EP3656245B1 - Goldlegierung die mindestens 990 gewichtspromille gold enthält, uhr- oder schmuckartikel auf der basis einer goldlegierung die mindestens 990 gewichtspromille gold enthält, und legierungsherstellungsverfahren - Google Patents

Goldlegierung die mindestens 990 gewichtspromille gold enthält, uhr- oder schmuckartikel auf der basis einer goldlegierung die mindestens 990 gewichtspromille gold enthält, und legierungsherstellungsverfahren Download PDF

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EP3656245B1
EP3656245B1 EP18208376.6A EP18208376A EP3656245B1 EP 3656245 B1 EP3656245 B1 EP 3656245B1 EP 18208376 A EP18208376 A EP 18208376A EP 3656245 B1 EP3656245 B1 EP 3656245B1
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Prior art keywords
gold
weight
alloy
alloying element
equal
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French (fr)
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EP3656245A1 (de
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Damien Colas
Frédéric DIOLOGENT
Gauthier DEPIERRE
Saphir LE MAITRE
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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
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • 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
    • A—HUMAN NECESSITIES
    • A44—HABERDASHERY; JEWELLERY
    • A44C—PERSONAL ADORNMENTS, e.g. JEWELLERY; COINS
    • A44C27/00—Making jewellery or other personal adornments
    • A44C27/001—Materials for manufacturing jewellery
    • A44C27/002—Metallic materials
    • A44C27/003—Metallic alloys

