EP3543368B1 - Hoch-entropie-legierungen für verkleidungskomponenten - Google Patents

Hoch-entropie-legierungen für verkleidungskomponenten Download PDF

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Publication number
EP3543368B1
EP3543368B1 EP18162716.7A EP18162716A EP3543368B1 EP 3543368 B1 EP3543368 B1 EP 3543368B1 EP 18162716 A EP18162716 A EP 18162716A EP 3543368 B1 EP3543368 B1 EP 3543368B1
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Prior art keywords
atomic concentration
alloy according
equal
alloy
major elements
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EP18162716.7A
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English (en)
French (fr)
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EP3543368A1 (de
Inventor
Joël Porret
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Swatch Group Research and Development SA
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Swatch Group Research and Development SA
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Priority to EP18162716.7A priority Critical patent/EP3543368B1/de
Priority to JP2019019528A priority patent/JP6802866B2/ja
Priority to US16/271,925 priority patent/US20190292633A1/en
Priority to KR1020190017908A priority patent/KR102180486B1/ko
Priority to CN201910207000.1A priority patent/CN110306094A/zh
Publication of EP3543368A1 publication Critical patent/EP3543368A1/de
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/18Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/44Ferrous alloys, e.g. steel alloys containing chromium with nickel with molybdenum or tungsten
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C30/00Alloys containing less than 50% by weight of each constituent
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C30/00Alloys containing less than 50% by weight of each constituent
    • C22C30/02Alloys containing less than 50% by weight of each constituent containing copper
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C30/00Alloys containing less than 50% by weight of each constituent
    • C22C30/04Alloys containing less than 50% by weight of each constituent containing tin or lead
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C30/00Alloys containing less than 50% by weight of each constituent
    • C22C30/06Alloys containing less than 50% by weight of each constituent containing zinc
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/18Ferrous alloys, e.g. steel alloys containing chromium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/18Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/24Ferrous alloys, e.g. steel alloys containing chromium with vanadium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/18Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/46Ferrous alloys, e.g. steel alloys containing chromium with nickel with vanadium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/18Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/50Ferrous alloys, e.g. steel alloys containing chromium with nickel with titanium or zirconium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/18Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/58Ferrous alloys, e.g. steel alloys containing chromium with nickel with more than 1.5% by weight of manganese
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C45/00Amorphous alloys
    • C22C45/006Amorphous alloys with Cr as the major constituent
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C45/00Amorphous alloys
    • C22C45/008Amorphous alloys with Fe, Co or Ni as the major constituent
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C45/00Amorphous alloys
    • C22C45/08Amorphous alloys with aluminium as the major constituent
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/02Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
    • GPHYSICS
    • G04HOROLOGY
    • G04BMECHANICALLY-DRIVEN CLOCKS OR WATCHES; MECHANICAL PARTS OF CLOCKS OR WATCHES IN GENERAL; TIME PIECES USING THE POSITION OF THE SUN, MOON OR STARS
    • G04B37/00Cases

