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(12) Patent Application Publication (10) Pub. No.: US 2007/0039665 A1 Johns Et Al

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(12) Patent Application Publication (10) Pub. No.: US 2007/0039665 A1 Johns Et Al US 20070039665A1 (19) United States (12) Patent Application Publication (10) Pub. No.: US 2007/0039665 A1 Johns et al. (43) Pub. Date: Feb. 22, 2007 (54) ENHANCING SILVER (52) U.S. Cl. ................................................. 148/271; 134/2 TARNISH-RESISTANCE (76) Inventors: Peter Gammon Johns, Hertfordshire (57) ABSTRACT (GB); Clare Elizabeth Harrison, Edmonton (GB) An alkanethiol, alkyl thioglycollate, dialkyl sulfide or dialkyl disulfide may be used to surface treat of an alloy of Correspondence Address: silver containing an amount of germanium that is effective Hans-Peter G Hoffmann to reduce firestain and/or tarnishing. The treatment has been Kelley Drye & Warren found to further reduce tarnishing of the alloy such that a Two Stamford Plaza sample can be supported close above a 20% solution of 281 Tresser Boulevard ammonium polysulphide for at least 30 minutes while Stamford, CT 06901-3229 (US) retaining a generally untarnished appearance. The treatment may be carried out at the end of manufacturing a shaped (21) Appl. No.: 10/551,476 article to give rise to an article that will preserve its untarnished appearance both during transit to a point of sale (22) PCT Filed: Mar. 30, 2004 but during Subsequent display for an extended period. The invention therefore also includes a method for manufactur (86). PCT No.: PCT/GBO4/O1373 ing a tarnish-resistant silver article, which comprises the steps of forming a shaped article of an alloy of silver S 371(c)(1), containing an amount of germanium that is effective to (2), (4) Date: Sep. 29, 2005 reduce firestain and/or tarnishing, Surface treating the article with an alkanethiol, alkylthioglycolate, dialkyl sulphide or (30) Foreign Application Priority Data dialkyl disulphide; and introducing the article into packag Mar. 31, 2003 (GB)......................................... O307290.7 ing. Also disclosed for use in treating an alloy of silver as aforesaid is a water-based composition comprising a treat Publication Classification ment agent selected from an alkanethiol, alkyl thioglycol late, dialkyl sulfide or dialkyl disulfide and a mixture of an (51) Int. Cl. anionic Surfactant and an amphoteric or nonionic Surfactant C23G I/00 (2006.01) in a concentration that is effective to solubilise the treatment C23C 22/58 (2007.01) agent. US 2007/0039665 A1 Feb. 22, 2007 ENHANCING SILVER TARNISH-RESISTANCE more productive of deep firestain because of the higher temperatures involved. When the depth of the firestain FIELD OF THE INVENTION exceeds about 0.025 mm (0.010 inches) the alloy is addi 0001. The present invention relates to the use of organo tionally prone to cracking and difficult to Solder because an Sulphur compounds in the enhancement of the tarnish resis oxide surface is not wetted by solder so that a proper tance of silver alloys, to silver articles of enhanced tarnish metallurgical bond is not formed. resistance that have been Surface-treated with the organo 0005 Patent GB-B-2255348 (Rateau, Albert and Johns; Sulphur compounds and to methods of keeping and display Metaleurop Recherche) disclosed a novel silver alloy that of the treated articles. It also relates to a water-based maintained the properties of hardness and lustre inherent in composition that can be used for the treatment of a metal Ag—Cu alloys while reducing problems resulting from the which may be a silver alloy but which may also be another tendency of the copper content to oxidise. The alloys were metal requiring Surface treatment to impart tarnish resistance ternary Ag—Cu—Ge alloys containing at least 92.5 wt % e.g. copper, brass or nickel. Ag, 0.5-3 wt % Ge and the balance, apart from impurities, copper. The alloys were stated to be stainless in ambient air BACKGROUND TO THE INVENTION during conventional production, transformation and finish ing operations, to be easily deformable when cold, to be Silver Alloys and Their Tarnish-Resistance easily brazed and not to give rise to significant shrinkage on 0002 Standard Sterling silver provides manufacturers casting. They were also stated to exhibit superior ductility and silversmiths with a versatile and reliable material but it and tensile strength and to be annealable to a required is inevitable that finished articles will require further clean hardness. Germanium was stated to exert a protective func ing and polishing to temporarily remove undesired tarnish tion that was responsible for the advantageous combination products. It is well-known that with exposure to everyday of properties exhibited by the new alloys, and was in solid atmospheric conditions, silver and silver alloys develop a solution in both the silver and the copper phases. The lustre-destroying dark film known as tarnish. microstructure of the alloy was said to be constituted by two phases, a solid solution of