EP3121297B1 - Herstellungsverfahren einer schmuckkomponente aus platinlegierung - Google Patents

Herstellungsverfahren einer schmuckkomponente aus platinlegierung Download PDF

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EP3121297B1
EP3121297B1 EP16177653.9A EP16177653A EP3121297B1 EP 3121297 B1 EP3121297 B1 EP 3121297B1 EP 16177653 A EP16177653 A EP 16177653A EP 3121297 B1 EP3121297 B1 EP 3121297B1
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hardness
semi
finished product
alloy
platinum
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English (en)
French (fr)
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EP3121297A1 (de
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Fréderic Diologent
Damien Colas
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Richemont International SA
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Cartier International AG
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    • 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
    • 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
    • C22C5/04—Alloys based on a platinum group metal

Definitions

  • the present invention relates to a process for obtaining an ornamental component made of a platinum alloy containing at least 80% by weight of platinum, having a particularly high hardness and which can be machined by the usual methods.
  • the component is intended for applications in watchmaking, jewelry, fine jewelry, eyewear, writing instruments, luxury accessories, and other decorative or functional applications where visual appearance is also important.
  • alloys of precious metals in particular platinum, since the properties of pure precious metal, such as platinum, are often not satisfactory, in particular in due to low hardness as well as medium gloss.
  • the document EP0621349 describes a process for hardening platinum on the surface with a surface layer containing boron.
  • the method described only allows the treatment of a finished part, and tends to affect the aesthetic appearance of the latter (color and temperature). On the other hand, even hardened, the surface can be damaged.
  • the restoration or refreshing of such a part requires a specific post-restoration process which can only be carried out under very specific conditions and is therefore not within the reach of restoration workshops equipped with conventional means.
  • the document GB2279967 provides a high purity platinum alloy containing cerium in small amounts. This alloy makes it possible to achieve hardnesses comparable, or even slightly higher, to that of a standard platinum alloy. Cerium being an element very sensitive to oxidation, the preparation of the alloy must be carried out under vacuum or under an inert gas, making the process complex. On the other hand, cerium has an average solid solubility in platinum, which also limits the homogeneity of the alloy obtained.
  • the document GB578956 provides a hardened platinum alloy by addition of oxides using a sintering process.
  • the process is complex and depends on the size of the powders and the homogeneity of the compound to be obtained.
  • the document JP1988145759 offers a platinum alloy containing in particular iron, palladium and copper, and the hardening of which is obtained in part by an operation of plastic deformation to the shape of the part to be obtained and by a heat treatment operation after the setting steps in shape.
  • This solution is therefore limited on the one hand by expensive matrix tools, and on the other hand by the heat treatment step which could promote recrystallization of the material, or even cause a surface texture to appear.
  • the document EP0947595 discloses a dispersion hardened platinum alloy. This alloy uses dispersion oxides in order to oxidize the non-noble metal. On the other hand, the dispersing elements not only tend to favor the wear of the tools, but they also make the polishing steps difficult.
  • Heat treatment hardening processes on finished platinum alloy components are also known. They have the disadvantage that the grain structure is changed, which affects the texture of polished surfaces.
  • EP2705170A1 proposes a process for obtaining a very high hardness platinum alloy by means of an amorphous structure, namely a metallic glass.
  • This high hardness involves a very particular material and a shaping process and moreover require very specific tools and very high associated costs.
  • the application of this technology to a wide range of products, very diverse in their geometries, is therefore not the most suitable from an industrial point of view.
  • the component obtained by the process of the invention has a hardness typically 25% to 50% higher than the hardness of the starting alloy.
  • the process allows the component to be obtained in its final shape and hardness without the need for heat treatment on the final component to modify its hardness.
  • the or severe plastic deformation cycles of step of hardening are intended to transform the crystal structure of platinum alloy into a grain structure ultrafine (English ultrafine grained UFG).
  • ultra-fine grain structure is meant a structure having a grain size of at least less than 1 ⁇ m in at least one grain orientation.
  • the grain size of the ultra-fine grain structure may be less than 500 nm, and even less than 200 nm, or even 100 nm.
  • the alloy comprises at least 80.0% of platinum and one or more of the following chemical elements: between 0% and 6% of ruthenium; between 0% and 5% copper; between 0% and 3% gallium.