Definitions

  • the present invention relates to a gold alloy.
  • the gold alloy comprises at least 990 ⁇ by weight of gold, or even at least 999 ⁇ . It has a hardness and stability compatible for use in the luxury industry, in particular for the manufacture of watchmaking or jewelery objects.
  • Jewelery gold is generally made of an alloy whose alloying elements provide the necessary hardness properties and/or make it possible to change the color. Thus, depending on its degree of purity and its alloying elements, gold can be yellow, white, pink, gray.
  • Pure gold, or quasi-pure ( ⁇ 990 ⁇ by weight of gold), has hardness properties which may prove to be unsatisfactory, the material being too ductile to produce certain objects such as fine jewelry items.
  • the alloys comprising at least 990 ⁇ by weight of gold or 24-carat gold have a Vickers hardness which is generally around 30 HV in the annealed state and around 65 HV in the annealed state. hardened state.
  • the hardness properties can be improved by means of specific treatments, in particular by hardening by solid solution, by hardening by plastic deformation (hardening) or by hardening by precipitation.
  • These treatments which can be combined, are based on the formation of obstacles to the movements of the dislocations responsible for the plastic deformation of the gold.
  • preventing or reducing the movements of the dislocations makes it possible to harden the gold.
  • Hardening by solid solution corresponds to the introduction into a metal matrix, which is generally pure, of a minority element (solute, soluble in the metal matrix).
  • Strain hardening is achieved by plastic deformation of a metal or alloy. It includes a heat treatment step. During hardening, the metal or alloy undergoes plastic deformations inducing dislocations.
  • the solute atoms can slow down the movement of the dislocations by interacting with them within the crystalline structure, that is to say the grains. This phenomenon can be amplified when the solute atoms have a strongly different size (lower or higher) than that of the atoms of the hardened metal, in this case gold.
  • the size and atomic mass of the solute atoms can have an influence on the hardness.
  • the improvement in hardness is proportional to the difference in atomic radius between the solvent and the solute.
  • the hardness can increase when the atomic mass of the solute is significantly lower than that of gold.
  • Structural hardening corresponds to the formation of precipitates in the metal or alloy. These precipitates are generally distributed homogeneously, for example at the grain boundaries or within the grains. These precipitates can result from the homogenization of the alloy or metal, for example following the formation of a more stable phase during a thermal quenching step. These precipitates can form obstacles to the movements of the dislocations and thus improve the hardness of the metal or the alloy.
  • the alloying elements can contribute to the improvement of the hardness of gold but the room for maneuver is narrow when the alloy comprises at least 990 ⁇ by weight of gold.
  • the document EP 0 882 805 describes an alloy comprising: gold, 200 to 2000 ppm of calcium, beryllium, germanium or boron and 10 to 1000 ppm of a rare earth.
  • the document JP PH093570 describes an alloy comprising: gold, 200 to 2000 ppm of calcium, beryllium or boron, 10 to 1000 ppm of a rare earth, 10 to 1000 ppm of aluminium, silicon, cobalt, nickel, tin or lead, 10 to 10,000 ppm ruthenium, iridium or rhodium.
  • the document JP 2003-328059 describes an alloy comprising gold, 0.12 to 0.28% yttrium, 0.02 to 0.18% calcium, and optionally 0.02 to 0.16% beryllium, boron, aluminum, silicon , nickel, copper, germanium, palladium, tin or antimony.
  • the document EP 0 685 565 discloses a gold alloy, having a Vickers hardness of 100 or greater, comprising between 618 and 734 ppm of calcium, beryllium, germanium and/or boron, and between 161 and 613 ppm of rare earths (including yttrium), the amount of rare earths is therefore lower than the amount of calcium, beryllium, germanium and boron.
  • alloys Although these alloys have a satisfactory hardness, it remains difficult to obtain an alloy comprising at least 990 ⁇ by weight of gold that can be used in the manufacture of timepieces or durable jewelry. This is all the more true for the luxury industry, where the quality of the articles must be irreproachable. To do this, it is preferable to have an alloy having a hardness greater than or equal to 90 HV, advantageously greater than or equal to 100 HV. This hardness is commonly considered sufficient to obtain excellent resistance of the article to scratches in particular.
  • the present invention solves this problem thanks to the development of an alloy based on gold and two alloying elements allowing the manufacture of high quality articles with great durability.
  • the present invention is defined in the appended claims.
  • the Applicant has discovered that the alloy of gold with certain specific elements makes it possible to improve its properties of hardness, enough to make it compatible for manufacturing watchmaking or jewelery objects, without requiring a specific aging treatment. .
