EP3656245A1 - Uhr- oder schmuckartikel auf der basis einer goldlegierung, die mindestens 990 gewichtspromille gold enthält - Google Patents

Uhr- oder schmuckartikel auf der basis einer goldlegierung, die mindestens 990 gewichtspromille gold enthält Download PDF

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Publication number
EP3656245A1
EP3656245A1 EP18208376.6A EP18208376A EP3656245A1 EP 3656245 A1 EP3656245 A1 EP 3656245A1 EP 18208376 A EP18208376 A EP 18208376A EP 3656245 A1 EP3656245 A1 EP 3656245A1
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EP
European Patent Office
Prior art keywords
gold
alloy
weight
alloying element
germanium
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.)
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Application number
EP18208376.6A
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English (en)
French (fr)
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EP3656245B1 (de
Inventor
Damien Colas
Frédéric DIOLOGENT
Gauthier DEPIERRE
Saphir LE MAITRE
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.)
Richemont International SA
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Richemont International SA
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Publication of EP3656245A1 publication Critical patent/EP3656245A1/de
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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 an object comprising a gold alloy.
  • the gold alloy used comprises at least 990% o by weight of gold, or even at least 999 ⁇ . It has a hardness and stability compatible for use in the luxury industry, especially for the manufacture of timepieces or jewelry.
  • Jewelry gold generally consists of an alloy, the alloying elements of which provide properties of necessary hardness and / or allow the color to be changed. Thus, depending on its degree of purity and its alloying elements, gold can be yellow, white, pink, gray.
  • Pure gold, or almost pure gold has hardness properties which can prove to be unsatisfactory, the material being too ductile to make certain objects such as fine jewelry.
  • alloys comprising at least 990 90 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 at l '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 (work 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 gold.
  • preventing or reducing the movements of dislocations makes it possible to harden the gold.
  • Hardening by solid solution corresponds to the introduction into a metallic matrix, which is generally pure, of a minority element (solute, soluble in the metallic matrix).
  • Hardening by work hardening is carried out by plastic deformation of a metal or an alloy. It includes a heat treatment step During the work hardening, the metal, or the alloy, undergoes plastic deformations inducing dislocations.
  • the solute atoms can slow down the movement of dislocations by interacting with them within the crystal structure, that is, grains. This phenomenon can be amplified when the solute atoms have a strongly different size (smaller or larger) 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 hardness.
  • the improvement in hardness is proportional to the difference in atomic radius between the solvent and the solute.
  • 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 the 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 movement of dislocations and thus improve the hardness of the metal or alloy.
  • the alloying elements can contribute to improving the hardness of gold but the margin of maneuver is narrow when the alloy comprises at least 990% or by weight of gold.
  • the document EP 0 685 565 discloses a gold alloy, having a Vickers hardness of 100 or more, 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 quantity of rare earths is therefore less than the quantity 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 usable in the manufacture of timepieces or durable jewelry. This is all the more true for the luxury industry whose quality of articles must be an. 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 to be sufficient to obtain excellent resistance of the article to scratches in particular.
  • the present invention solves this problem through the development of a gold-based alloy and two alloying elements allowing the manufacture of high quality articles and having great durability.
  • 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 as a percentage by weight or in tenths of a percentage by weight (per thousand,% o), relative to the weight of the gold alloy.
  • the gold alloy comprises 990 ⁇ by weight of gold, this means that it comprises 990 grams of the gold element per 1000 grams of gold alloy.
  • the alloy includes traces of impurities, generally resulting from the metals used to form the alloy.
  • these possible impurities represent less than 50 ppm by weight of the 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 timepiece or jewelry item.
  • 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 timepiece or jewelry item according to the invention can be a piece of jewelry, a leather-based item 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 handbag buckle, tie pin, cuff links, pliers for a 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 999.5 ⁇ by weight of gold, and even more advantageously between 999 ⁇ and 999.3 ⁇ by weight of gold. According to a particular embodiment, it can comprise 999.2 ⁇ by weight of gold.
  • alloying elements advantageously only the 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 quantity greater than 0 ⁇ and less than or equal to 5 ⁇ of the first alloy element and of the second alloy element.
  • the gold alloy comprises between at least 999 ⁇ by weight of gold, it comprises a total quantity greater than 0 ⁇ and less than or equal to 1 ⁇ of the first alloy element and of the second alloy element.
  • the timepiece or jewelry item according to the invention advantageously comprises a gold alloy comprising between 5.10 and 8.00 ⁇ by weight of the first alloy 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 timepiece or jewelry item according to the invention advantageously comprises a gold alloy comprising between 2.00 and 4.90 ⁇ by weight of the second alloy 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 the 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 alloy of gold. It is advantageously greater than or equal to 0.5 ⁇ , more advantageously greater than or equal to 0.6 ⁇ , even more advantageously greater than or equal to 0.7 ⁇ .
  • the gold alloy has a weight ratio 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 their mixtures.
  • 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 an amount by weight less 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 0 ⁇ and less than or equal to 5 ⁇ of the first alloying element and the second alloying element. More advantageously, it comprises at least 999 ⁇ by weight of gold and a total quantity greater than 0 ⁇ and less than or equal to 1 ⁇ of the first alloying element and the second alloying element. Preferably, this alloy comprises between 999 ⁇ and 999.5 ⁇ by weight of gold, more preferably between 999 ⁇ and 999.3 ⁇ by weight of gold.
  • the respective quantities and combinations of the alloying elements are as indicated above.
  • 0 ⁇ Q1 + Q2 ⁇ 5 ⁇ 0 ⁇ Q1 + Q2 ⁇ 1 ⁇ .
  • step a the respective proportions of the metals correspond to the proportions of the final alloy. This step is carried out conventionally, according to techniques known to those skilled in the art.
  • Step a) consists in mixing and melting the different metals so as to form a homogeneous mixture. This step is advantageously carried out by heating the mixture until the desired temperature is reached.
  • step a) is carried out at a temperature between 850 ° C and 1500 ° C, advantageously between 900 ° C and 1450 ° C.
  • the optional heat treatment in step b) corresponds to a homogenization treatment which involves re-solution of the alloy.
  • step b) and the work hardening in step c) make it possible to increase the hardness of the alloy.
  • the 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 a homogeneity of the mechanical properties of the alloy by dissolving and the diffusion of alloying elements in gold. It also makes it possible to reduce or eliminate any internal stresses which may result from heterogeneous solidification. Finally, it makes it possible to freeze the microstructure and to keep a supersaturated solution, which can prove useful when step d) of aging is implemented.
  • Step b) can be followed by a cooling step allowing the structure of the alloy to be frozen, prior to step c). It advantageously consists in carrying out a thermal quenching in air or in water. Even though the air quenching is much slower than the 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 into alloying elements, in particular when one or more alloying elements are sparingly or not soluble at room 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 between 65 and 90%.
  • the embodiments in which the first alloying element is silicon are particularly advantageous since it is possible to obtain a Vickers hardness greater than 100 HV with 75% hardening and greater than 110 HV with 90% hardening. In the other embodiments, 90% work hardening is preferred.
  • step c) The alloy obtained following step c) can optionally be subjected to an aging step, in particular by heating. However, the process is advantageously free from step d) of aging.
  • the optional aging step d) corresponds to a 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 d) of aging 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.
  • Aging can be carried out in air or, when the composition of the gold alloy is sensitive to oxidation, under an inert atmosphere, for example under argon.
  • the alloy obtained after hardening, or aging can then be shaped according to conventional techniques to form the timepiece or jewelry item 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 electro-erosion or by means of a laser.
  • the shaping can be carried out by additive manufacturing.
  • the alloy is previously transformed into powder form.
  • the present invention also relates to a method of manufacturing a timepiece or jewelry from the gold alloy presently described according to the conventional steps.
  • step c) corresponds to work hardening. It was carried out using a bench rolling mill. A strip of thickness less than 7 mm is passed several times between the two rollers of the rolling mill, the spacing of which is controlled by a hand wheel. Two levels of theoretical deformation were applied at 75% and 90%. To ensure better reproducibility during this step, all of the samples are deformed to the height of 0.35 mm per pass with a constant rolling speed of the rolls of 3.95 m / minute.
  • Examples 2 to 14 relate to different compositions of gold alloys comprising at least one alloying element from calcium, yttrium, titanium, germanium, tin and silicon.
  • the figure 1 illustrates the raw hardnesses of casting, after work hardening, possibly after aging, of these compositions and of pure gold (CE-1).
  • the figure 1 shows that the effect of hardening by solid solution (crude casting) remains insufficient for these compositions of gold alloy. However, the malleability of these compositions allows deformation rates of 90% without cracking.
  • compositions AuPd (CE-2) and AuZr (CE-3) are not satisfactory insofar as the hardness gain is less than 100 HV (80-85 HV) and remains too limited compared to pure gold ( CE-1, 65 HV).
  • the composition AuCa (CE-14) could be suitable for having a sufficiently hard gold alloy.
  • this composition requires an aging step.
  • it is difficult to implement because the calcium is sparingly 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 90% hardening .
  • the composition Au 999 Ge 0.665 Si 0.335 could not be used due to the complete cracking of the sample after work hardening of a few percent.
  • the composition Au 999 Ge 1 (not shown) has a relatively low raw casting hardness comparable to that of fine gold (30 HV). After 75% work 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 a main alloying element (INV-12 and INV-13).

