EP3550057A2 - Revêtement de surface multicouche - Google Patents

Revêtement de surface multicouche Download PDF

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Publication number
EP3550057A2
EP3550057A2 EP19167150.2A EP19167150A EP3550057A2 EP 3550057 A2 EP3550057 A2 EP 3550057A2 EP 19167150 A EP19167150 A EP 19167150A EP 3550057 A2 EP3550057 A2 EP 3550057A2
Authority
EP
European Patent Office
Prior art keywords
layer
surface coating
gold
multilayer surface
ausführungsform
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP19167150.2A
Other languages
German (de)
English (en)
Other versions
EP3550057A3 (fr
Inventor
Stefan LEHNIG
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Surpro GmbH
Original Assignee
Supro GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Supro GmbH filed Critical Supro GmbH
Publication of EP3550057A2 publication Critical patent/EP3550057A2/fr
Publication of EP3550057A3 publication Critical patent/EP3550057A3/fr
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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
    • 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
    • C25D5/627—Electroplating characterised by the visual appearance of the layers, e.g. colour, brightness or mat appearance
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00—Electroplating characterised by the article coated
    • C25D7/005—Jewels; Clockworks; Coins
    • 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
    • C25D3/56—Electroplating: Baths therefor from solutions of alloys
    • C25D3/567—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of platinum group metals
    • 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
    • C25D3/56—Electroplating: Baths therefor from solutions of alloys
    • C25D3/62—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of gold