  • the gold alloy used corresponds to Chuk Kam or 24-carat gold, the definition of which varies according to national or regional regulations.
  • the definition adopted for a 24 carat gold is that of China (24 carat gold comprising at least 990 ⁇ by weight of gold), advantageously that of Taiwan (at least 995 ⁇ by weight of gold), more advantageously that of Europe (at least 999 ⁇ by weight of gold).
  • the various quantities of the constituents of the gold alloy are expressed in percentage by weight or in tenths of a percentage by weight (per thousand, ⁇ ), relative to the weight of the gold alloy.
  • the gold alloy includes 990 ⁇ in gold weight, it means that it includes 990 grams of the gold element per 1000 grams of gold alloy.
  • the process for preparing the timepiece or jewelry item further comprises a step of shaping this gold alloy.
  • the invention also relates to the gold alloy used to prepare the watch or jewelry object.
  • This gold alloy has a hardness greater than or equal to 90 HV, advantageously greater than or equal to 100 HV and even more advantageously greater than or equal to 110 HV.
  • the watch or jewelry article according to the invention can be a piece of jewelry, a leather-based article or a clothing accessory. It can also be a watch, a writing accessory or a decorative item. For example, it could be one of the following items: ring, earring, necklace, bracelet, pendant, watch, belt or purse buckle, tie pin, cufflinks, clip ticket, a hairpin, a pen or even a paper knife.
  • the gold alloy comprises at least 990 ⁇ by weight of gold, advantageously at least 995 ⁇ by weight of gold, more advantageously at least 999 ⁇ by weight of gold.
  • the gold alloy comprises between 999 ⁇ and 999.4 ⁇ by weight of gold, and even more advantageously between 999 ⁇ and 999.3 ⁇ by weight Golden. According to a particular embodiment, it may comprise 999.2 ⁇ by weight of gold.
  • the person skilled in the art will know how to supplement with the sufficient quantity of alloying elements, first (Si, Y, Ti, Ge and their mixtures) and second alloying elements (Sn, Ge and their mixtures), to reach 1000 ⁇ .
  • the gold alloy comprises at least 995 ⁇ by weight of gold, it comprises a total amount greater than or equal to 0.6 ⁇ and less than or equal to 5 ⁇ of the first alloying element and the second alloying element. alloy.
  • the gold alloy comprises between at least 999 ⁇ by weight of gold, it comprises a total amount greater than or equal to 0.6 ⁇ and less than or equal to 1 ⁇ of the first alloying element and the second alloying element. 'alloy.
  • the watchmaking or jewelery article according to the invention advantageously comprises a gold alloy comprising between 5.10 and 8.00 ⁇ by weight of the first alloying element, more advantageously between 2.55 and 4.00 ⁇ , even more advantageously between 0.51 ⁇ and 0.90 ⁇ , preferably between 0.51 ⁇ and 0.80 ⁇ .
  • the watchmaking or jewelery article according to the invention advantageously comprises a gold alloy comprising between 2.00 and 4.90 ⁇ by weight of the second alloying element, more advantageously between 1.00 and 2.45 ⁇ , even more advantageously between 0.10 ⁇ and 0.49 ⁇ , preferably between 0.20 ⁇ and 0.49 ⁇ .
  • the total quantity of alloying elements (first + second) is less than or equal to 10 ⁇ , advantageously less than or equal to 5 ⁇ , more advantageously less than or equal to 1 ⁇ , by weight relative to the weight of the gold alloy . It is greater than or equal to 0.6 ⁇ , advantageously greater than or equal to 0.7 ⁇ .
  • the gold alloy has a ratio by weight of the first alloying element to the second alloying element strictly greater than 1, preferably greater than 1.5 and less than 9, more preferably a weight ratio equal to 2.
  • the quantity by weight of the first alloying element is always greater than the quantity by weight of the second alloying element.
  • the first alloying element is chosen from silicon, yttrium, titanium, germanium and mixtures thereof.
  • the second alloying element is tin or germanium or a mixture of tin and germanium.
  • the first alloying element is germanium
  • the second alloying element is tin
  • germanium is the second alloying element and is present in a lower amount by weight than the other alloying element.
  • germanium is associated with silicon, yttrium or titanium, the proportion by weight of germanium is the smallest.
  • the first element is silicon, yttrium, or germanium.
  • titanium can cause processing problems due to its affinity with oxygen.
  • the first alloying element is silicon.
  • the gold alloy comprising silicon as the first alloying element has a Vickers hardness which is advantageously greater than 100 HV.
  • the gold alloy is an alloy of gold, silicon and germanium (AuSiGe).
  • the Si/Ge weight ratio is advantageously equal to 2.
  • the gold alloy is an alloy of gold, silicon and tin (AuSiSn).
  • the Si/Sn weight ratio is advantageously equal to 2.