  • the severe plastic deformation cycle (s) can be achieved using one of the methods, or a combination of these methods, comprising: equal channel angular pressing (ECAP ), angular extrusion according to equal channels (ECAP- accordance), high pressure torsion (high pressure torsion tube twisting or high pressure, or HPTT HPT), accumulative roll-bonding (accumulative roll bonding, ARB), repetitive corrugation and straightening (straightening and repetitive corrugation, SCR ), asymmetric rolling ( asymmetric rolling, ASR), cyclic extrusion-compression ( cyclic extrusion-compression, CEC), roller stamping (rotary swaging), or any other suitable method to obtain said structure with ultra-fine grains.
  • ECAP equal channel angular pressing
  • ECAP- accordance high pressure torsion
  • HPTT HPT high pressure torsion tube twisting or high pressure, or HPTT HPT
  • accumulative roll-bonding accumulative roll bonding
  • ARB repetitive corrugation and straightening
  • the method comprises a step of shaping the alloy so as to give the semi-finished product a particular shape.
  • the semi-finished product may take the form of a plate, bar, ingot, billet, or any other shape advantageous for the subsequent machining step.
  • the method also comprises a step comprising one or more restorative heat treatments.
  • Restorative heat treatment can be performed after the severe plastic deformation cycle, or between the severe plastic deformation cycles.
  • the parameters of the restorative heat treatment are adjusted so as not to completely relax the platinum alloy, so as not to degrade the second hardness obtained during the work hardening step.
  • the restorative heat treatment (s) is carried out at a temperature below 600 ° C., above which the mechanical properties of the alloy drop rapidly and the ductility increases.
  • the restorative heat treatment (s) is preferably carried out at a temperature above 250 ° C and below 600 ° C. In fact, below 250 ° C., the restorative heat treatment may have little or no effect for treatment times which are less than 1 hour, the thermal activation not being sufficient.
  • the figure 1 reports the evolution of the elastic limit (Rm in MPa) and of the maximum stress (Rp0.2 in MPa) for an alloy comprising at least 80.0% of platinum as a function of the temperature.
  • the figure 2 reports the evolution of the hardness (HV) of the same alloy as a function of temperature.
  • the restorative heat treatment (s) is preferably carried out at a temperature between 250 ° C and 500 ° C, or even between 250 ° C and 400 ° C.
  • Restoration heat treatment time can be one hour or less than one hour.
  • the method comprises one or more heat hardening treatments.
  • the hardening heat treatment or treatments make it possible to further increase the second hardness of the semi-finished product by the precipitation of the alloying elements.
  • the process of the invention makes it possible to obtain the semi-finished product with a second hardness which is at least 25% and even 50% higher than the first hardness of the starting alloy.
  • the machining step may include a material removal process such as turning, milling, grinding, spark erosion, cutting, laser or water jet cutting, or any other suitable process.
  • the machining step can also comprise a method of shaping by deformation, or by assembly.
  • the machining step can also include one or more finishing treatments, such as machining, satin-finishing, polishing, sandblasting, micro-blasting, etching or any other suitable mechanical process.
  • finishing treatments such as machining, satin-finishing, polishing, sandblasting, micro-blasting, etching or any other suitable mechanical process.
  • the machining step provides the component in its final shape and hardness. It is therefore not necessary to carry out heat treatment on the component obtained by the present process to modify its hardness. Indeed, the second hardness obtained for the semi-finished product by the hardening step corresponds to the desired hardness of the component.
  • the ornamentation component may comprise a horological component, for example a component of the movement, the bracelet or a covering component such as the case, the bezel, the back.
  • the ornamentation component may also include a component for jewelry, jewelry, eyewear, writing instruments, luxury accessories (key ring, lighter, cufflink, tie bar, etc.) and others. decorative or functional applications where visual appearance is also important.
  • an alloy comprising about 95% platinum and about 5% ruthenium is provided, having a nominal first hardness of about 120Hv.
  • the alloy is subjected to the first forming step and to the hardening step comprising at least one cycle of severe plastic deformation, so as to increase the second hardness of the semi-finished product to a value of at least 250 Hv.
  • the hardened semi-finished product has a second hardness of about 250 Hv.
  • the hardening step is carried out by the high pressure twisting method, the semi-finished product has a second hardness greater than 400 Hv.
  • an alloy comprising about 95% platinum, between 1% and 4% copper and between 1% and 4% gallium (for a total of about 5% copper and gallium), having a first nominal hardness of at least 200Hv.
  • the semi-finished product when the hardening step is carried out by the accumulative co-rolling method, the semi-finished product has a second hardness of about 300 Hv.
  • the semi-finished product can then be subjected to a subsequent hardening heat treatment step so as to increase the second hardness to a value of about 400 Hv.
  • the hardening step comprising at least one cycle of severe plastic deformation which can be followed by at least one restorative heat treatment, as described above.
  • the process for obtaining an ornamental component described here applies to any alloy comprising at least 80% by mass of platinum, and which may contain one or more of the following chemical elements: between 0% and 6% of ruthenium; between 0% and 5% copper; between 0% and 3% gallium.