Definitions

  • the present invention relates to a high entropy alloy and to a covering component for a watch or a piece of jewelry made from this alloy.
  • Austenitic stainless steels generally contain nickel and also have limited hardnesses ( ⁇ 300 HV in the annealed state). Martensitic stainless steels are hard (> 600 HV) but ferromagnetic. Finally, titanium alloys, such as grade 5 titanium (Ti6Al4V), certainly represent the best compromise among the properties presented above but they have a particular color and hardness (around 350 HV for grade 5 titanium) not significantly higher. higher than some austenitic stainless steels for example. For comparison, amorphous metals, also very interesting for cladding components, may have hardnesses greater than 500 HV. However, very specific implementations are necessary to obtain components made of amorphous metal, which further limits their use as a trim element.
  • high entropy alloys In the field of watch dressing, there is therefore always a strong interest in obtaining hard crystalline alloys (> 400 HV in the annealed state), non-ferromagnetic, corrosion resistant and exhibiting good polishability.
  • high entropy alloys currently very studied and which constitute a new class of alloys, are particularly promising.
  • high entropy alloys are considered to be all alloys containing at least 5 main elements with an atomic fraction between 5 and 35%, the elements having an atomic fraction of less than 5% being considered as minor.
  • alloys containing 4 main elements can also be considered as high entropy alloys.
  • the high entropy resulting from the mixing of numerous main elements would make it possible to stabilize the phases in solid solution with respect to the formation of potentially embrittling intermetallic phases.
  • unique and little observed properties in traditional alloys based on one or two main elements are obtained.
  • obtaining simple phases in solid solution is very advantageous, because this promotes good polishability and good corrosion resistance.
  • the mixing of many different elements results in solid solution hardening.
  • high hardnesses have thus already been demonstrated, particularly for those which have a centered cubic structure.
  • the object of the invention is to provide a high entropy alloy with a composition specifically adapted to the needs of the trim components.
  • the present invention thus aims more particularly to develop an alloy having, after processing, a hardness greater than or equal to 400 HV, a non-ferromagnetic behavior and a high corrosion resistance.
  • the alloy contains 3 main elements which are Cr, Fe and V, each having atomic concentrations between 20 and 40%. It also contains as main element Al and / or Si having the effect of destroying the ferromagnetic behavior of the alloy. These elements each have an atomic concentration greater than or equal to 5% with a total atomic concentration for Al and Si less than or equal to 25%.
  • the alloy can also optionally comprise one or more main elements chosen from Mn, Mo, Ti and Ni each having an atomic concentration greater than or equal to 5% with a total atomic concentration for these 4 main elements less than or equal to 35 %.
  • the Ni content is specifically maintained at a value less than 20% to avoid, during implementation and in particular heat treatments, the formation of undesirable phases which weaken the material and reduce corrosion resistance. .
  • Some grades are also Ni-free to ensure high biocompatibility.
  • the remainder can be composed of possible impurities and / or of one or more minor elements each having an atomic concentration of less than 5%.
  • the material obtained after processing has, depending on the composition and the thermomechanical treatments, a single phase with a centered cubic structure, which promotes good resistance to corrosion and good polishability for a better surface finish or in the case of of multiphase alloys, a matrix (main phase) with a centered cubic structure reinforced with nanoprecipitates. It has the other advantage of having a color close to that of austenitic stainless steels.
  • the present invention relates to high entropy alloys and to their use for trim components for watches or jewelry, in particular for components intended to be in contact with the skin.
  • the covering component can be a caseband, a back, a bezel, a push-piece, crown, bracelet link, dial, hand, dial index, clasp, etc.
  • a watch case 1 produced in the alloy according to the invention is shown in figure 1 .
  • the alloys have between 4 and 9 main elements.
  • the term “main elements” is understood to mean elements having an atomic concentration greater than or equal to 5%. Alloys contain the following 3 main elements: Cr, Fe, V with an atomic concentration of between 20 and 40%. They also contain 1 or 2 main elements chosen from Al and Si with a total atomic concentration for these two elements less than or equal to 25%. They also optionally comprise one or more main elements chosen from Mn, Mo, Ti and Ni with a total atomic concentration for these 4 main elements of less than or equal to 35%.
  • the total atomic concentration for all of the aforementioned main elements is greater than or equal to 80%.
  • the balance may optionally contain minor elements chosen from the list comprising Si, Mn, Mo, Al, Nb, H, B, C, N, O, Mg, Sc, Ti, Cu, Ni, Zn, Ga, Ge, Sr, Y, Zr, Rh, Pd, Ag, Sn, Sb, Hf, Ta, W, Pt and Au.
  • the term “minor elements” is understood to mean elements having an atomic concentration of less than 5%.
  • the balance may also contain residual impurities from processing.
  • alloys according to the invention all the forming processes can be envisaged. It is in particular possible to obtain these alloys by casting, by powder metallurgy processes, by additive manufacturing techniques or even by layer deposition technologies. This also includes possible thermomechanical treatments (heat treatment, hot deformation, cold deformation) and stages of sintering and hot isostatic compression (HIP).
  • thermomechanical treatments heat treatment, hot deformation, cold deformation
  • HIP hot isostatic compression
  • the alloys according to the invention After shaping and carrying out any thermomechanical treatments, the alloys according to the invention mainly exhibit a centered cubic structure (BCC), which can be disordered (structure A2, space group Im3m ) or ordered (structure B2, space group Pm3m ).
  • BCC centered cubic structure
  • a single-phase microstructure can be obtained at ambient temperature for the alloys according to the invention which contain neither Ni, nor Ti as main elements, nor minor elements, which promotes corrosion resistance and polishability. .
  • the alloys according to the invention can exhibit a microstructure with a second phase in the form of precipitates which in certain cases make it possible to improve the mechanical properties (hardness, ductility, toughness, etc. .).
  • the precipitates are small with sizes which may be nanometric and when the matrix has an almost unchanged composition, i.e. that it retains a composition which satisfies the definition of the alloys according to the invention (phases in multi-element solid solution), good polishability, high corrosion resistance and the absence of ferromagnetism are retained.
  • the addition of Ni or Ni and Ti is particularly advantageous, since this makes it possible to obtain very hardening nanoprecipitates.
  • the alloys according to the invention have, after processing, the following properties required for the trim components: non-ferromagnetic behavior, hardness greater than or equal to 400HV, high corrosion resistance, with in particular no sign of corrosion after salt spray test according to ISO 9227.
  • alloy compositions which meet all these criteria after processing are given in Table 1 below.
  • the alloys were produced by arc melting ( arc melting ) without further heat treatment.
  • atomic fractions have been rounded to the nearest whole number and hardnesses have been rounded to the nearest ten.

