EP3808865B1 - Weissgoldlegierung und ihr herstellungsverfahren - Google Patents

Weissgoldlegierung und ihr herstellungsverfahren Download PDF

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Publication number
EP3808865B1
EP3808865B1 EP19203757.0A EP19203757A EP3808865B1 EP 3808865 B1 EP3808865 B1 EP 3808865B1 EP 19203757 A EP19203757 A EP 19203757A EP 3808865 B1 EP3808865 B1 EP 3808865B1
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Prior art keywords
gold
gold alloy
alloy
vanadium
iron
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EP19203757.0A
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English (en)
French (fr)
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EP3808865A1 (de
Inventor
Fanny LALIRE
Gauthier DEPIERRE
Mélanie CARBAJAL BELLO
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Richemont International SA
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Richemont International SA
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C5/00—Alloys based on noble metals
    • C22C5/02—Alloys based on gold
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/14—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of noble metals or alloys based thereon

Definitions

  • the present invention relates to a white gold alloy comprising at least 750 ⁇ by weight of gold.
  • This alloy has the advantage of being scratch resistant while offering a neutral and stable color as well as an exceptional shine.
  • the fields of use of the present invention relate in particular to jewelry, watches, leather goods, writing instruments, etc.
  • gold has been mixed with other elements in order to modify its properties.
  • the properties of the gold for example its hardness and/or its color.
  • nickel is an allergenic metal and the preparation of gold alloys comprising nickel can be complicated.
  • the main disadvantages relating to the use of palladium include its price and its low contribution to the improvement of the mechanical properties of gold alloys. Moreover, the refining of alloys containing palladium is not easy. Adding palladium also drops the brilliance of the alloy.
  • Examples of prior art white gold alloys include Au 750 Pd 125 Ag 30 Cu 95 , Au 750 Pd 130 Cu 100 In 15 Ga 5 , Au 750 Pd 150 Fe 60 Cu 40 and Au 750 Pd 210 In 35 Ga 5 .
  • WO 2010/127458 describes a gray gold alloy comprising in particular, by weight, at least 750 ⁇ of gold, plus 180 ⁇ and less than 240 ⁇ of palladium.
  • EP 3 070 182 describes an iron-free, nickel-free, cobalt-free, iron-free, silver-free, copper-free, zirconium-free, niobium-free, chromium-free and manganese-free gray gold alloy comprising, by weight, 750 to 765 ⁇ of gold , 150 to 230 ⁇ of palladium and 5 to 50 ⁇ of rhodium.
  • EP 2 546 371 describes a gray gold alloy comprising at least 750 ⁇ of gold, 130 to 230 ⁇ of chromium and 20 to 120 ⁇ of at least one element chosen from among palladium, iron, ruthenium, platinum, cobalt, gallium, germanium, manganese and nickel.
  • rhodium plating In order to improve the whiteness, shine, resistance to scratches or corrosion, it is also possible to treat gold alloys by rhodium plating, i.e. subjecting them to a rhodium plating treatment. .
  • rhodium plating involves a specific binding process, generally of the galvanic type.
  • the present invention makes it possible to remedy the problems of the prior art thanks to a white gold alloy which can be devoid of nickel and does not require rhodium plating.
  • the present invention relates to a gold-based alloy as defined in claim 1. This alloy is white in color.
  • the amounts of the elements of the alloy are expressed by weight relative to the weight of the alloy. For example, 1000 grams of an alloy comprising 750 ⁇ of gold contains 750 grams of gold.
  • the gold and the first and second alloying elements advantageously represent 1000 ⁇ by weight of the gold alloy.
  • the vanadium advantageously represents 120 ⁇ to 180 ⁇ .
  • the vanadium advantageously represents 10% to 50 ⁇ .
  • Silver, vanadium, niobium, palladium and chromium are elements with well-defined solubility ranges in gold. Thus, in these proportions, they are non-weakening elements of the gold alloy. Alone, or in a mixture, they can lead to a homogeneous gold alloy.
  • Vanadium, iron, titanium, niobium and chromium are elements with a whitening effect. Alone, or in a mixture, they therefore improve the whiteness of the gold alloy.
  • Iron also improves the solubility and rollability of the alloy. In small quantities, 30% to 70% according to the invention, it does not impact the corrosion resistance.
  • the gold alloy comprises between 750%o ( ⁇ 750 ⁇ ) and 825%o ( ⁇ 825 ⁇ ) of gold, more advantageously 750 to 780 ⁇ of gold.
  • the alloy according to the invention comprises 2% 0 (by weight relative to the weight of the alloy) or less of at least one grain refiner element. In other words, it comprises between 0 ⁇ and 2 ⁇ of at least one grain refiner element, more advantageously 1 ⁇ or less.
  • the grain refiner can advantageously represent at least 0.01% by weight relative to the weight of the alloy (ie ⁇ 10 ppm). It is an element selected from the group comprising ruthenium, rhenium, iron, iridium, cobalt, vanadium, molybdenum and mixtures thereof. Elements such as ruthenium, rhenium or iron guarantee the fineness of the grain, without significantly modifying the hardness or affecting the color.