Definitions

  • the present invention relates to a multilayer surface coating, an article comprising the multilayer surface coating, the use of a silver layer for the manufacture or use in the manufacture of a multilayer surface coating, the use of a palladium nickel alloy layer for the manufacture or for use in the manufacture of a multilayer surface coating , the use of a gold layer for the manufacture or for use in the manufacture of a multilayer surface coating, the use of a palladium layer for the manufacture or for use in the manufacture of a multilayer surface coating, a process for producing a multilayer surface coating, and a process for providing a multilayer Surface coating on an article.
  • Such surface coatings find a variety of applications such as in writing instruments or body jewelry.
  • Such surface coatings of the prior art have a layer structure with a base layer of nickel.
  • a body surface such as a finger or the neck of a human
  • release of nickel occurs, which can cause undesirable reactions in humans.
  • the object of the present invention is to provide a surface coating which prevents the release of nickel.
  • Another object of the present invention is to prevent the release of nickel from a surface coating, at least to the extent that the criteria of the nickel release test according to DIN EN 1811: 2015-10 and the guidelines of the European Chemicals Agency, ECA, more specifically of entry 27 of Annex XVII of REACH Regulation (EC) 1907/2006.
  • the object underlying the present invention is achieved in a first aspect, which is also a first embodiment of the first aspect, by a multilayer surface coating comprising a first layer and a second layer, wherein the first layer comprises a silver layer, a pre-gold layer or a gold layer and the second layer is an alloy layer of palladium nickel or a palladium layer.
  • the object underlying the present invention is achieved in a second aspect, which is also a first embodiment of the second aspect, by a multilayer surface coating comprising a first layer, a second layer and a third layer, wherein the first layer is a layer of pre-gold is, the second layer is a first gold layer and the third layer is a second layer of gold.
  • the object underlying the present invention is achieved in a third aspect, which is also a first embodiment of the third aspect, by an article comprising a multilayer surface coating according to the first and / or second aspect, including any embodiment thereof.
  • a fourth aspect which is also a first embodiment of the fourth aspect, by the use of a silver layer as described in connection with the first aspect, including any embodiment thereof, for the production or the Use in the manufacture of a multilayer surface coating according to the first aspect, including any embodiment thereof, wherein the silver layer is the first layer.
  • a fifth aspect which is also a first embodiment of the fifth aspect, by the use of a pre-gold layer as described in connection with the first aspect, including any embodiment thereof, for the production or the Use in the manufacture of a multilayer surface coating according to the first aspect, including any embodiment thereof, wherein the pre-gold layer is the first layer.
  • the object underlying the present invention is achieved in a sixth aspect, which is also a first embodiment of the sixth aspect, by the use of an alloy layer of palladium nickel as described in connection with the first aspect, including each embodiment thereof, for the production or for use in producing a multilayer surface coating according to the first aspect, including any embodiment thereof, wherein the palladium nickel alloy layer is the second layer.
  • a seventh aspect which is also a first embodiment of the seventh aspect, by the use of a gold layer as in the first aspect, including any embodiment thereof, described for manufacture or use in the manufacture of a multilayer surface coating according to the first aspect, including any embodiment thereof, wherein the gold layer is the third layer.
  • an eighth aspect which is also a first embodiment of the eighth aspect, by the use of a palladium layer as in the first aspect, including any embodiment thereof, described for manufacture or use in the production of a multilayer surface coating according to the first aspect, including any embodiment thereof, wherein the palladium layer is the second layer.
  • the object underlying the present invention is solved in an eleventh aspect, which is also a first embodiment of the eleventh aspect, by a method of providing a multi-layer surface coating on an article, wherein the article comprises a base material on a surface and the method Method according to the ninth and / or tenth aspect, including any embodiment thereof.
  • the present inventor assumes that the first layer serves as a base layer and replaces the nickel-based base layer of multilayer surface coatings according to the prior art.
  • layers are formed from or comprise pre-gold.
  • gold is a gold having a cobalt foreign metal content of from 0.3% to 1% by weight.
  • pre-gold is the pre-gold available under the trade name Auruna 311.
  • the layer formed from gold has a layer thickness of 0.1 .mu.m to 5 .mu.m.
  • the second layer of the multilayer surface coating according to the invention formed from a first gold layer is one made of gold, wherein the gold has an external metal content of from 0.1% by weight to 3% by weight.
  • the composition may consist of or comprise gold and iron or gold and cobalt.
  • the Fe content of the gold layer is 0.3 wt .-% to 0.5 wt .-%.
  • the thickness of the gold layer is 0.5 ⁇ m to 4 ⁇ m.
  • the third layer of the multilayer surface coating formed of a second gold layer is one of gold containing nickel and indium, which is preferably a ternary alloy of Au, Ni and In.
  • the proportion of these ingredients, particularly Ni and In may vary within a range of 0.1% to 5% by weight; preferred is a content of Ni and / or In of 0.3 wt .-%.
  • the thickness of the layer of Au, Ni and In, in particular the thickness of the second gold layer formed therefrom or existing is 0.1 ⁇ m to 3 ⁇ m.
  • the present invention appears to be based on that in a multilayer surface coating of the prior art comprising a layer of palladium-nickel or an alloy layer of palladium nickel and a nickel layer of nickel from the base layer
  • the pores of the layer of palladium-nickel or alloy layer of palladium nickel passes through and thus reaches the surface when the multilayer surface coating comes into contact with an electrolyte.
  • the nickel of the base layer behaves as a sacrificial anode as a result of the residual stress potentials of the individual (metal) layers, dissolves and comes to the surface of the multilayer surface coating, where it can trigger the unwanted reactions, especially skin irritation in humans.
  • the base layer is formed from a silver layer, a pre-gold layer or a gold layer, these processes do not occur.
  • the release of nickel is determined by means of the nickel release test according to DIN EN 1811: 2015-10.
  • the multilayer surface coating according to the present invention satisfies the nickel release test according to DIN EN 1811: 2015-10.
  • the multilayer surface coating according to the invention prevents the release of nickel at least to the extent that the criteria of the nickel release test according to DIN EN 1811: 2015-10 as well as the Guidelines of the European Chemicals Agency, ECA, more precisely of entry 27 of Annex XVII of REACH Regulation (EC) 1907/2006.
  • the release of nickel, in particular from the palladium nickel alloy layer is less than 0.5 ⁇ g Ni / cm 2 surface area of an article / week comprising the multilayer surface coating according to the invention.
  • the pre-gold layer serves as an adhesive layer, i. provides or improves adhesion between the two layers between which the pre-gold layer is disposed.
  • the thickness of the pre-gold layer can be adapted to this function, i. it is chosen so that its function as an adhesive layer is guaranteed. The determination of this strength is known to those skilled in the art and is performed in routine tests. It will be appreciated by those skilled in the art that a pre-gold layer as used in the present invention differs from a gold layer, first gold layer or second gold layer only in its strength; in terms of composition, the disclosure provided herein applies to the gold layer, first gold layer, and second gold layer used in accordance with the present invention, which is incorporated herein by reference.
  • a gold layer is provided.
  • This may be a pre-gold layer which, in one embodiment, has a content of cobalt of 0.3% by weight.
  • a pre-gold layer can have a particularly high layer hardness, expressed as Vickers hardness (HV).
  • HV Vickers hardness
  • a pure gold layer may have a hardness of 180-260 HV.
  • the gold layer is applied with a thickness of preferably 1 ⁇ m or less, in particular if it is a pre-gold layer.
  • the preferred minimum thickness of the gold layer, especially if it is a pre-gold layer of gold is 0.1 ⁇ m.
  • a layer thickness of 0.1 ⁇ m is typically required to provide a covering gold layer; covering preferably means that the surface formed by the gold layer is clearly recognizable as a gold surface and / or (an) underlying layer (s) are not recognizable as such, in particular with the unaided eye.