germanium and copper in silver 0003. Since ancient times it has been appreciated that Surrounded by a filamentous Solid solution of germanium unalloyed fine silver is too soft to withstand normal usage, and silver and copper. The germanium in the copper-rich and it has been the practice to add a proportion of a base phase was said to inhibit surface oxidation of that phase by metal to increase hardness and strength. In the UK, legis forming a thin GeO or GeO protective coating which lation that has existed since the fourteenth century specifies prevented the appearance of firestain during brazing and a minimum silver content of articles for sale at 92.5% (the flame annealing which results from the oxidation of copper Sterling standard), but does not specify the base metal at high temperatures. Furthermore the development of tar constituents. Experience convinced early silversmiths that nish was appreciably delayed by the addition of germanium, copper was the most suitable of the metals available to them. the surface turned slightly yellow rather than black and Modern silver-sheet manufacturers generally adhere to this tarnish products were easily removed by ordinary tap water. composition, although sometimes a proportion of copper is The alloy was said to be useful inter alia in jewellery. replaced by cadmium to attain even greater ductility. Ster However, the alloy disclosed in the above patent suffers ling with a 2.5% cadmium content is a standard material for limitations insofar as it can exhibit large grain size, leading spinning and stamping. Lower grades of silver alloys are to poor deformation properties and formation of large pools common in many parts of Europe for the production of from low-melting eutectics resulting in localised surface hollow-ware and cutlery. The 800-grade alloys (Ag parts per melting when the alloy is subject to the heat of an air torch. thousand) are predominantly used in Southern and mid 0006 Patents U.S. Pat. No. 6,168,071 and EP-B-0729398 Europe whereas in Scandinavia the 830 standard is predomi (Johns) disclose a silver/germanium alloy which comprised nant. a silver content of at least 77 wt % and a germanium content 0004. In all but the largest manufacturing companies, of between 0.4 and 7%, the remainder principally being most of the annealing and soldering required to assemble copper apart from any impurities, which alloy contains finished or semi-finished articles is carried out with the elemental boron as a grain refiner at a concentration of more flame of an air-gas blowtorch. The oxidising or reducing than 0 ppm and less than 20 ppm. The boron content of the nature of the flame and the temperature of the articles are alloy can be achieved by providing the boron in a master controlled only by the skill of the silversmith. Pure silver copper/boron alloy having 2 wt % elemental boron. It was allows oxygen to pass easily through it, particularly when reported that Such low concentrations of boron Surprisingly the silver is heated to above red heat. Silver does not oxidise provide excellent grain refining in a silver/germanium alloy, in air, but the copper in a silver/copper alloy is oxidised to imparting greater strength and ductility to the alloy com cuprous or cupric oxide. Pickling of the oxidised surface of pared with a silver/germanium alloy without boron. The the article in hot dilute sulphuric acid removes the superfi boron in the alloy. inhibits grain growth even attemperatures cial but not the deeper-seated copper oxide so that the used in the jewellery trade for soldering, and samples of the Surface consists of fine or unalloyed silver covering a layer alloy were reported to have resisted pitting even upon of silver/copper oxide mixture. The pure silver is easily heating repeatedly to temperatures where in conventional permeated during further heating, allowing copper located alloys the copper/germanium eutectic in the alloy would deeper below the surface to become oxidised. Successive melt. Strong and aesthetically pleasing joints between sepa annealing, cold working and pickling produces a surface that rate elements of the alloy can be obtained without using a exhibits the pure lustre of silver when lightly polished but filler material between the free surfaces of the two elements with heavier polishing reveals dark and disfiguring stains and a butt or lap joint can be formed by a diffusion process known as firestain or fire. Soldering operations are much or resistance or laser welding techniques. Compared to a US 2007/0039665 A1 Feb. 22, 2007 weld in Sterling silver, a weld in the above-described alloy 0014) washing the surface with a detergent solution, has a much smaller average grain size that improved the rinsing the surface with hot water and allowing it to dry. The formability and ductility of the welds, and an 830 alloy has above process is stated to provide a “long-term finish been welded by plasma welding and polished without the intended to last the intended shelf-life until the article need for grinding.
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