains citric acid, oxalic acid, succsinic acid, tartrate, toxilic acid, xitix, fumaric acid etc.; The polyamine of quadrol, ethylenediamine tetraacetic acid (EDTA) (EDTA) etc.; The aqueous solution of the amino acid of glycine, aspartic acid etc. etc.Wherein, from etch capabilities and cost aspect, preferably use acidic aqueous solution.
Because Porous coating surface of the present invention has concavo-convexly, therefore, in hole, be difficult to etchedly, protuberance is easily etched.And, easily form overlay coating at etched position.Therefore, the overlay coating thin thickness of the overlay coating Thickness Ratio protuberance in hole is easy.Therefore,, from saving fund effect aspect, it is also favourable that activation treatment is carried out in the surface of Porous coating.
In addition, also preferably after the second plating operation, oxide treatment is carried out in the surface of multicoating., preferably after formation overlay coating, carry out oxide treatment.By such operation, overlay coating does not form and the oxidized processing in surface of exposing the Porous coating of the part of Porous coating and the thin part of overlay coating thickness, therefore, can make erosion resistance effectively improve.Oxidation treatment method now can adopt the condition identical with the oxidation treatment method carrying out between the first plating operation and the second plating operation, also can be unlike this.
In addition, in the manufacture method of plating product of the present invention, can also further add the operation that forms the bottom coating taking the metal identical with Porous coating as main component.That is, forming before the first plating operation of Porous coating, base material is applied to plating, form the bottom coating taking the metal identical with Porous coating as main component.Plating bath while forming bottom coating is not particularly limited, and can use the plating bath using from above-mentioned the first plating operation to remove the plating bath etc. of quaternary ammonium salt.In addition, about the condition of plating, suitably set current density and time, making bottom coating is desirable thickness.
In addition, multicoating of the present invention, as long as in the scope of not damaging effect of the present invention, also can comprise overlay coating, oxide skin, Porous coating, bottom coating coating in addition.For example, between base material and bottom coating, between Porous coating and overlay coating, can be gripped with other coating.Wherein, preferably between Porous coating and overlay coating, be gripped with the intermediate deposit of the intermediate potential of the current potential that shows Porous coating current potential and overlay coating.By such operation, can dwindle the potential difference between the coating of direct contact, therefore, can suppress the generation of corrosion current, can further improve erosion resistance.As such intermediate deposit, can enumerate coating taking Pd as main component, with coating taking Sn as main component.Here, more than " for main component " refers to and contains 50 % by weight.As the intermediate deposit taking Pd as main component, can illustrate the coating only being formed by Pd, the coating being formed by Pd-Ni alloy, Pd-P alloy.As the intermediate deposit taking Sn as main component, can illustrate the coating only being formed by Sn, the coating being formed by Sn-Ni alloy.In addition, when overlay coating is the coating taking Au as main component, also preferably use the coating taking Ag as main component as intermediate deposit.Here, more than " for main component " refers to and contains 50 % by weight.As the intermediate deposit taking Ag as main component, can illustrate the coating only being formed by Ag, the coating being formed by Ag-Sn alloy.
From preventing the viewpoint of corrosion, can also implement surface treatment on the surface of multicoating.During taking Au as main component, can illustrate sealing of hole processing etc. at overlay coating,, can illustrate and prevent sulfidizing (preventing variable color processing) etc. during taking Ag as main component at overlay coating.In addition, the viewpoint improving from oilness, also can be at the surface coated lubricant of multicoating of the present invention.In addition, for the water-repellancy that makes multicoating of the present invention improves, also can implement drying processing by effects on surface.
The purposes of plating product of the present invention is not particularly limited.Can utilize low contact resistance and excellent erosion resistance, sliding, in various uses, use.Wherein, the part that is formed with above-mentioned multicoating is that the electric parts of electric terminal is applicable embodiment.The electric terminal that maintains desired electrical specification and excellent in te pins of durability can be provided.More specifically, this electric parts is web member or the switch terminal with contact portion and portion of terminal, is formed with above-mentioned multicoating in this contact portion, is applicable embodiment.Contact portion contacts with other web member etc., the part of circulating current, and portion of terminal is the part being connected with cable etc.Web member terminal of the present invention, even plug repeatedly, electrical specification is also difficult for declining, so preferably.In addition, the electric parts being made up of plating product of the present invention is that printed-wiring board (PWB) is also applicable embodiment.