  • a layer thickness of at least 0.1 ⁇ m is preferably sufficient to ensure a positive test course in a nickel release test according to DIN 1811. However, a layer thickness of more than 0.1 .mu.m may be required in order to give the layer an optionally increased chemical or mechanical stability, in particular against mechanical abrasion. The same applies to the first and second gold layers.
  • the gold layer is different from a pre-gold.
  • This gold layer which differs from a pre-gold, preferably has a content of one or more foreign metals.
  • the one or more foreign metals selected from the group include iron, nickel, indium, cobalt, palladium and copper.
  • the foreign metal present in the gold layer is iron.
  • nickel and indium are contained in the gold layer.
  • a content of one or more foreign metals in the gold layer preferably leads to an increase in the hardness of the gold layer.
  • Such a gold layer alloyed with one or more foreign metals is also referred to as a hard gold layer.
  • a content of one or more foreign metals in the gold layer results in obtaining a more advantageous coating result.
  • the coating result can be determined by a film adhesion test, as known to those skilled in the art.
  • the hardness of such a hard gold layer is up to 280 HV. In one embodiment, it is provided that the gold content in the gold layer is at least 97.5 wt .-%. In one embodiment of the invention, the gold content of the gold layer is at least 50% by weight.
  • the effects of adding one or more foreign metals to a gold layer or a melt forming a gold layer are known to those skilled in the art. Thus, the addition of copper, preferably 50% by weight, results in the formation of a pink gold layer.
  • the gold layer has a content of nickel and indium, it is provided that the content of nickel and the content of indium are the same. In an alternative embodiment, it is provided that the content of nickel is different from the content of indium.
  • gold layer pre-gold layer, first gold layer and / or second pre-gold layer.
  • gold alloy is Auruna 311, supplied by Umicore, Sch Reginabisch Gmünd, Germany.
  • a gold layer is present in a multilayer surface coating according to the present invention.
  • more than one gold layer is present in a multilayer surface coating in accordance with the present invention.
  • the formation of a gold layer in a multilayer surface coating according to the present invention from a plurality of gold layers or partial gold layers may be necessary or advantageous where different deposition rates for individual (partial) gold layers should or can be realized in the multilayer surface coating.
  • a gold layer in a multilayer surface coating according to the present invention may be required or advantageous from multiple gold layers or partial gold layers where a lighter gold hue is desired, formed by a gold layer of multiple gold layers or partial gold layers a lighter gold hue compared to a Gold layer of a gold layer or partial gold layer.
  • a silver layer is provided as the first layer.
  • the silver content of the silver layer is at least 99.7% by weight.
  • the silver content of the silver layer is less than 99.7 wt .-%.
  • the minimum silver content of the silver layer can be determined by those skilled in the art through routine testing. It will be appreciated by those skilled in the art that the level of silver can be significantly defined by the degree of purity of the electrodeposited silver.
  • the thickness of the silver layer is about 2 ⁇ m to about 15 ⁇ m. It will be appreciated by those skilled in the art that this thickness of the silver layer is essentially due to the deposition process and / or coating process, more specifically the current density ranges applied thereto. Preferably, the thickness of the silver layer is about 5 ⁇ m.
  • the second layer is an alloy layer of palladium nickel.
  • the palladium content is about 75% by weight to 85% by weight.
  • the palladium content of the palladium nickel alloy layer is 100% by weight, i. the alloy layer of palladium nickel is actually a palladium layer.
  • the thickness of the palladium nickel alloy layer is about 1 ⁇ m to 10 ⁇ m; the minimum thickness of the palladium nickel alloy layer is defined by the fact that the palladium nickel alloy layer functions as a barrier layer, more specifically as a diffusion barrier.
  • the diffusion barrier prevents diffusion of silver into the gold.
  • the thickness of one or more of the layers forming the multilayer surface coating according to the first and second aspects of the invention may have a certain range of variation.
  • the fluctuation range preferably depends on the different current density ranges of the respective coating electrolytes, ie the electrolytes used for the formation of the respective layer of the multilayer surface coating.
  • These ranges of variation are, preferably, for silver -50% / + 100%, for a palladium-nickel alloy -50% / + 100% and for gold -50% / + 50%. Accordingly, with an average thickness of a silver layer of 5 ⁇ m, a scatter of min. 2.5 ⁇ m to max.
  • the multilayer surface coating serves for corrosion protection, preferably technical corrosion protection.
  • the corrosion protection is detected by a test familiar to the person skilled in the art, such as, for example, a salt spray test or a hand sweat test. It will be appreciated by those skilled in the art that the scope of the corrosion protection sought or to be achieved has an effect on the thickness of one or more of the layers forming the multilayer surface coating of the first and second aspects of the invention and performs this layer (s) accordingly to provide the scope of the desired or to be implemented corrosion protection.
  • the multilayer surface coating is used for decorative metal finishing.
  • the base material is selected from the group comprising non-ferrous metals, steels and stainless steels.
  • a non-ferrous metal is one consisting of a copper alloy or pure copper.
  • a preferred copper alloy is brass.
  • the article to which the multilayer surface coating of the invention is applied is made of the base material.
  • the object underlying the present invention is solved in a third aspect by an article comprising a multilayer surface coating according to the first aspect and the second aspect of the present invention, including any embodiment thereof.
  • such an article may be any article made of a metal and, preferably, serving a decorative purpose.
  • the article is a product which is in contact with or suitable for skin, preferably human skin.
  • the article is selected from the group comprising a writing utensil, a jewelery article, a body jewelry article, a pair of glasses and an accessory.
  • the multilayer surface coating is a multi-layer surface coating according to the first aspect of the present invention, including any embodiment thereof.
  • the multi-layer surface coating is a multi-layer surface coating according to the second aspect of the present invention, including each embodiment thereof.
  • an indication of a metal or alloy layer means that there is a layer comprising the metal or alloy, preferably consisting of the metal or alloy.
  • Fig. 1 shows a micrograph of a multilayer surface coating according to the present invention, which is applied to a base material.
  • the silver layer serving as the base layer is applied directly to the base material.
  • the silver layer is immediately followed by an alloy layer of palladium nickel.
  • the palladium nickel alloy layer is provided with a gold layer serving as a third layer, which finishes the multilayer surface coating and thus is that layer which can come in contact with the environment, for example, the skin of a human.
  • Fig. 2 shows a micrograph of a multilayer surface coating according to the prior art comprising a base layer of nickel, which on a base material is applied.
  • the base layer of nickel immediately follows an alloy layer of palladium nickel.
  • the palladium nickel alloy layer is provided with a gold layer serving as a third layer, which finishes the multilayer surface coating and thus is that layer which can come in contact with the environment, for example, the skin of a human.
  • the magnification at the in Fig. 2 shown microsection is higher than in the Fig. 1 shown micrograph, which is indicated in each case by the size dimensioning illustrative bar.
  • Example 1 Various multilayer surface coatings
  • Vorgold was 99.5 wt .-% Au, the balance cobalt.
  • Example 1 The multilayer surface coatings described in Example 1 ("New Ag-PdNi Aging System") were subjected to a nickel release test according to DIN EN 1811: 2015-10 and compared with multilayer surface coatings according to the prior art (“Altes Schichtsystem Ni-PdNi”), in which the first layer was formed as a nickel layer. The results are summarized in Table 1.
  • Example 1 showed a significantly lower nickel release compared to the multilayer surface coatings of the prior art.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Laminated Bodies (AREA)
  • Catalysts (AREA)
EP19167150.2A 2018-04-03 2019-04-03 Revêtement de surface multicouche Withdrawn EP3550057A3 (fr)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP18165562 2018-04-03

