WO2014010662A1 - 無電解金めっき処理方法、および金めっき被覆材料 - Google Patents
無電解金めっき処理方法、および金めっき被覆材料 Download PDFInfo
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- WO2014010662A1 WO2014010662A1 PCT/JP2013/068956 JP2013068956W WO2014010662A1 WO 2014010662 A1 WO2014010662 A1 WO 2014010662A1 JP 2013068956 W JP2013068956 W JP 2013068956W WO 2014010662 A1 WO2014010662 A1 WO 2014010662A1
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- gold plating
- layer
- plating
- gold
- electroless
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
- C23C18/1824—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
- C23C18/1827—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment only one step pretreatment
- C23C18/1831—Use of metal, e.g. activation, sensitisation with noble metals
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- B32B15/00—Layered products comprising a layer of metal
- B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
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- B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
- B32B15/017—Layered products comprising a layer of metal all layers being exclusively metallic one layer being formed of aluminium or an aluminium alloy, another layer being formed of an alloy based on a non ferrous metal other than aluminium
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- B32B15/00—Layered products comprising a layer of metal
- B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
- B32B15/018—Layered products comprising a layer of metal all layers being exclusively metallic one layer being formed of a noble metal or a noble metal alloy
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
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- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/043—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of metal
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- C22C21/06—Alloys based on aluminium with magnesium as the next major constituent
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- C22C5/02—Alloys based on gold
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- 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
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- C23C28/021—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material including at least one metal alloy layer
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- C—CHEMISTRY; METALLURGY
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- 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
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- 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
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- H01—ELECTRIC ELEMENTS
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- 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
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Definitions
- the present invention relates to an electroless gold plating method and a gold plating coating material.
- the method of forming a gold plating layer by such electroless displacement gold plating has the following problems.
- the metal substrate that is the material to be plated may elute locally, resulting in the formation of minute recesses on the surface of the metal substrate.
- gold is not properly deposited in the recessed portions, and pinholes are generated on the surface of the formed gold plating layer.
- the obtained electrical contact material has a problem that the corrosion resistance and the conductivity are lowered, and peeling occurs at the interface with the solder at the time of joining with the solder.
- Patent Document 1 discloses a method in which a palladium plating treatment is performed on a substrate to form a palladium plating layer, and then a gold plating layer is formed on the palladium plating layer by electroless reduction gold plating. ing.
- Patent Document 1 uses a cyan-based gold plating bath when forming the gold-plated layer, it is necessary to treat a highly toxic cyan-based waste liquid, and the working environment and external There was a problem that the load on the environment was large.
- an electroless reduction plating treatment is performed on a palladium plating layer using a non-cyan gold plating bath instead of a cyan gold plating bath, the resulting gold plating layer has a coverage rate. There is a problem that it is extremely low and, in addition, the adhesion is extremely low.
- the present invention has been made in view of such a situation, and can form a gold-plated film that has excellent adhesion and suppresses the generation of pinholes.
- An object of the present invention is to provide an electroless gold plating method with improved load.
- the present inventors formed a base alloy layer composed of a predetermined element on a base material, and provided a non-cyan gold plating bath on the base alloy layer. It was found that the object can be achieved by forming a gold plating layer by electroless reduction plating, and the present invention has been completed.
- An electroless gold plating method comprising: forming an M1-M2-M3 alloy (where M1 is made of Ni, Fe, Co, Cu, Zn, and Sn). At least one element selected, M2 is at least one element selected from Pd, Re, Pt, Rh, Ag, and Ru, and M3 is at least one element selected from P and B.
- the electroless gold plating method is provided.
- a gold plating coating material comprising a base material, a base alloy layer formed on the base material, and a gold plating layer formed on the base alloy layer,
- the base alloy layer is an M1-M2-M3 alloy (where M1 is at least one element selected from Ni, Fe, Co, Cu, Zn, and Sn, and M2 is Pd, Re, Pt, Rh, Ag) , And at least one element selected from Ru, M3 is at least one element selected from P and B.)
- M1-M2-M3 alloy where M1 is at least one element selected from Ni, Fe, Co, Cu, Zn, and Sn, and M2 is Pd, Re, Pt, Rh, Ag
- M3 is at least one element selected from P and B.
- an electroless gold plating process that can form a gold plating film that has excellent adhesion and suppresses the generation of pinholes and that has improved the load on the working environment and the external environment.
- a method can be provided.
- FIG. 1 is an SEM photograph of the surface of the gold plating coating material obtained in Examples and Comparative Examples.
- FIG. 2 is a graph showing ion elution concentrations of the gold plating coating materials obtained in Examples and Comparative Examples.