Embodiment
Below, use embodiment to illustrate in greater detail the present invention, but the present invention is not limited by these embodiment.Test method in the present embodiment is carried out according to following method.
(1) section is observed
The focused ion beam processing observing device " FB-2100 " that uses the Hitachi High-Technologies of Co., Ltd. to produce, obtain plating the scanning ion microscope image after FIB (Focused Ion Beam, the focused ion beam) processing of product section.
(2) surface observation
The electric field radioactive scanning electronic microscope (FE-SEM) " S-4800 " that uses the Hitachi High-Technologies of Co., Ltd. to produce, photographs to the surface of plating product, obtains secondary electron image.
(3) specific surface area
By laser microscope, the resolution of (X-Y) direction is set as 0.001 μ m in length and breadth, highly the resolution of (Z) direction is set as 0.001 μ m, measures the surface-area of plating product.Then, with above-mentioned surface-area with respect to 1664 μ m
2the ratio of mensuration place viewed in plan area be specific surface area.Laser microscope is the colored 3D laser microscope " VK-9700 " that the KEYENCE of Co., Ltd. produces.
(4) friction wear test
Use the friction wear trier (form SSWT) of Shen Gangzao machine Co., Ltd. production, measure the skin friction coefficient of the plating product that obtained with following test conditions.Then, obtain taking transverse axis as coming and going slip number of times, the longitudinal axis chart as frictional coefficient.The frictional coefficient of obtaining every 20 circulations according to obtained chart, calculates average friction coefficient.
Ball: Φ 9.8mm, brass (after Ni bottom 1 μ m, Au0.4 μ m plating)
Test temperature: 22 DEG C
Testing load: 500mN
Stroke: 4.00mm
Frequency: 2.00Hz
Come and go slip number of times: 3600 circulations
(5-1) corrosion resistance test (gaseous corrosion test)
According to the sulfur dioxide gas test of recording in JIS H8502, test with following condition.Then the corrosion default, occurring on plating product surface with point stages of digital evaluation.Here, point stages of digital is the scoring that represents shared corroded area rate (%) ratio of test face, is divided into 10～0.Situation about not having completely taking corrosion is as 10, and generally speaking, point stages of digital more than 9 is chosen as well.
Device: the mixed gas corrosion testing machine " GPL-91-C " that Jing Ji institute of Yamazaki Co. Ltd. produces
Sulfur dioxide concentration: 10ppm
Test temperature: 40 DEG C
Relative humidity: 80%
Test period: 96 hours
(5-2) corrosion resistance test (salt spray testing)
Use the following device of recording, at plating product surface spray salt solution, after 48 hours, observe plating product surface.Then the corrosion default, occurring on plating product surface with point stages of digital evaluation.Metewand about point stages of digital is same as described above.
Device: the salt spray testing machine " CAP-90 " that Suga Test Instruments Co., Ltd. produces
Experimental liquid: 47% salt solution
Test temperature: 35 DEG C
Test period: 48 hours
(6) contact resistance test
The electric terminal simulator " CRS-113-AU type " that uses Jing Ji institute of Yamazaki Co. Ltd. to produce, the contact resistance by four-terminal method with following condition mensuration plating product.Particularly, mensuration is slowly pin to be pressurizeed from no load condition, applies the loading of maximum 1.0N.Then, measure loading is slowly declined, the variation of the contact resistance while finally turning back to no load condition.The measurement of contact resistance, the resistance value when loading when measuring respectively the loading of pressurization when (past) and being 0.5N, as the 1.0N of maximum loading time, when decompression (returning) is 0.5N.
Probe: R025-K-18 type (radius 0.1mm shape)
Probe material: K18 (Φ 1mm)
Apply electric current: 10mA
(7) chemical composition analysis of plated film
Use following determinator to plate the chemical composition analysis of product tunicle.Particularly, carry out the obtained hole of plating product and the analysis of the chemical constitution of protuberance.