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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)

Claims (18)

  1. Verfahren zur Herstellung einer Zierkomponente, die mindestens 80 Gewichts-% Platin umfasst, wobei das Verfahren umfasst:
    Bereitstellen eines Rohmaterials, das mindestens 80,0 Gewichts-% Platin umfasst und eine erste Härte aufweist;
    Durchführen eines Schritts zur Kaltverformung der Legierung, damit ein Halbfertigerzeugnis mit einer zweiten Härte erhalten wird, die höher ist als die erste Härte; und
    Durchführen eines Schritts zum Zerspanen des Halbfertigerzeugnisses zum Erhalten der Komponente,
    dadurch gekennzeichnet, dass der Schritt zur Kaltverformung mindestens einen Zyklus zur hochgradigen plastischen Verformung umfasst, der mittels Gleichkanalwinkelpressen durchgeführt wird, damit die kristallografische Struktur der Legierung in eine Struktur mit einer Korngröße von unter 1 µm und vorzugsweise unter 500 nm umgewandelt wird.
  2. Verfahren zur Herstellung einer Zierkomponente, die mindestens 80 Gewichts-% Platin umfasst, wobei das Verfahren umfasst:
    Bereitstellen eines Rohmaterials, das mindestens 80,0 Gewichts-% Platin umfasst und eine erste Härte aufweist;
    Durchführen eines Schritts zur Kaltverformung der Legierung, damit ein Halbfertigerzeugnis mit einer zweiten Härte erhalten wird, die höher ist als die erste Härte; und
    Durchführen eines Schritts zum Zerspanen des Halbfertigerzeugnisses zum Erhalten der Komponente;
    dadurch gekennzeichnet, dass der Schritt zur Kaltverformung mindestens einen Zyklus zur hochgradigen plastischen Verformung umfasst, der mittels kumulativem Walzen durchgeführt wird, damit die kristallografische Struktur der Legierung in eine Struktur mit einer Korngröße von unter 1 µm und vorzugsweise unter 500 nm umgewandelt wird.
  3. Verfahren zur Herstellung einer Zierkomponente, die mindestens 80 Gewichts-% Platin umfasst, wobei das Verfahren umfasst:
    Bereitstellen eines Rohmaterials, das mindestens 80,0 Gewichts-% Platin umfasst und eine erste Härte aufweist;
    Durchführen eines Schritts zur Kaltverformung der Legierung, damit ein Halbfertigerzeugnis mit einer zweiten Härte erhalten wird, die höher ist als die erste Härte; und
    Durchführen eines Schritts zum Zerspanen des Halbfertigerzeugnisses zum Erhalten der Komponente;
    dadurch gekennzeichnet, dass der Schritt zur Kaltverformung mindestens einen Zyklus zur hochgradigen plastischen Verformung umfasst, der mittels Hochdrucktorsion durchgeführt wird, damit die kristallografische Struktur der Legierung in eine Struktur mit einer Korngröße von unter 1 µm und vorzugsweise unter 500 nm umgewandelt wird.
  4. Verfahren zur Herstellung einer Zierkomponente, die mindestens 80 Gewichts-% Platin umfasst, wobei das Verfahren umfasst:
    Bereitstellen eines Rohmaterials, das mindestens 80,0 Gewichts-% Platin umfasst und eine erste Härte aufweist;
    Durchführen eines Schritts zur Kaltverformung der Legierung, damit ein Halbfertigerzeugnis mit einer zweiten Härte erhalten wird, die höher ist als die erste Härte; und
    Durchführen eines Schritts zum Zerspanen des Halbfertigerzeugnisses zum Erhalten der Komponente,
    dadurch gekennzeichnet, dass der Schritt zur Kaltverformung mindestens einen Zyklus zur hochgradigen plastischen Verformung umfasst, der mittels Rundverformung durchgeführt wird, damit die kristallografische Struktur der Legierung in eine Struktur mit einer Korngröße von unter 1 µm und vorzugsweise unter 500 nm umgewandelt wird.
  5. Verfahren zur Herstellung einer Zierkomponente, die mindestens 80 Gewichts-% Platin umfasst, wobei das Verfahren umfasst:
    Bereitstellen eines Rohmaterials, das mindestens 80,0 Gewichts-% Platin umfasst und eine erste Härte aufweist;
    Durchführen eines Schritts zur Kaltverformung der Legierung, damit ein Halbfertigerzeugnis mit einer zweiten Härte erhalten wird, die höher ist als die erste Härte; und
    Durchführen eines Schritts zum Zerspanen des Halbfertigerzeugnisses zum Erhalten der Komponente;