  • the alloy includes 30 ⁇ to 70 ⁇ of iron as the second alloying element, the refining element is not iron. Indeed, the refining element is distinct from gold, from the first alloying element and from the second alloying element.
  • the gold alloy according to the invention may also contain any minute quantities that can be assimilated to impurities ( ⁇ 10 ppm or ⁇ 0.01 ⁇ ). These impurities can in particular be carbon, oxygen or nitrogen for example.
  • the gold alloy according to the invention is advantageously devoid of rhodium and/or copper.
  • the alloy is devoid of platinum and/or gallium and/or indium.
  • a gold alloy devoid of an element means that it contains less than 0.01 ⁇ ( ⁇ 10 ppm) of this element, advantageously less than 0.001 ⁇ ( ⁇ 1 ppm), more advantageously 0 ⁇ .
  • the gold alloy according to the invention has a hardness advantageously between 120 and 300 Hv, more advantageously between 160 and 240 Hv. This is the hardness of the alloy in the annealed state, that is to say after step d) described below.
  • an alloy having a hardness of at least 120 HV has sufficient scratch resistance properties to be used in watches or jewelry.
  • the gold alloy advantageously consists of at least 750 ⁇ of gold, 80 ⁇ to 120 ⁇ of silver, 80 ⁇ to 120 ⁇ of chromium and 30 ⁇ to 70 ⁇ iron.
  • the gold alloy is advantageously of the formula Au 750 Ag 100 Cr 100 Fe 50 , the respective amounts of the elements being expressed by weight.
  • the gold alloy advantageously consists of at least 750 ⁇ of gold, from 150 ⁇ to 220 ⁇ of niobium, and from 30 ⁇ to 70 ⁇ of chromium.
  • the gold alloy is advantageously of the formula Au 750 Nb 200 Cr 50 , the respective amounts of the elements being expressed by weight.
  • the gold alloy advantageously consists of at least 750 ⁇ of gold, 120 ⁇ to 180 ⁇ of vanadium, 30 ⁇ to 70 ⁇ of iron and 20 ⁇ to 60 ⁇ of palladium.
  • the gold alloy is advantageously of the formula Au 750 V 160 Fe 50 Pd 40 or Au 750 V 140 Pd 60 Fe 50 , the respective amounts of the elements being expressed by weight.
  • the gold alloy comprises palladium and vanadium
  • it has a Pd/V weight ratio advantageously between 0.20 and 0.50. This ratio, in this type of alloy comprising palladium and vanadium, makes it possible to optimize the corrosion resistance properties.
  • the gold alloy advantageously consists of at least 750 ⁇ of gold, 80 ⁇ to 120 ⁇ of palladium, 80 ⁇ to 120 ⁇ of chromium, 10 ⁇ to 50 ⁇ vanadium and 5 ⁇ to 40 ⁇ titanium.
  • the gold alloy is advantageously of the formula Au 750 Pd 100 Cr 100 V 30 Ti 20 , the respective amounts of the elements being expressed by weight.
  • the gold alloy advantageously consists of at least 750 ⁇ of gold, 130 ⁇ to 170 ⁇ of vanadium, 30 ⁇ to 70 ⁇ of iron and 30 ⁇ to 70 ⁇ iron.
  • the gold alloy is advantageously of the formula Au 750 V 150 Fe 50 Nb 50 , the respective amounts of the elements being expressed by weight.
  • the gold alloy according to the invention is white. This color is due to the presence of the first and second alloying elements and their specific amounts.
  • a material whose a ⁇ and b ⁇ components are close to 0 and whose L ⁇ component is close to 100 is a white and shiny material.
  • the CIE L ⁇ a ⁇ b ⁇ coordinates can in particular be obtained by means of a conventional spectrophotometer, by measuring the reflectance properties as a function of the illumination wavelength.
  • the gold alloy according to the invention has an L ⁇ value advantageously between 80 and 95.
  • the gold alloy according to the invention has a C ⁇ value advantageously between 0 and 6, more advantageously between 2 and 4.
  • this alloy Due to its properties such as color, shine and hardness, this alloy can be used in many fields and, more particularly, in the luxury industry.
  • the present invention also relates to an article comprising this gold alloy or consisting of it. It may in particular be a watchmaking article, a jewelry article, a leather goods article or a writing article.
  • This article is advantageously devoid of metal plating. Thus, advantageously, it does not include rhodium plating.
  • watchmaking article we refer in particular to watch cases, dials, metal watch straps, clasps, mechanical parts of a watch movement, etc.
  • jewelry article also denotes jewelry articles and ornaments, for example fashion accessories (cufflinks, money clips, hair clips, etc.).
  • leather goods refers in particular to metal elements such as belt buckles, handbag clasps, etc.
  • step a the respective proportions of the metals correspond to the proportions of the final alloy. This step is carried out conventionally, according to the techniques known to those skilled in the art.
  • Step a) consists in mixing and melting the various metals so as to form a homogeneous mixture. This step is advantageously carried out by heating the mixture until the desired temperature is reached (>T liquidus ).
  • the alloying is advantageously carried out by an induction furnace, for example.
  • step a) is carried out at a temperature between 800°C and 2000°C, advantageously between 1200°C and 1700°C.