Determinator: scanning electron microscope (FE-SEM/EDX)
FE-SEM portion: " S-4800 " that the Hitachi High-Technologies of Co., Ltd. produces
EDX portion: " SX-350 " that Horiba Ltd produces
Condition determination: 10000 times of acceleration voltage 10kV, operating distance (W.D.) 15mm, multiplying powers
Embodiment 1
(electrolytic degreasing processing)
First, as base material, prepare the copper coin of 30mm × 40mm × 0.3mm, taking this copper coin as negative electrode, be immersed in 60g/L and be dissolved with in 50 DEG C of aqueous solution of electrolytic degreasing agent " PAKUNA THE-210 " of YUKEN Industrial Co., Ltd production, with cathode current density 4A/dm
2carry out 60 seconds of skimming treatment.With after the base material of ion exchanged water washing skimming treatment 3 times, in the aqueous sulfuric acid of 2vol%, flooded for 60 seconds in room temperature, carry out pickling clean., then wash 3 times then.
(formation of bottom Ni coating)
The sample that electrolytic degreasing was processed is immersed in the aqueous solution of following composition of the pH4.4 of 50 DEG C of insulations.Then, pneumatic blending is carried out on limit, and limit is with cathode current density 3A/dm
2carry out electrolysis plating Ni and processed for 190 seconds, form the bottom Ni coating of thickness 1 μ m.After this, clean sample 3 times with ion exchanged water.
Nickel sulfamic acid [Ni (SO
3nH
2)
24H
2o]: 396g/L
Nickelous chloride [NiCl
26H
2o]: 30g/L
Boric acid [H
3bO
3]: 30g/L
(formation of Porous Ni coating)
The sample that is formed with bottom Ni coating is immersed in the aqueous solution of following composition of the pH4.2 of 50 DEG C of insulations.Then, pneumatic blending is carried out on limit, and limit is with cathode current density 3A/dm
2carry out electrolysis plating Ni and processed for 80 seconds, on bottom Ni coating, form the Porous Ni coating of thickness 1 μ m.After this,, with after the clean sample of ion exchanged water 3 times, in ion exchanged water, flood ultrasonic cleansing 1 minute.
Nickel sulfamic acid [Ni (SO
3nH
2)
24H
2o]: 396g/L
Nickelous chloride [NiCl
26H
2o]: 30g/L
Boric acid [H
3bO
3]: 30g/L
Dodecyl trimethyl ammonium chloride: 0.02mol/L
Sample after the Porous Ni coating in embodiment 1 being formed by FIB (Focused Ion Beam) is processed, and observes section.In Fig. 1, represent the scanning ion microscope image of section.As shown in Figure 1, the sample after known Porous Ni electrolytic coating forms, has and enters the multiple recesses for concavity from surface towards base material low-lying area.
(formation of surfaces A u electrolytic coating)
The sample that is formed with Porous Ni coating is immersed in the Au plating solution " BAR7 " (Au content is 5g/L) of Japan Pure Chemical Co., Ltd.'s production of the pH4.2 of 60 DEG C of insulations.Then, stir with magnetic stirring apparatus on limit, and limit is with cathode current density 3A/dm
2carry out electrolysis plating Au and processed for 8 seconds, on Porous Ni electrolytic coating, form the Au coating of thickness 0.05 μ m.After this, clean sample 3 times with ion exchanged water, in the ion exchanged water of 60 DEG C, flooded for 60 seconds, after ultrasonic cleansing, be dried, obtain thus the plating product of embodiment 1.
In Fig. 2, represent the secondary electron image on the plating product surface of embodiment 1.As shown in Figure 2, confirm to there is hole on the plating product surface of embodiment 1, be formed with the coating of Porous.In addition, in the secondary electron image of the plating product of the embodiment 1 representing, select at random multiple holes in Fig. 2, obtain respectively area.Now, while being not circle in hole, to be equivalent to circular diameter as diameter.Then, obtain the mean diameter in hole with area loading mean value, result mean diameter is approximately 3.5 μ m.
In Fig. 3, represent the result of the friction wear test of the plating product of embodiment 1.As shown in Figure 3, in mensuration, do not confirm the obvious rising of frictional coefficient.In addition, in Fig. 4, represent the secondary electron image after the friction wear test of plating product of embodiment 1.As shown in Figure 4, known, even also maintain the porous structure with fine concavity after friction wear test.In addition, for the plating product of embodiment 1, evaluate specific surface area, average friction coefficient, erosion resistance and contact resistance according to above-mentioned test method.Result is gathered in table 2 to expression.