- the gold plating coating material obtained by the electroless gold plating method of the present invention comprises a base alloy layer and a gold plating layer on a base material, and the base alloy layer is an M1-M2-M3 alloy (however, , M1 is at least one element selected from Ni, Fe, Co, Cu, Zn, and Sn, M2 is at least one element selected from Pd, Re, Pt, Rh, Ag, and Ru, M3 Is at least one element selected from P and B.)
- ⁇ Base material> Although it does not specifically limit as a base material, Steel, stainless steel, Al, Al alloy, Ti, Ti alloy, Cu, Cu alloy, Ni, Ni alloy etc. are mentioned.
- the shape of the substrate is not particularly limited and can be appropriately selected depending on the intended use. For example, a conductive metal part processed into a linear or plate shape, or a plate processed into an uneven shape. What is processed into a required shape can be used according to uses, such as a conductive member which becomes, a component of an electronic device processed into a spring shape or a cylindrical shape.
- the thickness (diameter) and thickness (plate thickness) of a base material are not specifically limited, It can select suitably according to a use application.
- the base alloy layer is a base layer for satisfactorily forming a gold plating layer, and is made of an M1-M2-M3 alloy.
- the M1-M2-M3 alloy is composed of different elements M1, M2, and M3, and M1 is at least one element selected from Ni, Fe, Co, Cu, Zn, and Sn.
- M2 is at least one element selected from Pd, Re, Pt, Rh, Ag, and Ru, and M3 is at least one element selected from P and B.
- the method for forming the base alloy layer is not particularly limited, but can be formed by electrolytic plating, electroless plating, sputtering, or the like. And as shown below, it is especially preferable to form by electroless plating.
- M1 in the M1-M2-M3 alloy is at least one element selected from Ni, Fe, Co, Cu, Zn, and Sn. These may be used alone or in combination of two or more. For example, Ni—Fe, Ni—Co, Ni—Cu, or the like may be used.
- Each element constituting M1 is an element having a characteristic that a plating layer can be formed on a base material alone, and all have an effect of bringing the base alloy layer into close contact with the base material.
- M2 in the M1-M2-M3 alloy is at least one element selected from Pd, Re, Pt, Rh, Ag, and Ru, and these may be used alone or in combination of two or more. May be used.
- Each element constituting M2 is an element having an autocatalytic action, and all of them act as a catalyst for the reaction of the reducing agent in the plating bath when deposited on the base material, and continuously perform the metal deposition reaction. It has an advancing action.
- M2 is preferably at least one element selected from Pd and Ag, and particularly preferably Pd, from the viewpoint of cost reduction.
- M3 in the M1-M2-M3 alloy is at least one element selected from P and B. These elements may be used alone or in combination of two or more, for example, P— B may be used.
- Each element constituting M3 is a metalloid constituting a reducing agent in a plating bath for forming a base alloy layer, and is usually inevitably taken into the base alloy layer when the base alloy layer is formed. Become.
- the ratio of each element in the M1-M2-M3 alloy is preferably 20 to 50 atomic% for M1, 30 to 50 atomic% for M2, and 20 to 30 atomic% for M3.
- the M1-M2-M3 alloy has A slight amount of impurities inevitably mixed in may be included.
- impurities that are inevitably mixed include heavy metals such as Pb, Tl, and Bi that are added as stabilizers that prevent self-decomposition of the plating solution and stabilize the plating solution.
- Bi is preferably used from the viewpoint of reducing environmental burden.
- any combination of the elements can be used. From the viewpoint that self-decomposition of the plating solution can be prevented and the stability of the plating solution can be improved.
- a —Pd—P alloy and a Co—Ag—P alloy are preferable, and a Ni—Pd—P alloy is particularly preferable.
- the formation of the base alloy layer made of the M1-M2-M3 alloy is performed using a plating bath (base alloy electroless plating bath) containing the elements shown in M1, M2, and M3 and containing a reducing agent and a complexing agent. This is done by plating on the substrate.
- a plating bath base alloy electroless plating bath
- the base alloy electroless plating bath may be one obtained by mixing a commonly used nickel plating bath and palladium plating bath. Can be used.
- a nickel plating bath for example, a plating comprising a nickel salt such as nickel chloride, nickel sulfate, nickel nitrate and nickel acetate, a reducing agent containing phosphorus such as hypophosphite, and a complexing agent such as citric acid.
- a nickel salt such as nickel chloride, nickel sulfate, nickel nitrate and nickel acetate
- a reducing agent containing phosphorus such as hypophosphite
- a complexing agent such as citric acid.