    dadurch gekennzeichnet, dass der Schritt zur Kaltverformung mindestens einen Zyklus zur hochgradigen plastischen Verformung umfasst, der mittels Cyclic extrusion compression durchgeführt wird, damit die kristallografische Struktur der Legierung in eine Struktur mit einer Korngröße von unter 1 µm und vorzugsweise unter 500 nm umgewandelt wird.
  6. Verfahren zur Herstellung einer Zierkomponente, die mindestens 80 Gewichts-% Platin umfasst, wobei das Verfahren umfasst:
    Bereitstellen eines Rohmaterials, das mindestens 80,0 Gewichts-% Platin umfasst und eine erste Härte aufweist;
    Durchführen eines Schritts zur Kaltverformung der Legierung, damit ein Halbfertigerzeugnis mit einer zweiten Härte erhalten wird, die höher ist als die erste Härte; und
    Durchführen eines Schritts zum Zerspanen des Halbfertigerzeugnisses zum Erhalten der Komponente;
    dadurch gekennzeichnet, dass der Schritt zur Kaltverformung mindestens einen Zyklus zur hochgradigen plastischen Verformung umfasst, der mittels Repetitive corrugation and straightening durchgeführt wird, damit die kristallografische Struktur der Legierung in eine Struktur mit einer Korngröße von unter 1 µm und vorzugsweise unter 500 nm umgewandelt wird.
  7. Verfahren nach einem der Ansprüche 1 bis 6,
    ferner umfassend mindestens eine Wärmebehandlung zum Erholungsglühen, die nach dem Zyklus zur hochgradigen plastischen Verformung durchgeführt wird.
  8. Verfahren nach einem der Ansprüche 1 bis 7,
    ferner umfassend mindestens eine Wärmebehandlung zum Härten, die so ausgelegt ist, dass sie die Härte des gehärteten Halbfertigerzeugnisses durch Ausscheidung von Legierungselementen weiter erhöht.
  9. Verfahren nach einem der Ansprüche 1 bis 8,
    wobei die Legierung in Gewichtsprozent mindestens 80,0 % Platin und ein oder mehrere der folgenden chemischen Elemente enthält: zwischen 0% und 6% Ruthenium; zwischen 0% und 5% Kupfer; zwischen 0% und 3% Gallium.
  10. Verfahren nach einem der Ansprüche 1 bis 9,
    wobei die Legierung in Gewichtsprozent ungefähr 95% Platin und ungefähr 5% Ruthenium enthält und eine erste Härte von ungefähr 120 HV aufweist; und wobei das Halbfertigerzeugnis nach dem Schritt zur Kaltumformung eine Härte von mindestens 250 HV aufweist.
  11. Verfahren nach Anspruch 10,
    wobei der Schritt zur Kaltumformung mit dem kumulativen Walzverfahren durchgeführt wird, damit das Halbfertigerzeugnis eine Härte von mindestens 250 HV aufweist.
  12. Verfahren nach Anspruch 10,
    wobei der Schritt zur Kaltumformung mit dem Hochdrucktorsionsverfahren durchgeführt wird, damit das Halbfertigerzeugnis eine Härte von über 400 HV aufweist.
  13. Verfahren nach einem der Ansprüche 1 bis 8,
    wobei die Legierung in Gewichtsprozent ungefähr 95% Platin, ungefähr 2% Kupfer und ungefähr 3% Gallium enthält und eine erste Härte von ungefähr 200 HV aufweist; und
    wobei das Halbfertigerzeugnis nach dem Schritt zur Kaltumformung eine Härte von mindestens 300 HV aufweist.
  14. Verfahren nach Anspruch 13,
    wobei der Schritt zur Kaltumformung mit dem kumulativen Walzverfahren durchgeführt wird, damit das Halbfertigerzeugnis eine Härte von mindestens 300 HV aufweist.
  15. Verfahren nach Anspruch 8 und 14,
    wobei das Halbfertigerzeugnis nach der Wärmebehandlung zum Härten eine Härte von mindestens 400 HV aufweist.
  16. Verfahren nach Anspruch 13,
    wobei der Schritt zur Kaltumformung mit dem Hochdrucktorsionsverfahren durchgeführt wird, damit das Halbfertigerzeugnis eine Härte von mindestens 600 HV aufweist.
  17. Verfahren nach einem der Ansprüche 1 bis 14, ferner umfassend einen Schritt zur Formgebung der Legierung, damit das Halbfertigerzeugnis eine bestimmte Form erhält, insbesondere Platte, Barren, Block oder Bolzen.
  18. Verwendung der mit dem Verfahren nach einem der Ansprüche 1 bis 17 hergestellten Zierkomponente für eins der folgenden Gebiete:
    Uhrenindustrie, Schmuckindustrie, Juwelierskunst, Brillenherstellung, Schreibgeräte, Luxusaccessoires oder dekorative Anwendungen.
EP16177653.9A 2015-07-23 2016-07-01 Herstellungsverfahren einer schmuckkomponente aus platinlegierung Active EP3121297B1 (de)