Embodiment 2
Embodiment 2 is examples that sealing of hole processing has been implemented on the plating product surface to obtaining in embodiment 1.In the aqueous solution (200mL/L) of limit produces the plating product of embodiment 1 plating Au hole sealing processing agent " TETRA No.4 " at the TETRA of Co., Ltd. of 45 DEG C of insulations, apply ultrasonic wave limit and flooded for 10 seconds.Then, remove the aqueous solution in surface attachment with air knife, obtain the plating product of embodiment 2.In addition, for the plating product of embodiment 2, also evaluate average friction coefficient, erosion resistance and contact resistance according to above-mentioned test method.Result is gathered in table 2 to expression.
Embodiment 3
Stir with magnetic stirring apparatus on limit, and limit is with cathode current density 3A/dm
2carry out electrolysis plating Au and processed for 5 seconds, on Porous Ni electrolytic coating, form the Au coating of thickness 0.03 μ m, in addition, obtain plating product with method similarly to Example 1.In addition, for the plating product of embodiment 3, also evaluate erosion resistance and contact resistance according to above-mentioned test method.Result is gathered in table 2 to expression.
Embodiment 4
Embodiment 4 is examples that sealing of hole processing has been implemented on the plating product surface to obtaining in embodiment 3.The method of sealing of hole processing is identical with embodiment 2.In addition, for the plating product of embodiment 4, also evaluate erosion resistance and contact resistance according to above-mentioned test method.Result is gathered in table 2 to expression.
Embodiment 5
Stir with magnetic stirring apparatus on limit, and limit is with cathode current density 3A/dm
2carry out electrolysis plating Au and processed for 3 seconds, on Porous Ni electrolytic coating, form the Au coating of thickness 0.02 μ m, in addition, obtain plating product with method similarly to Example 1.In addition, for the plating product of embodiment 5, also evaluate erosion resistance and contact resistance according to above-mentioned test method.Result is gathered in table 2 to expression.
Embodiment 6
Embodiment 6 is examples that sealing of hole processing has been implemented on the plating product surface to obtaining in embodiment 5.The method of sealing of hole processing is identical with embodiment 2.In addition, for the plating product of embodiment 6, also evaluate erosion resistance and contact resistance according to above-mentioned test method.Result is gathered in table 2 to expression.
Embodiment 7
Embodiment 7 has formed after Porous Ni coating in embodiment 1, after oxide treatment, processes with acidic aqueous solution, forms the example of surfaces A u coating.After the sample that is formed with Porous Ni coating is washed, is dried, in the thermostatic bath that is warmed to 260 DEG C, place after 10 minutes, take out from thermostatic bath.The sample that oxide treatment has been carried out in operation is like this flooded after 1 minute in the hydrochloric acid at 5vol% in room temperature, wash.After this, operation, carries out the formation of surfaces A u coating similarly to Example 1.
In Fig. 8, represent the secondary electron image on the plating product surface of embodiment 7.As shown in Figure 8, confirm that the plating product of embodiment 7 have hole on its surface, be formed with the coating of Porous.In addition, for the plating product of embodiment 7, according to above-mentioned test method, evaluate average friction coefficient, erosion resistance and contact resistance.Result is gathered in table 2 to expression.In the plating product of embodiment 7, the ultimate analysis in hole (spectrum 1) and the protuberance (spectrum 2) that has also carried out representing in Fig. 8.In table 1, represent result.
[table 1]
Embodiment 8
Embodiment 8 forms after surfaces A u electrolytic coating in embodiment 1, has carried out the example of oxide treatment.The method of oxide treatment is identical with embodiment 7.According to above-mentioned test method, evaluate average friction coefficient, erosion resistance and contact resistance.Result is gathered in table 2 to expression.
Embodiment 9
Embodiment 9 replaces the surfaces A u coating in embodiment 1, the example of formation surfaces A g coating., the plating product of embodiment 9 form successively bottom Ni coating, Porous Ni coating and surfaces A g coating on base material.The operation of carrying out the operation of electrolytic degreasing processing, the operation that forms bottom Ni coating, formation Porous Ni coating is identical with embodiment 1.The operation that forms surfaces A g coating is as described below.
(formation of surfaces A g coating)
In the aqueous solution of the following composition of room temperature, dipping is formed with the sample of Porous Ni coating.Then, with cathode current density 2A/dm
2carry out striking plating Ag and processed for 10 seconds.After this, clean sample 3 times with ion exchanged water.