- the palladium plating bath include a palladium salt such as palladium chloride, a reducing agent containing phosphorus such as hypophosphite and phosphite, and a plating bath serving as a complexing agent such as thiodiglycolic acid.
- nickel chloride as the nickel salt
- palladium chloride as the palladium salt
- the mixing ratio of the nickel plating bath and the palladium plating bath may be appropriately set according to the ratio of each element constituting the Ni—Pd—P alloy. In the above, the case where the base alloy layer is a Ni—Pd—P alloy has been exemplified.
- the base alloy layer is made of a material other than the Ni—Pd—P alloy
- the base alloy layer is preferably formed using the above-described base alloy electroless plating bath under the conditions of pH 4.0 to 7.0, bath temperature 30 to 50 ° C., and immersion time 5 to 20 minutes.
- the thickness of the base alloy layer is preferably 0.01 to 1.0 ⁇ m, more preferably 0.05 to 0.2 ⁇ m.
- the base alloy layer when the base alloy layer is formed on the base material, it may be formed directly on the base material, but in order to improve the adhesion between the base material and the base alloy layer, the modified layer May be provided.
- the modified layer can be appropriately formed according to the characteristics of the base material and the base alloy layer. From the viewpoint of improving the adhesion to the base alloy layer, M1-M2-M3 constituting the base alloy layer is used. A layer containing the same element as M1 of the alloy is preferable.
- the modified layer is preferably a Ni-based layer containing Ni which is an element corresponding to M1, and such Ni
- a Ni—P plating layer or the like can be used.
- the modified layer may be only one layer or two or more layers. In the case of two or more layers, the components constituting each layer may be different or the same. It may be a thing.
- the method for forming the modified layer is not particularly limited, but it can be formed by electrolytic plating, electroless plating, sputtering, or the like.
- the gold plating layer is a layer formed by performing electroless reduction plating treatment directly on the base alloy layer using a non-cyanide gold plating bath.
- the base alloy layer composed of the M1-M2-M3 alloy is formed on the base material, and the gold plating layer is formed on the base alloy layer by electroless reduction plating.
- a good gold plating layer having no holes can be formed. Therefore, according to the present invention, when the gold-plated coating material on which such a gold-plated layer is formed is used for various materials such as an electrical contact material, the corrosion resistance and the conductivity are reduced, or when soldering is performed. The occurrence of solder peeling can be effectively prevented.
- a gold plating layer can be formed using a non-cyanide gold plating bath by forming a layer composed of an M1-M2-M3 alloy as a base alloy layer. Therefore, it is possible to reduce the load on the work environment and the external environment. That is, there is no problem of load on the working environment and the external environment when a cyan gold plating bath is used.
- the non-cyan gold plating bath used for forming the gold plating layer is a non-cyan gold plating bath usually used for electroless reduction plating, that is, as a gold salt, chloroaurate, gold sulfite.
- a plating bath containing at least one gold thiosulfate, gold thiomalate, and the like can be used.
- the gold plating layer is preferably formed using a non-cyan gold plating bath containing the above gold salt under the conditions of pH 7.0 to 8.5 and bath temperature 55 to 65 ° C.
- the immersion time in a gold plating bath in forming the gold plating layer is not particularly limited, and can be set according to the required film thickness of the gold plating layer.
- a method of forming a gold plating layer on a base material a method of forming a gold plating layer directly by performing an electroless displacement gold plating process on a base material has been conventionally used.
- the metal base material that is the material to be plated may be locally eluted, resulting in the formation of recesses on the surface of the metal base material.
- gold does not appropriately precipitate in the generated concave portion, and pinholes are generated on the surface of the formed gold plating layer.
- the electroless gold plating method of the present invention by forming a layer composed of the M1-M2-M3 alloy as the base alloy layer, without performing the electroless displacement gold plating process, Such a problem of pinholes can be solved by forming a gold plating layer by electroless reduction plating.
- a gold plating layer can be satisfactorily formed by electroless reduction plating by forming a layer composed of an M1-M2-M3 alloy as the base alloy layer. In order to solve the pinhole problem described above, it is not necessary to increase the thickness of the gold plating layer.
- the electroless gold plating method disclosed in the above-mentioned Patent Document 1 Japanese Patent Laid-Open No. 2005-54267
- a palladium plating layer is formed by performing electroless reduction palladium plating on a substrate.
- a method of forming a gold plating layer on the palladium plating layer by electroless reduction gold plating uses a cyan-based gold plating bath when forming the gold plating layer.