  • Optional step b) is advantageously carried out at a temperature between 800 and 1200°C, more advantageously between 1000 and 1100°C.
  • step b) is advantageously between 10 and 120 minutes, more advantageously between 30 and 90 minutes.
  • step b) can make it possible to standardize the composition of alloying elements and to ensure homogeneity of the mechanical properties of the alloy thanks to solution treatment and the dissemination of alloying elements in gold.
  • step c) and the annealing heat treatment according to step d) make it possible to increase the hardness of the alloy.
  • step c) can be repeated several times, advantageously between 2 and 10 times.
  • step d) of annealing is advantageously followed by step d) of annealing.
  • the annealing or the different annealings of stage d), following the work hardening of stage c), makes it possible(try) to reinitialize the microstructure of the alloy and thus to optimize the work hardening by avoiding the formation of cracks.
  • the annealing step d) makes it possible to recrystallize the alloy and to reduce or eliminate any internal stresses following a hardening step for example.
  • the annealing step d) can be followed by a cooling step making it possible to freeze the structure of the alloy.
  • This cooling can also be carried out prior to a new hardening according to step c). It advantageously consists in carrying out thermal quenching in air or in water. Even though air quenching is much slower than water quenching, the alloys obtained according to these two routes have similar hardness properties.
  • step d) the various heat treatments (annealed) of step d) are followed by quenching, advantageously with water, in order to avoid hardening during the slow cooling which would prevent further hardening.
  • the process according to the invention can also comprise such a quenching step before and/or after the strain hardening of step c), for example after step a) and/or after step b) and/or after step d).
  • step c) corresponds to hardening by deformation, for example by rolling or by drawing. It is advantageously carried out between 50 and 99% reduction in thickness, more advantageously between 60 and 95%. In other words, the alloy undergoes a deformation advantageously comprised between 50 and 99%, more advantageously between 65 and 95%.
  • Work hardening is advantageously carried out at ambient temperature, more advantageously between 15°C and 25°C.
  • the process comprises a step d) of annealing following work hardening. This annealing makes it possible in particular to bring out the grains of the alloy by relaxing any internal stresses within the alloy.
  • Step d) is advantageously carried out at a temperature between 800 and 1200°C, more advantageously between 900 and 1100°C.
  • step d) is advantageously between 30 and 120 minutes, more advantageously between 45 and 90 minutes.
  • the alloy obtained following step d) can optionally be subjected to an aging or structural hardening step, in particular by heating.
  • Optional step e) corresponds to structural hardening by precipitation.
  • the structural hardening is manifested by the formation of precipitates of various origins within the alloy, either at the grain boundaries or within the grains.
  • Step e) is optional. It can be carried out at a temperature between 500°C and 900°C, more advantageously between 700 and 800°C. Its duration is advantageously between 15 minutes and 120 minutes.
  • step e) is advantageously between 15 minutes and 90 minutes, more advantageously between 15 minutes and 30 minutes.
  • Step e) can be carried out under vacuum or under an inert atmosphere, for example under argon or under nitrogen.
  • Step e) is mainly used when the alloy is intended for the field of jewelry.
  • the method advantageously and successively comprises steps a), c), d) and e).
  • the method successively comprises steps a), c), d) and e), the method comprising repeating the sequence of steps c) and d), advantageously 2 to 10 times.
  • the alloy obtained at the end of step d) or of step e), can be in the form of a semi-finished product, for example a bar, a tube or a plate. It can then be shaped using conventional techniques to form an article of timepieces, jewelry, leather goods or writing according to the invention.
  • the shaping is carried out by cold or hot deformation, then by stamping, cutting, machining, for example by means of a cutting tool or by electroerosion or by means of a laser.
  • the shaping can be carried out by additive manufacturing.
  • the alloy is first transformed into powder form.
  • the present invention also relates to a process for manufacturing a timepiece or jewelery item from the gold alloy described herein according to conventional processes.
  • steps c) and d) are repeated 2 to 10 times.
  • Tables 1 and 2 list the CIE L ⁇ a ⁇ b ⁇ coordinates and hardness of these gold alloys.
  • Table 1 CIE L ⁇ sup> ⁇ /sup>a ⁇ sup> ⁇ /sup>b ⁇ sup> ⁇ /sup> coordinates of the gold alloys according to the invention
  • Table 2 specifies the hardness of these alloys after heat treatment (step d)), after work hardening (step c)) or after work hardening and hardening (steps e) and d)).