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Adornments (AREA)
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)

Priority Applications (1)

Application Number Priority Date Filing Date Title
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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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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EP3656245A1 true EP3656245A1 (de) 2020-05-27
EP3656245B1 EP3656245B1 (de) 2022-04-06

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114351002A (zh) * 2022-01-11 2022-04-15 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

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
EP0685565A1 (de) 1993-09-06 1995-12-06 Mitsubishi Materials Corporation Gold-ornament-material,gehaertet durch legieren mit minderen komponenten
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

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
EP0685565A1 (de) 1993-09-06 1995-12-06 Mitsubishi Materials Corporation Gold-ornament-material,gehaertet durch legieren mit minderen komponenten
EP0882805A1 (de) * 1993-09-06 1998-12-09 Mitsubishi Materials Corporation Goldlegierung für Schmuckzwecke, ausgehärtet mittels zusätzen niedrige Mengen von Legierungselementen
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

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
ASTM ASTM: "ASTM Standard B562", STANDARD SPECIFICATION FOR REFINED GOLD, 31 December 2005 (2005-12-31), West Conshohocken, PA, XP055562362, Retrieved from the Internet <URL:http://web.askewindustrial.com/ASTM/B562.pdf> [retrieved on 20190227], DOI: 10.1520/B0562-95R05 *
VIVEK CHIDAMBARAM ET AL: "Development of Au-Ge based candidate alloys as an alternative to high-lead content solders", JOURNAL OF ALLOYS AND COMPOUNDS., vol. 490, no. 1-2, 23 October 2009 (2009-10-23), CH, pages 170 - 179, XP055562623, ISSN: 0925-8388, DOI: 10.1016/j.jallcom.2009.10.108 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114351002A (zh) * 2022-01-11 2022-04-15 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
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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