- a gold plating layer can be formed using a non-cyanide gold plating bath, and the load on the work environment and the external environment is reduced. It becomes possible to reduce.
- the thickness of the gold plating layer is preferably 1 to 200 nm, more preferably 5 to 100 nm. If the thickness of the gold plating layer is too thin, a uniform gold plating layer is not formed on the underlying alloy layer, and when used as a gold plating coating material, the corrosion resistance, conductivity, and solderability may be reduced. On the other hand, if the thickness of the gold plating layer is too thick, it is disadvantageous in terms of cost.
- a base alloy layer composed of an M1-M2-M3 alloy is formed on a substrate, and a gold plating layer is formed thereon by electroless reduction plating. Therefore, it is possible to provide a gold plating coating material having a good gold plating layer having no pinholes and having excellent corrosion resistance, conductivity, and solderability.
- a gold plating coating material according to the present invention is suitably used as an electrical contact material used for a connector, a switch, a printed wiring board or the like.
- such a gold plating coating material according to the present invention is suitably used as a fuel cell separator which is a member of a fuel cell.
- the separator for a fuel cell has an uneven surface that functions as a flow path for fuel gas or air on its surface, and plays a role of collecting electrons generated at the electrode. A layer needs to be formed, and further, corrosion resistance and conductivity are required.
- the gold plating coating material according to the present invention is one in which a gold plating layer is formed by electroless reduction plating, a gold plating layer is formed well even on uneven portions, and excellent corrosion resistance, Since it has conductivity, it can be suitably used as such a fuel cell separator.
- Example 1 5000 series 5086 aluminum alloy specified in JIS H4000 (Si: 0.4 wt%, Fe: 0.5 wt%, Cu: 0.1 wt%, Mn: 0.2 wt%, Mg: 3.5
- the surface has an arithmetic average roughness Ra of 0.1 nm and a thickness of 10 ⁇ m by electroless plating on Zn: 0.25 wt%, Cr: 0.25 wt%, Al: balance).
- a base material having a total thickness of 1.27 mm on which a Ni—P layer (P content: 12% by weight) was formed was prepared.
- the prepared base material was degreased, washed with water, and a 2 ⁇ m-thickness was formed on the base material by electroless plating using a Ni—P plating bath (Okuno Pharmaceutical Co., Ltd., ICP Nicolon GM-NP).
- a Ni—P plating layer (P content: 7 wt%) was formed.
- a Ni—Pd—P alloy layer having a thickness of 0.79 ⁇ m was formed on the Ni—P plating layer by performing plating treatment at 40 ° C. for 7 minutes.
- the palladium salt, reducing agent, and complexing agent in the plating bath conventionally known compounds were used.
- the base material on which the Ni—P plating layer and the Ni—Pd—P alloy layer were formed using a non-cyan electroless reduction gold plating bath (Okino Pharmaceutical Co., Ltd., Self Gold OTK) at 60 ° C.
- An electroless reduction plating treatment was performed for 4 minutes to form a gold plating layer having a thickness of 55 nm on the Ni—Pd—P alloy layer, thereby obtaining a gold plating coating material.
- the evaluation of adhesion was performed on the gold plating layer of the gold plating coating material. Specifically, the adhesion is evaluated by applying a peel test after applying an adhesive tape (made by Nichiban Co., Ltd., Ny stack strong type) to the gold plating layer of the gold plating coating material, and then gold plating. The peeled state of the layer was observed and evaluated according to the following criteria. The evaluation results are shown in Table 1. ⁇ : No peeling of the gold plating layer was confirmed. X: Peeling of the gold plating layer occurred.
- IM-PT manufactured by Japan High Purity Chemical Co., Ltd.
- a Pd plating bath (Okuno Seiyaku Kogyo Co., Ltd., Paratop) is used for electroless plating to form a palladium plating with a thickness of 0.5 ⁇ m on the Ni—P plating layer.
- a layer was formed, and a non-cyanide electroless reduction gold plating bath (Okino Pharmaceutical Co., Ltd., self-gold OTK) was directly applied on the formed palladium plating, except that electroless reduction plating treatment was performed.
- a gold plating coating material was obtained in the same manner as in Example 1 and evaluated in the same manner. The evaluation results are shown in Table 1.
- a Ni—Pd—P alloy layer, a Ni—Pt—P alloy layer, and a Co—Pd—P alloy layer were formed as the base alloy layer.
- the formed gold plating layer was uneven plating. The appearance was good, no gold deposits were observed, and the adhesion was also good.
- Comparative Example 1 in which such a base alloy layer was not formed, the gold plating layer was not formed, and therefore the adhesion of the gold plating layer could not be measured.