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
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Claims (15)

  1. Goldlegierung bestehend, nach Gewicht, aus:
    - mindestens 750 ‰ Gold,
    - mindestens einem ersten Legierungselement, ausgewählt aus der Gruppe, bestehend aus 30 bis 220 ‰ Niobium, 80 bis 120 ‰ Silber und 10 bis 180 ‰ Vanadium,
    - mindestens einem zweiten Legierungselement, ausgewählt aus der Gruppe, bestehend aus 30 bis 70 ‰ Eisen, 20 bis 120 ‰ Palladium, 30 bis 120 ‰ Chrom und 5 bis 40 ‰ Titan,
    - 0 bis 2 ‰ aus mindestens einem Kornfeinungselement, ausgewählt aus der Gruppe mit Ruthenium, Rhenium, Eisen, Iridium, Kobalt, Vanadium, Molybdän und ihren Mischungen,
    - das Komfeinungselement unterscheidet sich dabei von Gold, dem ersten Legierungselement und dem zweiten Legierungselement.
    - die Gesamtmenge der ersten und zweiten Goldlegierungselemente beträgt zwischen 150 ‰ und 250 %o.
  2. Goldlegierung nach Anspruch 1, dadurch gekennzeichnet, dass die Goldlegierung besteht aus:
    - mindestens 750 ‰ Gold,
    - 80 ‰ bis 120 ‰ Silber,
    - 80 ‰ bis 120 ‰ Chrom,
    - 30 ‰ bis 70 ‰ Eisen,
    - mindestens 0 bis 2 ‰ eines Kornfeinungselementes, das nicht Eisen ist.
  3. Goldlegierung nach Anspruch 1, dadurch gekennzeichnet, dass die Goldlegierung besteht aus:
    - mindestens 750 ‰ Gold,
    - 150 ‰ bis 220 ‰ Niobium,
    - 30 ‰ bis 70 ‰ Chrom,
    - 0 bis 2 ‰ mindestens eines Kornfeinungselements.
  4. Goldlegierung nach einem der Ansprüche 1, dadurch gekennzeichnet, dass die Goldlegierung besteht aus:
    - mindestens 750 ‰ Gold,
    - 120 ‰ bis 180 ‰ Vanadium,
    - 30 ‰ bis 70 ‰ Eisen,
    - 20 ‰ bis 60 ‰ Palladium,
    - 0 bis 2 ‰ mindestens eines Kornfeinungselementes, das weder Eisen noch Vanadium ist.
  5. Goldlegierung nach einem der Ansprüche 1, dadurch gekennzeichnet, dass die Goldlegierung besteht aus:
    - mindestens 750 ‰ Gold,
    - 80 ‰ bis 120 ‰ Palladium,
    - 80 ‰ bis 120 ‰ Chrom,
    - 10 ‰ bis 50 ‰ Vanadium,
    - 5 ‰ bis 40 ‰ Titan,
    - 0 bis 2 ‰ mindestens eines Kornfeinungselementes, das nicht Vanadium ist.
  6. Goldlegierung nach einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, dass die Goldlegierung zwischen 750 ‰ und 825 ‰ Gold enthält.
  7. Goldlegierung nach Anspruch 1, dadurch gekennzeichnet, dass die Goldlegierung die Formel Au750Ag100Cr100Fe50 hat.
  8. Goldlegierung nach Anspruch 1, dadurch gekennzeichnet, dass die Goldlegierung die Formel Au750Nb200Cr50 hat.
  9. Goldlegierung nach Anspruch 1, dadurch gekennzeichnet, dass die Goldlegierung die Formel Au750V160Fe50Pd40 oder Au750V140Pd60Fe50 hat.
  10. Goldlegierung nach Anspruch 1, dadurch gekennzeichnet, dass die Goldlegierung die Formel Au750Pd100Cr1ooV30T120 hat.