  • This alloy advantageously comprises at least 995 ⁇ by weight of gold and a total quantity greater than or equal to 0.6 ⁇ and less than or equal to 5 ⁇ of the first alloying element and of the second alloying element. More advantageously, it comprises at least 999 ⁇ by weight of gold and a total quantity greater than or equal to 0.6 ⁇ and less than or equal to 1 ⁇ of the first alloying element and of the second alloying element. Preferably, this alloy comprises between 999 ⁇ and 999.4 ⁇ by weight of gold, more preferably between 999 ⁇ and 999.3 ⁇ by weight of gold. The respective amounts and combinations of the alloying elements are as indicated above.
  • 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.
  • the alloying is advantageously carried out by an induction furnace, for example.
  • step a) is carried out at a temperature between 850°C and 1500°C, advantageously between 900°C and 1450°C.
  • step b) corresponds to a homogenization treatment which involves bringing the alloy back into solution.
  • step b) and the work hardening of step c) make it possible to increase the hardness of the alloy.
  • Optional step b) is advantageously carried out at a temperature between 600 and 800°C, more advantageously between 700 and 800°C.
  • step b) The duration of step b) is between 45 and 120 minutes, more advantageously between 45 and 60 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. It also makes it possible to reduce or eliminate any internal stresses that may result from heterogeneous solidification. Finally, it makes it possible to freeze the microstructure and to keep a supersaturated solution, which can prove to be useful when step d) of aging is implemented.
  • Stage b) can be followed by a cooling stage allowing the structure of the alloy to be fixed, prior to stage 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.
  • Thermal quenching advantageously with water, makes it possible to supersaturate the alloy with alloying elements, in particular when one or more alloying elements are little or not soluble at ambient temperature.
  • step c) corresponds to hardening by deformation, for example by rolling. 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 65 and 90%.
  • the embodiments in which the first alloying element is silicon are particularly advantageous because it is possible to obtain a Vickers hardness greater than 100 HV with a work hardening of 75% and greater than 110 HV with a work hardening of 90%. In the other embodiments, a work hardening of 90% is preferred.
  • step c) The alloy obtained following step c) can optionally be subjected to an aging step, in particular by heating.
  • the method is advantageously free of step d) of ageing.
  • the optional step d) of aging 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.
  • the aging step d) is optional. It can be carried out at a temperature between 150°C and 300°C. Its duration is advantageously between 0.5 and 3 hours.
  • the aging can be carried out in air or, when the composition of the gold alloy is sensitive to oxidation, in an inert atmosphere, for example under argon.
  • the alloy obtained at the end of hardening, or aging can then be shaped according to conventional techniques to form the watchmaking or jewelery article 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.
  • Shaping by rolling in step c) corresponds to work hardening. It was made using a bench rolling mill. A lamella with a thickness of less than 7 mm is passed several times between the two rolls of the rolling mill, the spacing of which is controlled by a handwheel. Two theoretical strain levels were applied at 75% and 90%. To ensure better reproducibility during this step, all the samples are deformed at a height of 0.35 mm per pass with a constant rolling speed of the rollers of 3.95 m/minute.
  • Examples 2 to 14 relate to various compositions of gold alloys comprising at least one alloying element from among calcium, yttrium, titanium, germanium, tin and silicon.
  • the figure 1 illustrates the as-cast hardnesses, after strain hardening, possibly after ageing, of these compositions and of pure gold (CE-1).
  • the figure 1 shows that the effect of hardening by solid solution (as cast) remains insufficient for these gold alloy compositions. However, the malleability of these compositions allows deformation rates of 90% without cracking.
  • the AuPd (CE-2) and AuZr (CE-3) compositions are not satisfactory insofar as the gain in hardness is less than 100 HV (80-85 HV) and remains too limited compared to pure gold ( CE-1, 65HV).
  • the AuCa (CE-14) composition could be suitable to have a sufficiently hard gold alloy.
  • this composition requires an aging step.
  • it is difficult to implement because calcium is not very soluble in gold (1.8 atomic % at 800° C.) and oxidizes easily during heat treatments, which creates an embrittling phase. This is also the case for AuCaSi (CE-11).
  • compositions (AuTiGe (INV-7), AuGeSn (INV-9), AuYGe (INV-10) and AuSiGe (INV-12) have a hardness greater than 100 HV after work hardening at 90% .
  • the composition Au 999 Ge 0.665 Si 0.335 could not be implemented due to complete cracking of the sample after work hardening of a few percent.
  • the Au 999 Ge 1 composition (not shown) has a relatively low as-cast hardness comparable to that of fine gold (30 HV). After 75% hardening, it is only 50 HV, which is insufficient.
  • Silicon makes it possible to increase the hardness after work hardening when it is present as the main alloying element (INV-12 and INV-13).