Silver cyanide [AgCN]: 3g/L
Potassium cyanide [KCN]: 160g/L
Salt of wormwood [K
2cO
3]: 100g/L
In " S-900 " 2L producing in Metalor Technologies Japan Co., Ltd., add dipping in the electroplate liquid of following compositions to be formed with the sample of Ag striking coating.55 DEG C of insulations, with cathode current density 5A/dm
2plate Ag15 second.After this, clean sample 3 times with ion exchanged water, carry out ultrasonic cleansing, on Porous Ni coating, form thus the surfaces A g coating of thickness 0.4 μ m.
Silver potassium cyanide [KAg (CN)
2]: 150g/L
Potassium cyanide [KCN]: 2.5g/L
Further implement to prevent variable color processing on the plating product surface obtaining.In the aqueous solution (200mL/L) of the anti-blushing agent " CE-9700W " of particularly, obtained plating product being produced in the ChemicalDensi of 55 DEG C of insulations company limited, flooded for 5 seconds.Then, clean 3 times with ion exchanged water, be dried.For the plating product of embodiment 9, according to above-mentioned test method, evaluate erosion resistance and contact resistance.Result is gathered in table 2 to expression.
Comparative example 1
Comparative example 1 is the example that does not carry out the formation of Porous Ni coating in embodiment 1.Particularly, the plating product of comparative example 1 form successively bottom Ni coating and surfaces A u coating on base material.The base material of skimming treatment is immersed in the plating bath of pH4.4 of 50 DEG C of insulations.Then, pneumatic blending limit is carried out with 3A/dm in limit
2current density carry out electrolysis plating Ni and process, form the Ni coating of thickness 2 μ m.After this, clean sample 3 times with ion exchanged water, in the ion exchanged water of 60 DEG C, flood 60 seconds, ultrasonic cleansing.The composition of the plating bath of the composition of plating bath when forming bottom Ni coating in embodiment 1 is identical.
Then, form the surfaces A u coating of thickness 0.05 μ m at the specimen surface that is formed with bottom Ni coating, obtain the plating product of comparative example 1.Condition while forming surfaces A u coating is identical with the condition of explanation in embodiment 1.
In Fig. 5, represent the surperficial secondary electron image of the plating product of comparative example 1.As shown in Figure 5, do not confirm hole on electrolytic coating surface.
In Fig. 6, represent the result of the friction wear test of the plating product of comparative example 1.As shown in Figure 6, in mensuration, because rising rapidly, frictional coefficient stops test.In addition, in Fig. 7, represent the secondary electron image after the friction wear test of plating product of comparative example 1.As shown in Figure 7, after known friction wear test, plated film is pruned.In addition, for the plating product of comparative example 1, according to above-mentioned test method, evaluate average friction coefficient, erosion resistance and contact resistance.Result is gathered in table 2 to expression.
Comparative example 2
Comparative example 2 is examples that sealing of hole processing has been implemented on the plating product surface to obtaining in comparative example 1.The condition of sealing of hole processing is identical with embodiment 1.In addition, for the plating product of comparative example 2, according to above-mentioned test method, evaluate average friction coefficient, erosion resistance and contact resistance.Result is gathered in table 2 to expression.
As shown in table 2, the specific surface area that to have confirmed with respect to the specific surface area of the plating product of comparative example 1 be the plating product of 1.0043, embodiment 1 is 1.5112, is increased to approximately 1.5 times.By the comparison of embodiment and comparative example, confirm that erosion resistance increases substantially by having hole on surface, meanwhile, average friction coefficient declines.In addition, even have hole on the surface of multicoating, also not confirming contact resistance value has large variation.From the result of embodiment 1～6, even if make the thickness attenuation of overlay coating, also maintain erosion resistance and contact resistance value.In addition, more known by embodiment 1 and embodiment 7, by also have oxidation Ni layer between Porous coating and overlay coating, erosion resistance further improves.More known by embodiment 1 and embodiment 8, carries out oxide treatment having formed effects on surface after overlay coating, and erosion resistance also further improves.Therefore, the known plating product that meet the present invention's formation, can maintain electrical characteristic and obtain excellent erosion resistance and wear resistant.
Claims (14)
1. plating product, is characterized in that:
On the base material being formed by conductive metal, be formed with multicoating,
On described base material, have successively taking Ni or Cu as the Porous coating of main component and overlay coating taking Au or Ag as main component,
Be formed with a large amount of holes on the surface of described multicoating.