- Comparative Example 2 in which a palladium plating layer was formed instead of the base alloy layer, the gold plating layer had a very low coverage, and in addition, the adhesion was low.
- FIG. 1A shows the first embodiment
- FIG. 1B shows the second embodiment
- FIG. 1C shows the third embodiment
- FIG. 1D shows the first comparative example
- FIG. ) Corresponds to Comparative Example 2, respectively.
- the gold plating layer was uniformly formed as shown in FIGS. 1 (A) to 1 (C).
- Comparative Example 1 shows that no gold plating layer was formed on the Ni—P plating layer.
- Comparative Example 2 as shown in FIG. 1 (E), the gold plating layer (white portion in FIG. 1 (E)) was formed unevenly, and gold non-deposited portions were scattered.
- Example 4 The thickness of the gold plating layer to be formed is changed to 36 nm (Example 4), 49 nm (Example 5), and 63 nm (implementation) by changing the immersion time in electroless reduction plating when forming the gold plating layer.
- a gold plating coating material was obtained in the same manner as in Example 1 except that Example 6) was used.
- ⁇ Comparative Example 3> For Comparative Example 3, a non-cyanide electroless displacement gold plating bath (Okuno Pharmaceutical Co., Ltd., Flash Gold NC) was directly formed on the Ni—P plating layer without forming the Ni—Pd—P alloy layer. The electroless displacement plating treatment was performed at 55 ° C. for 1 minute, and then at 60 ° C., 1 ° C. using a non-cyan electroless reduction gold plating bath (Okino Pharmaceutical Co., Ltd., Self Gold OTK). A gold-plated coating material was obtained in the same manner as in Example 1 except that the electroless reduction plating treatment was performed under the condition of minutes and a gold-plated layer having a thickness of 35 nm was formed.
- a non-cyanide electroless displacement gold plating bath (Okuno Pharmaceutical Co., Ltd., Flash Gold NC) was directly formed on the Ni—P plating layer without forming the Ni—Pd—P alloy layer.
- the electroless displacement plating treatment was performed at 55 ° C. for 1 minute
- the obtained gold plating coating materials were evaluated for corrosion resistance. Specifically, the corrosion resistance was evaluated by masking the gold plating coating material with polyimide tape so that the area of 35 mm in length and 20 mm in width was exposed, and immersed in a 90 ° C. sulfuric acid aqueous solution (volume 80 ml, pH: 1) for 50 hours. After that, the gold plating coating material is taken out, and the concentration of ions (Ni, Pd, P) eluted from the gold plating coating material in the sulfuric acid aqueous solution is measured by an inductively coupled plasma emission spectrometer (ICPE-9000, manufactured by Shimadzu Corporation).
- ICPE-9000 inductively coupled plasma emission spectrometer
Abstract
Description