Publications (2)

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EP3550057A2 true EP3550057A2 (fr) 2019-10-09
EP3550057A3 EP3550057A3 (fr) 2019-11-13

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EP19167150.2A Withdrawn EP3550057A3 (fr) 2018-04-03 2019-04-03 Revêtement de surface multicouche

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Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3505473C1 (de) * 1985-02-16 1986-06-05 Degussa Ag, 6000 Frankfurt Bad zur galvanischen Abscheidung von Gold-Indium-Legierungsueberzuegen
EP1295961B1 (fr) * 2000-06-27 2012-05-30 Citizen Holdings Co., Ltd. Article décoratif comportant un revêtement blanc
EP1978582A1 (fr) * 2007-04-05 2008-10-08 Atotech Deutschland Gmbh Procédé pour la préparation d'électrodes à utiliser dans une pile à combustible
KR100947904B1 (ko) * 2007-12-13 2010-03-17 오고균 금속 장신구 제조 방법
ES2355283T3 (es) * 2008-11-21 2011-03-24 Umicore Galvanotechnik Gmbh Secuencia de capas con contenido en metales preciosos para artículos decorativos.
AT514818B1 (de) * 2013-09-18 2015-10-15 W Garhöfer Ges M B H Ing Abscheidung von Cu, Sn, Zn-Beschichtungen auf metallischen Substraten

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
None

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