  11. Goldlegierung nach Anspruch 1, dadurch gekennzeichnet, dass die Goldlegierung die Formel Au750V150Fe50Nb50 hat.
  12. Goldlegierung nach einem der Ansprüche 1 bis 11, dadurch gekennzeichnet, dass die Goldlegierung eine Härte zwischen 120 Hv und 300 Hv hat, vorteilhafterweise zwischen 160 Hv und 240 Hv.
  13. Uhr-, Schmuck-, Lederwaren- oder Schreibwarenartikel mit der Goldlegierung nach einem der Ansprüche 1 bis 12.
  14. Uhr-, Schmuck-, Lederwaren- oder Schreibwarenartikel mit der Goldlegierung nach einem der Ansprüche 1 bis 12, wobei der Artikel keine Metallbeschichtung hat.
  15. Herstellungsverfahren der Goldlegierung nach einem der Ansprüche 1 bis 12, das mindestens aus den nachstehenden aufeinanderfolgenden Schritten besteht:
    a) Legierung einer Mischung bestehend aus, nach Gewicht, bezogen auf das Gesamtgewicht der Metalle:
    - mindestens 750 %o Gold,
    - mindestens einem ersten Legierungselement, ausgewählt aus der Gruppe bestehend aus 30 bis 220 ‰ Niobium, 80 bis 120 ‰ Silber und 10 bis 180 ‰ Vanadium,
    - mindestens einem zweiten Legierungselement, ausgewählt aus der Gruppe bestehend aus 30 bis 70 ‰ Eisen, 20 bis 120 ‰ Palladium, 30 bis 120 ‰ Chrom und 5 bis 40 ‰ Titan,
    - 0 bis 2 ‰ mindestens eines Kornfeinungselementes, ausgewählt aus der Gruppe, bestehend aus Ruthenium, Rhenium, Eisen, Iridium, Kobalt, Vanadium, Molybdän und ihren Mischungen,
    das Kornfeinungselement ist weder Gold, nach das erste Legierungselement noch das zweite Legierungselement,
    die Gesamtmenge der ersten und zweiten Elemente liegt zwischen 150 ‰ und 250 ‰,
    b) optional Wärmebehandlung der im Schritt a) erzeugten Legierung,
    c) optional, Kaltverfestigung der im Schritt a) oder b) erzeugten Legierung,
    d) Tempern der Legierung aus Schritt c),
    e) optional Alterung durch Wärmebehandlung der Legierung aus Schritt c).
EP19203757.0A 2019-10-17 2019-10-17 Weissgoldlegierung und ihr herstellungsverfahren Active EP3808865B1 (de)

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EP3808865A1 EP3808865A1 (de) 2021-04-21
EP3808865B1 true EP3808865B1 (de) 2023-01-18

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Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2251444A1 (de) 2009-05-06 2010-11-17 Rolex Sa Graugoldlegierung ohne Nickel und Kupfer
PT2546371T (pt) 2011-07-12 2017-02-14 Cendres + Métaux Sa Ouro branco de 18 quilates
EP3070182B1 (de) 2015-03-17 2017-08-30 The Swatch Group Research and Development Ltd. Weissgoldlegierung
US9738951B1 (en) * 2016-03-31 2017-08-22 Leachgarner, Inc. 18K palladium and platinum containing age hardenable white gold alloy

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