本発明の無電解金めっき処理方法により得られる金めっき被覆材料は、基材上に、下地合金層と、金めっき層と、を備え、前記下地合金層が、M1-M2-M3合金(ただし、M1は、Ni、Fe、Co、Cu、Zn、およびSnから選択される少なくとも1つの元素、M2は、Pd、Re、Pt、Rh、Ag、およびRuから選択される少なくとも1つの元素、M3は、P、およびBから選択される少なくとも1つの元素である。)であることを特徴とする。
基材としては、特に限定されないが、鋼、ステンレス鋼、Al、Al合金、Ti、Ti合金、Cu、Cu合金、Ni、Ni合金などが挙げられる。基材の形状としては、特に限定されず、使用用途に応じて適宜選択することができるが、たとえば、線状や板状に加工された導電性の金属部品、板を凹凸状に加工してなる導電性部材、ばね状や筒状に加工された電子機器の部品などの用途に応じて必要な形状に加工したもの用いることができる。また、基材の太さ(直径)や厚み(板厚)は、特に限定されず、使用用途に応じて適宜選択することができる。
下地合金層は、金めっき層を良好に形成するための下地層であり、M1-M2-M3合金からなる。ここで、M1-M2-M3合金は、互いに異なる元素であるM1、M2、およびM3から構成され、M1は、Ni、Fe、Co、Cu、Zn、およびSnから選択される少なくとも1つの元素であり、また、M2は、Pd、Re、Pt、Rh、Ag、およびRuから選択される少なくとも1つの元素であり、さらに、M3は、P、およびBから選択される少なくとも1つの元素である。
金めっき層は、下地合金層上に、直接、非シアン系の金めっき浴を用いて、無電解還元めっき処理を施すことにより形成される層である。
JIS H4000に規定された5000系の5086アルミニウム合金(Si:0.4重量%、Fe:0.5重量%、Cu:0.1重量%、Mn:0.2重量%、Mg:3.5重量%、Zn:0.25重量%、Cr:0.25重量%、Al:残部)上に、無電解めっきにより、表面の算術平均粗さRaが0.1nmであり、厚みが10μmであるNi-P層(Pの含有割合が12重量%)が形成された、総厚1.27mmの基材を準備した。次いで、準備した基材を脱脂した後、水洗し、Ni-Pめっき浴(奥野製薬工業社製、ICPニコロンGM-NP)を用いて、無電解めっきにより、基材上に、厚さ2μmのNi-Pめっき層(Pの含有割合が7重量%)を形成した。
<Pdめっき浴>
パラジウム塩:Pdめっき浴中におけるPdが0.15重量%となる量
還元剤:1.8重量%
錯化剤:0.63重量%
水:97.2重量%
pH:5.8
<Ni-Pめっき浴>
ニッケル塩(塩化ニッケル):1.8重量%
還元剤(次亜燐酸ナトリウム):2.4重量%
錯化剤:2.4重量%
水:93.2重量%
pH:5.2
そして、このようにして得られた金めっき被覆材料について、目視、および走査型電子顕微鏡(日立ハイテクノロジーズ社製、S-4800)にて観察し、得られた金めっき被覆材料の表面について、金めっき層の外観、および金の未析出部の有無を確認した。評価結果を表1に示す。
次いで、金めっき被覆材料の金めっき層に対し、密着性の評価を行った。密着性の評価は、具体的には、金めっき被覆材料の金めっき層に粘着テープ(ニチバン社製、ナイスタック強力タイプ)を貼付した後、剥がすことにより剥離試験を実施し、その後、金めっき層の剥離状態を観察して、以下の基準で評価した。評価結果を表1に示す。
○:金めっき層の剥離が確認されなかった。
×:金めっき層の剥離が発生した。
上述したNi-Pd-P合金層に代えて、Ptめっき浴(日本高純度化学社製、IM-PT)と、上述したNi-Pd-P合金層を形成する際に用いたNi-Pめっき浴とを、Ptめっき浴:Ni-Pめっき浴=3:7(体積比)の割合で混合しためっき浴を用いて、35℃、10分間、pH4.0の条件で、めっき処理を施すことにより、Ni-Pめっき層上に、厚さ50nmのNi-Pt-P合金層を形成し、さらに、金めっき層を形成する際の、無電解還元めっき処理における浸漬時間などを変更することにより、厚さ5nmの金めっき層を形成した以外は、実施例1と同様にして金めっき被覆材料を得て、同様に評価を行った。評価結果を表1に示す。
上述したNi-Pd-P合金層に代えて、Pdめっき浴(奥野製薬工業社製、パラトップ)と、下記に示すCoめっき浴とを、Pdめっき浴:Coめっき浴=1:6(体積比)の割合で混合しためっき浴を用いて、60℃、10分間、pH8.5の条件で、めっき処理を施すことにより、Ni-Pめっき層上に、厚さ50nmのCo-Pd-P合金層を形成し、さらに、金めっき層を形成する際の、無電解還元めっき処理における浸漬時間などを変更することにより、厚さ5nmの金めっき層を形成した以外は、実施例1と同様にして金めっき被覆材料を得て、同様に評価を行った。評価結果を表1に示す。
<Coめっき浴>
コバルト塩(硫酸コバルト):10g/L
還元剤(次亜燐酸ナトリウム):25g/L
錯化剤(クエン酸3ナトリウム):30g/L
錯化剤(酒石酸ナトリウム):30g/L
錯化剤(グリシン):7.58g/L
酢酸鉛:0.3ppm
上述したNi-Pd-P合金層を形成せずに、Ni-Pめっき層上に、直接、非シアン系の無電解還元金めっき浴(奥野製薬工業社製、セルフゴールドOTK)を用いて、無電解還元めっき処理を施した以外は、実施例1と同様にして金めっき被覆材料を得て、同様に評価を行った。評価結果を表1に示す。
Ni-Pd-P合金層を形成する代わりに、Pdめっき浴(奥野製薬工業社製、パラトップ)を用いて、無電解めっきにより、Ni-Pめっき層上に厚さ0.5μmのパラジウムめっき層を形成し、形成したパラジウムめっき上に、直接、非シアン系の無電解還元金めっき浴(奥野製薬工業社製、セルフゴールドOTK)を用いて、無電解還元めっき処理を施した以外は、実施例1と同様にして金めっき被覆材料を得て、同様に評価を行った。評価結果を表1に示す。
金めっき層を形成する際の、無電解還元めっきにおける浸漬時間などを変更して、形成される金めっき層の厚みを、36nm(実施例4)、49nm(実施例5)、および63nm(実施例6)とした以外は、実施例1と同様にして金めっき被覆材料を得た。
比較例3については、Ni-Pd-P合金層を形成せず、Ni-Pめっき層上に、直接、非シアン系の無電解置換金めっき浴(奥野製薬工業社製、フラッシュゴールドNC)を用いて、55℃、1分間の条件で無電解置換めっき処理を施し、次いで、非シアン系の無電解還元金めっき浴(奥野製薬工業社製、セルフゴールドOTK)を用いて、60℃、1分間の条件で無電解還元めっき処理を施し、厚さ35nmの金めっき層を形成した以外は、実施例1と同様にして金めっき被覆材料を得た。