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CN107058788B (zh) * 2017-04-12 2019-02-12 深圳市星光达珠宝首饰实业有限公司 一种多元铂钌合金及其制备方法
CN107671159B (zh) * 2017-10-18 2020-02-18 大连理工大学 超声振动辅助脱模的限制性模压模具及晶粒细化方法
CN107893201B (zh) * 2017-11-17 2019-09-20 合肥工业大学 制备超细晶材料的往复挤扭镦等径角成形方法
GB202015742D0 (en) * 2020-10-05 2020-11-18 Oxmet Tech Limited A platinum alloy composition

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DE838067C (de) 1942-02-07 1952-03-27 Baker Platinum Limited, London Gesinterte Platinlegierung
FR2381832A1 (fr) * 1977-02-23 1978-09-22 Johnson Matthey Co Ltd Alliages de joaillerie
JPS63145759A (ja) 1986-12-09 1988-06-17 Citizen Watch Co Ltd 装飾用白金合金の熱処理方法
DE4313272C1 (de) 1993-04-23 1994-05-05 Degussa Oberflächen gehärtete Gegenstände aus Platin- und Palladiumlegierungen und Verfahren zu deren Herstellung
JPH0734162A (ja) 1993-07-14 1995-02-03 Nagahori:Kk 硬質高純度白金合金
US5846352A (en) * 1996-11-22 1998-12-08 Kretchmer; Steven Heat treatment of a platinum-gallium alloy for jewelry
DE19813988C1 (de) 1998-03-28 1999-10-28 Heraeus Gmbh W C Verfahren zur Herstellung eines aus durch feinverteilte, kleine Teilchen aus Unedelmetalloxid dispersionsverfestigtem Platinwerkstoff bestehenden, geschweißten, insbesondere mindestens eine Innenwand aufweisenden Formkörpers, isnbesondere eines Rohres
US6562158B1 (en) * 1998-12-01 2003-05-13 Steven Kretchmer Heat-treatable platinum-gallium-palladium alloy for jewelry
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