2. plating product as claimed in claim 1, is characterized in that:
In area loading mean value, the mean diameter in described hole is 0.2～20 μ m.
3. plating product as claimed in claim 1 or 2, is characterized in that:
The thickness of described Porous coating is 0.1～20 μ m, and the thickness of described overlay coating is 0.001～3 μ m.
4. the plating product as described in any one in claim 1～3, is characterized in that:
Between described Porous coating and described overlay coating, also there is the oxide skin being formed by oxidation Ni or oxidation Cu.
5. the plating product as described in any one in claim 1～4, is characterized in that:
The overlay coating thin thickness of the overlay coating Thickness Ratio protuberance in described hole.
6. the plating product as described in any one in claim 1～5, is characterized in that:
Between base material and Porous coating, be also formed with the bottom coating taking the metal identical with this Porous coating as main component.
7. plating product as claimed in claim 6, is characterized in that:
The thickness of described bottom coating is 0.1～20 μ m.
8. a manufacture method for the plating product described in any one in claim 1～7, is characterized in that possessing:
In the plating bath that contains Ni ion or Cu ion, form the first plating operation of Porous coating, and
In the plating bath that contains Au ion or Ag ion, form the second plating operation of overlay coating.
9. the manufacture method of plating product as claimed in claim 8, is characterized in that:
Between described the first plating operation and described the second plating operation, also possesses the operation of Porous coating surface being carried out to oxide treatment.
10. the manufacture method of plating product as claimed in claim 9, is characterized in that:
After described the first plating operation, after Porous coating surface is carried out to oxide treatment, activation treatment is carried out in this surface.
The manufacture method of 11. plating product as described in any one in claim 8～10, is characterized in that: after described the second plating operation, oxide treatment is carried out in the surface of multicoating.
12. 1 kinds of electric partss that are made up of the plating product described in any one in claim 1～7, is characterized in that:
The part that is formed with described multicoating is electric terminal.
13. electric partss as claimed in claim 12, is characterized in that:
Described electric parts is web member terminal or the switch terminal with contact portion and portion of terminal, in this contact portion, is formed with described multicoating.
14. electric partss as claimed in claim 12, is characterized in that:
Described electric parts is printed-wiring board (PWB).
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2011-282348 | 2011-12-22 | ||
| JP2011282348 | 2011-12-22 | ||
| PCT/JP2012/083371 WO2013094766A1 (en) | 2011-12-22 | 2012-12-22 | Plated article and manufacturing method therefor |
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|---|---|
| CN104040035A true CN104040035A (en) | 2014-09-10 |
| CN104040035B CN104040035B (en) | 2017-05-03 |
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|---|---|
| JP (1) | JP6089341B2 (en) |
| CN (1) | CN104040035B (en) |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113474486A (en) * | 2019-05-09 | 2021-10-01 | 纳美仕有限公司 | Composite copper material |
| CN113614284A (en) * | 2019-05-09 | 2021-11-05 | 纳美仕有限公司 | Method for producing metal material having metal layer |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP5851231B2 (en) * | 2011-12-22 | 2016-02-03 | 日本圧着端子製造株式会社 | parts |
| JP5851232B2 (en) * | 2011-12-22 | 2016-02-03 | 日本圧着端子製造株式会社 | parts |
| JP5975351B2 (en) * | 2013-05-27 | 2016-08-23 | スガ試験機株式会社 | Corrosion promotion tester and corrosion promotion test method |
| WO2015060449A1 (en) | 2013-10-25 | 2015-04-30 | オーエム産業株式会社 | Method for producing plated article |
| JP6978262B2 (en) * | 2017-09-22 | 2021-12-08 | セーレン株式会社 | Breathable waterproof metal leaf |
| JP2022100002A (en) | 2020-12-23 | 2022-07-05 | Ｄｏｗａメタルテック株式会社 | Ag PLATING MATERIAL, PRODUCTION METHOD OF Ag PLATING MATERIAL, AND ELECTRICAL COMPONENT |
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| CN113614284A (en) * | 2019-05-09 | 2021-11-05 | 纳美仕有限公司 | Method for producing metal material having metal layer |
Also Published As
| Publication number | Publication date |
|---|---|
| JPWO2013094766A1 (en) | 2015-04-27 |
| WO2013094766A1 (en) | 2013-06-27 |
| JP6089341B2 (en) | 2017-03-08 |
| CN104040035B (en) | 2017-05-03 |
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