金めっき層を形成する際の、無電解還元めっきにおける浸漬時間などを変更して、形成される金めっき層の厚みを、78nm(比較例4)、132nm(比較例5)、および186nm(比較例6)とした以外は、比較例3と同様にして金めっき被覆材料を得た。
次いで、実施例4~6、および比較例3~6においては、得られた金めっき被覆材料に対し、耐食性の評価を行った。耐食性の評価は、具体的には、金めっき被覆材料を縦35mm、横20mmの面積が露出するようにポリイミドテープでマスキングし、90℃の硫酸水溶液(体積80ml、pH:1)に50時間浸漬した後、金めっき被覆材料を取り出し、金めっき被覆材料から硫酸水溶液中に溶出したイオン(Ni、Pd、P)の濃度を誘導結合プラズマ発光分析装置(島津製作所社製、ICPE-9000)により測定することにより行った。結果を図2に示す。なお、図2に示す結果は、比較例3における、金めっき層の厚みが35nmであるときのイオン(Ni、Pd、P)溶出濃度を100として、相対値で示している。
Claims (2)
- 基材上に、下地合金層を形成する工程と、
前記下地合金層上に、直接、非シアン系の金めっき浴を用いて、無電解還元めっきにより金めっき層を形成する工程と、を有する無電解金めっき処理方法であって、
前記下地合金層が、M1-M2-M3合金(ただし、M1は、Ni、Fe、Co、Cu、Zn、およびSnから選択される少なくとも1つの元素、M2は、Pd、Re、Pt、Rh、Ag、およびRuから選択される少なくとも1つの元素、M3は、P、およびBから選択される少なくとも1つの元素である。)であることを特徴とする無電解金めっき処理方法。 - 基材と、
前記基材上に形成された下地合金層と、
前記下地合金層上に形成された金めっき層と、を備える金めっき被覆材料であって、
前記下地合金層が、M1-M2-M3合金(ただし、M1は、Ni、Fe、Co、Cu、Zn、およびSnから選択される少なくとも1つの元素、M2は、Pd、Re、Pt、Rh、Ag、およびRuから選択される少なくとも1つの元素、M3は、P、およびBから選択される少なくとも1つの元素である。)であることを特徴とする金めっき被覆材料。
Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US14/414,655 US9388497B2 (en) | 2012-07-13 | 2013-07-11 | Method of electroless gold plating |
EP13816391.0A EP2873752B1 (en) | 2012-07-13 | 2013-07-11 | Electroless gold plating method and gold-plate-coated material |
CN201380037493.XA CN104471109B (zh) | 2012-07-13 | 2013-07-11 | 化学镀金处理方法和镀金覆盖材料 |
JP2014524860A JP6231982B2 (ja) | 2012-07-13 | 2013-07-11 | 無電解金めっき処理方法、および金めっき被覆材料 |
US15/163,437 US20160265115A1 (en) | 2012-07-13 | 2016-05-24 | Method of electroless gold plating |
US15/163,419 US10006125B2 (en) | 2012-07-13 | 2016-05-24 | Gold plate coated material |
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JP2012157180 | 2012-07-13 | ||
JP2012-157180 | 2012-07-13 |
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US14/414,655 A-371-Of-International US9388497B2 (en) | 2012-07-13 | 2013-07-11 | Method of electroless gold plating |
US15/163,437 Continuation US20160265115A1 (en) | 2012-07-13 | 2016-05-24 | Method of electroless gold plating |
US15/163,419 Division US10006125B2 (en) | 2012-07-13 | 2016-05-24 | Gold plate coated material |
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WO2014010662A1 true WO2014010662A1 (ja) | 2014-01-16 |
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US (3) | US9388497B2 (ja) |
EP (1) | EP2873752B1 (ja) |
JP (1) | JP6231982B2 (ja) |
CN (1) | CN104471109B (ja) |
WO (1) | WO2014010662A1 (ja) |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2014116121A (ja) * | 2012-12-07 | 2014-06-26 | Toyo Kohan Co Ltd | 燃料電池用セパレータ、燃料電池セル、燃料電池スタック、および燃料電池用セパレータの製造方法 |
JP2015155566A (ja) * | 2014-02-21 | 2015-08-27 | 三菱瓦斯化学株式会社 | 無電解めっき液 |
EP3064611A4 (en) * | 2013-10-28 | 2017-04-12 | Toyo Kohan Co., Ltd. | Alloy-plate-coated material, and method for producing alloy-plate-coated material |