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

  1. Goldlegierung bestehend aus:
    - mindestens 990 Gewichts-‰ Gold,
    - eine Menge von größer oder gleich 0.6 ‰ und kleiner oder gleich 10 ‰ zweier Legierungselemente:
    ∗ ein erstes Legierungselement ausgewählt aus Silizium, Yttrium, Titan und Germanium, und ihren Mischungen, und
    ∗ ein zweites Legierungselement ausgewählt aus Zinn, Germanium und ihren Mischungen,
    - eventuelle Unreinheiten betragen dabei weniger als 50 ppm des Gewichtes der Legierung,
    das erste Legierungselement und das zweite Legierungselement unterscheiden sich dabei voneinander und die Menge des ersten Legierungselementes ist höher, als die Menge des zweiten Legierungselementes,
    Goldlegierung mit einer Härte von mindestens 90 Hv.
  2. Legierung nach Anspruch 1, dadurch gekennzeichnet, dass sie mindestens 990 Gewichts-‰ Gold enthält und eine Gesamtmenge des ersten Legierungselements und des zweiten Legierungselementes von kleiner oder gleich 1 ‰.
  3. Uhr- oder Schmuckartikel mit einer Goldlegierung nach Anspruch 1.
  4. Uhr- oder Schmuckartikel nach Anspruch 3, dadurch gekennzeichnet, dass die Goldlegierung mindestens 995 Gewichts-‰ Gold enthält und eine Gesamtmenge von größer oder gleich 0.6 Gewichts-‰ und kleiner oder gleich 5 Gewichts-‰ des ersten Legierungselementes und des zweiten Legierungselementes.
  5. Uhr- oder Schmuckartikel nach Anspruch 3 oder 4, dadurch gekennzeichnet, dass die Goldlegierung zwischen mindestens 999 Gewichts-‰ Gold und eine Gesamtmenge von größer oder gleich 0.6 Gewichts-‰ und kleiner oder gleich 1 Gewichts-‰ des ersten Legierungselementes und des zweiten Legierungselementes enthält.
  6. Uhr- oder Schmuckartikel nach einem der Ansprüche 3 bis 5, dadurch gekennzeichnet, dass die Goldlegierung zwischen 0.51 und 0.90 Gewichts-‰ der Legierung enthält, vorzugsweise zwischen 0.51 und 0.80 Gewichts-‰.
  7. Uhr- oder Schmuckartikel nach Anspruch nach einem der Ansprüche 3 bis 6, dadurch gekennzeichnet, dass die Goldlegierung zwischen 0.10 und 0.49 Gewichts-‰ des zweiten Legierungselementes, vorzugsweise zwischen 0.20 und 0.49 Gewichts-‰, enthält
  8. Uhr- oder Schmuckartikel nach einem der Ansprüche 3 bis 7, dadurch gekennzeichnet, dass die Goldlegierung ein Gewichtsverhältnis des ersten Legierungselement zum zweiten Legierungselement von strikt über 1.5 und unter 9 aufweist, vorzugsweise gleich 2.
  9. Uhr- oder Schmuckartikel nach einem der Ansprüche 3 bis 8, dadurch gekennzeichnet, dass das erste Legierungselement Silizium ist.
  10. Uhr- oder Schmuckartikel nach einem der Ansprüche 3 bis 9, dadurch gekennzeichnet, dass es sich bei der Goldlegierung um eine Legierung aus Gold, Silizium und Germanium handelt.
  11. Uhr- oder Schmuckartikel nach einem der Ansprüche 3 bis 9, dadurch gekennzeichnet, dass es sich bei der Goldlegierung um eine Legierung aus Gold, Silizium und Zinn handelt.
  12. Verfahren zur Herstellung einer Goldlegierung, das mindestens die folgenden Schritten umfasst:
    a) Bildung einer Legierung aus einer Mischung, die nach Gewicht, bezogen auf das Gesamtgewicht der Metalle besteht aus:
    - mindestens 990 ‰ Gold,
    - eine Menge Q1 aus einem ersten Legierungselement, ausgewählt aus Silizium, Yttrium, Titan und Germanium, und ihren Mischungen,
    - eine Menge Q2 eines zweiten Legierungselementes, ausgewählt aus Zinn, Germanium, und ihren Mischungen,
    mit 0.6 ≤ Q1 + Q2 ≤ 10 ‰ und Q1 > Q2,
    - eventuelle Unreinheiten betragen dabei weniger als 50 ppm des Gewichtes der Mischung,
    b) optional Wärmebehandlung der im Schritt a) erzeugten Legierung,
    c) Formung durch Kaltverfestigung der im Schritt a) oder b) erzeugten Legierung,
    d) optional Alterung durch Wärmebehandlung der Legierung aus Schritt c).
  13. Verfahren nach Anspruch 12, dadurch gekennzeichnet, dass Schritt b) bei einer Temperatur zwischen 850°C und 1500°C durchgeführt wird, vorteilhafterweise zwischen 900°C und 1450°C.
  14. Verfahren gemäß einem der Ansprüche 12 bis 13, dadurch gekennzeichnet, dass Schritt b) bei einer Temperatur zwischen 700°C und 800°C für eine Dauer zwischen 45 und 120 Minuten durchgeführt wird.
  15. Verfahren nach einem der Ansprüche 12 bis 14, dadurch gekennzeichnet, dass die Kaltverfestigung aus Schritt c) zwischen 75 % und 90 % durchgeführt wird.
EP18208376.6A 2018-11-26 2018-11-26 Goldlegierung die mindestens 990 gewichtspromille gold enthält, uhr- oder schmuckartikel auf der basis einer goldlegierung die mindestens 990 gewichtspromille gold enthält, und legierungsherstellungsverfahren Active EP3656245B1 (de)

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EP18208376.6A EP3656245B1 (de) 2018-11-26 2018-11-26 Goldlegierung die mindestens 990 gewichtspromille gold enthält, uhr- oder schmuckartikel auf der basis einer goldlegierung die mindestens 990 gewichtspromille gold enthält, und legierungsherstellungsverfahren

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CN114351002B (zh) * 2022-01-11 2023-11-14 云南先导新材料有限公司 一种高硬高纯黄金首饰材料及其制备方法

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JPS6030158A (ja) * 1983-07-29 1985-02-15 Sumitomo Metal Mining Co Ltd ボンデイングワイヤ−
JPS63145729A (ja) * 1986-03-28 1988-06-17 Nittetsu Micro Metal:Kk 半導体素子ボンデイング用金線
JP2780611B2 (ja) * 1993-09-06 1998-07-30 三菱マテリアル株式会社 少量成分の合金化で硬質化した金装飾品材
JPH093570A (ja) * 1995-06-23 1997-01-07 Mitsubishi Materials Corp Ａｕ含有量の高い硬質金合金製装飾部材
JP2003328059A (ja) * 2002-05-10 2003-11-19 Matsuda Sangyo Co Ltd 硬化型金合金

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