Claims (11)

  1. Hoch-Entropie-Legierung mit einer Zusammensetzung, die zwischen 4 und 9 Hauptelemente enthält, ausgewählt aus der Liste bestehend aus Cr, Fe, V, AI, Si, Mn, Mo, Ti und Ni mit:
    - 3 Hauptelementen, nämlich Cr, Fe und V mit jeweils einer Atomkonzentration zwischen 20 und 40 %,
    - 1 oder 2 Hauptelement(en), ausgewählt aus AI und Si, die jeweils eine Atomkonzentration von größer oder gleich 5 % aufweisen, wobei die Gesamtkonzentration für diese 2 Hauptelemente kleiner oder gleich 25 % ist,
    - 0, 1, 2, 3 oder 4 Hauptelementen, ausgewählt aus Mn, Mo, Ti und Ni, die jeweils eine Atomkonzentration von größer oder gleich 5 % mit einer Gesamtatomkonzentration für diese 4 Hauptelemente kleiner oder gleich 35 % aufweisen,
    wobei die Gesamtatomkonzentration für alle 4 bis 9 Hauptelemente größer oder gleich 80 % ist und der Rest aus Verunreinigungen und/oder einem oder mehreren Nebenelementen mit einer Atomkonzentration von jeweils weniger als 5 % besteht.
  2. Legierung nach Anspruch 1, dadurch gekennzeichnet, dass das oder die Nebenelement/e aus der Liste ausgewählt ist/sind, die Si, Mn, Mo, AI, Nb, H, B, C, N, O, Mg, Sc, Ti, Cu, Ni, Zn, Ga, Ge, Sr, Y, Zr, Rh, Pd, Ag, Sn, Sb, Hf, Ta, W, Pt und Au umfasst.
  3. Legierung nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass sie zwischen 0,005 und 0,1 % in atomarer Konzentration von B als Nebenelement enthält.
  4. Legierung nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass sie zwischen 7 und 15 % in atomarer Konzentration von Ni als Hauptelement enthält.
  5. Legierung nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass sie einer der folgenden Formeln in ihren Atomanteilen ausgedrückt entspricht: Al10Fe25Cr40V25, Al10Fe40Cr25V25, Al10Fe25Cr25V40, Al10Fe30Cr30V30, Al5Cr30Fe30Mo5V30, Al6Cr30Fe30Mo5V29, Al5Cr30Fe30Si5V30, Al5Cr30Fe30Mn5V30, Al13Cr25Fe25Ni12V25, Cr31Fe31V31Si7 oder Fe25Cr25V25Al10Ni10Ti5.
  6. Legierung nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass sie eine einzige Mischkristallphase mit kubisch zentrierter Struktur umfasst.
  7. Legierung nach einem der vorhergehenden Ansprüche 1 bis 5, dadurch gekennzeichnet, dass sie eine zweiphasige Struktur aufweist, die eine Matrix mit einer kubisch zentrierten Struktur und Nanoausfällungen umfasst.
  8. Legierung nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass sie ein nicht ferromagnetisches Verhalten zeigt und keine Anzeichen von Korrosion aufweist, nachdem sie dem Salzsprühnebeltest nach ISO 9227 unterzogen wurde.
  9. Legierung nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass sie eine Härte HV10 von größer oder gleich 400 aufweist.
  10. Verkleidungskomponente für Uhren oder Schmuck, dadurch gekennzeichnet, dass sie aus der Legierung nach einem der vorhergehenden Ansprüche hergestellt ist.
  11. Komponente nach Anspruch 10, dadurch gekennzeichnet, dass sie aus der Liste ausgewählt ist, die einen Gehäusemittelteil, einen Boden, eine Lünette, einen Drücker, eine Krone, ein Glied eines Armbands, eine Schließe, eine Schnalle, einen Dorn, ein Zifferblatt, einen Zeiger und einen Zifferblattindex umfasst.
EP18162716.7A 2018-03-20 2018-03-20 Hoch-entropie-legierungen für verkleidungskomponenten Active EP3543368B1 (de)

Priority Applications (5)

Application Number Priority Date Filing Date Title
EP18162716.7A EP3543368B1 (de) 2018-03-20 2018-03-20 Hoch-entropie-legierungen für verkleidungskomponenten
JP2019019528A JP6802866B2 (ja) 2018-03-20 2019-02-06 外装部品のための高エントロピー合金
US16/271,925 US20190292633A1 (en) 2018-03-20 2019-02-11 High entropy alloy for external components
KR1020190017908A KR102180486B1 (ko) 2018-03-20 2019-02-15 외부 컴포넌트를 위한 고엔트로피 합금
CN201910207000.1A CN110306094A (zh) 2018-03-20 2019-03-19 用于外部组件的高熵合金

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EP18162716.7A EP3543368B1 (de) 2018-03-20 2018-03-20 Hoch-entropie-legierungen für verkleidungskomponenten

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EP3543368B1 true EP3543368B1 (de) 2020-08-05

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CN (1) CN110306094A (de)

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JP6802866B2 (ja) 2020-12-23
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