CN110325665A (zh) * | 2017-06-28 | 2019-10-11 | 小岛化学药品株式会社 | 无电解镀敷工艺 |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP2873752B1 (en) | 2012-07-13 | 2020-05-20 | Toyo Kohan Co., Ltd. | Electroless gold plating method and gold-plate-coated material |
JP6651271B2 (ja) * | 2017-02-15 | 2020-02-19 | 三菱電機株式会社 | 半導体素子及びその製造方法 |
EP4006201A4 (en) * | 2019-07-31 | 2023-11-29 | Resonac Corporation | LAMINATE AND METHOD FOR PRODUCING THEREOF |
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WO2007116769A1 (ja) * | 2006-03-27 | 2007-10-18 | Nippon Sheet Glass Company, Limited | 金色調を有する光輝性顔料、これを含有する化粧料、塗料、インク、または樹脂組成物 |
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EP2873752B1 (en) * | 2012-07-13 | 2020-05-20 | Toyo Kohan Co., Ltd. | Electroless gold plating method and gold-plate-coated material |
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2013
- 2013-07-11 EP EP13816391.0A patent/EP2873752B1/en active Active
- 2013-07-11 US US14/414,655 patent/US9388497B2/en active Active
- 2013-07-11 WO PCT/JP2013/068956 patent/WO2014010662A1/ja active Application Filing
- 2013-07-11 JP JP2014524860A patent/JP6231982B2/ja active Active
- 2013-07-11 CN CN201380037493.XA patent/CN104471109B/zh active Active
-
2016
- 2016-05-24 US US15/163,419 patent/US10006125B2/en active Active
- 2016-05-24 US US15/163,437 patent/US20160265115A1/en not_active Abandoned
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JPH05335315A (ja) * | 1992-06-02 | 1993-12-17 | Seiko Epson Corp | 電極の製造方法 |
JP2005054267A (ja) | 2003-07-24 | 2005-03-03 | Electroplating Eng Of Japan Co | 無電解金めっき方法 |
WO2007116769A1 (ja) * | 2006-03-27 | 2007-10-18 | Nippon Sheet Glass Company, Limited | 金色調を有する光輝性顔料、これを含有する化粧料、塗料、インク、または樹脂組成物 |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2014116121A (ja) * | 2012-12-07 | 2014-06-26 | Toyo Kohan Co Ltd | 燃料電池用セパレータ、燃料電池セル、燃料電池スタック、および燃料電池用セパレータの製造方法 |
EP3064611A4 (en) * | 2013-10-28 | 2017-04-12 | Toyo Kohan Co., Ltd. | Alloy-plate-coated material, and method for producing alloy-plate-coated material |
US10000038B2 (en) | 2013-10-28 | 2018-06-19 | Toyo Kohan Co., Ltd. | Alloy plate coated material and method of producing alloy plate coated material |
JP2015155566A (ja) * | 2014-02-21 | 2015-08-27 | 三菱瓦斯化学株式会社 | 無電解めっき液 |
CN110325665A (zh) * | 2017-06-28 | 2019-10-11 | 小岛化学药品株式会社 | 无电解镀敷工艺 |
Also Published As
Publication number | Publication date |
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US20160265115A1 (en) | 2016-09-15 |
US20150176134A1 (en) | 2015-06-25 |
US9388497B2 (en) | 2016-07-12 |
CN104471109A (zh) | 2015-03-25 |
CN104471109B (zh) | 2017-05-24 |
EP2873752A1 (en) | 2015-05-20 |
EP2873752B1 (en) | 2020-05-20 |
EP2873752A4 (en) | 2016-03-23 |
JPWO2014010662A1 (ja) | 2016-06-23 |
US20160265114A1 (en) | 2016-09-15 |
JP6231982B2 (ja) | 2017-11-15 |
US10006125B2 (en) | 2018-06-26 |
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