WO2015184438A1 - Verres or-aluminium portant des métaux de terres rares - Google Patents

Verres or-aluminium portant des métaux de terres rares Download PDF

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Publication number
WO2015184438A1
WO2015184438A1 PCT/US2015/033496 US2015033496W WO2015184438A1 WO 2015184438 A1 WO2015184438 A1 WO 2015184438A1 US 2015033496 W US2015033496 W US 2015033496W WO 2015184438 A1 WO2015184438 A1 WO 2015184438A1
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WO
WIPO (PCT)
Prior art keywords
alloy
metallic glass
percent
range
atomic fraction
Prior art date
Application number
PCT/US2015/033496
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English (en)
Inventor
Jong Hyun Na
Danielle Duggins
Chase Crewdson
Maximilien LAUNEY
Marios D. Demetriou
William L. Johnson
Original Assignee
Glassimetal Technology, Inc.
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Application filed by Glassimetal Technology, Inc. filed Critical Glassimetal Technology, Inc.
Publication of WO2015184438A1 publication Critical patent/WO2015184438A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C45/00—Amorphous alloys
    • C22C45/003—Amorphous alloys with one or more of the noble metals as major constituent
    • 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
    • C22C1/11—Making amorphous alloys
    • 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 disclosure is directed to Au-Al-RE alloys, where RE is a rare earth metal, capable of forming a metallic glass.
  • the disclosure provides Au-Al-RE metallic glass-forming alloys and metallic glasses comprising various other additions including, but not limited to, Cu, Pd, Sn and Mg.
  • RE designates a rare-earth metal selected from Y, Sc and the Lanthanides, which include La, Ce Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, and Lu, or a combination thereof.
  • the disclosure provides a metallic glass-forming alloy or metallic glass that comprises at least Au, Al, and RE, where the atomic fraction of Au is in the range of 40 to 90 percent, the atomic fraction of Al is in the range of 0.5 to 40 percent, and the atomic fraction of RE is in the range of 1 to 20 percent.
  • RE is one of Y, Er, or Dy, or combinations thereof.
  • RE is Y.
  • the atomic fraction of Al is in the range of 2 to 20 percent.
  • the atomic fraction of Al is in the range of 4 to 18 percent.
  • the atomic fraction of Y is in the range of 3 to 15 percent.
  • the atomic fraction of Y is in the range of 5 to 12 percent.
  • the alloy or metallic glass also comprises Cu in an atomic fraction in the range of up to 20 percent.
  • the alloy or metallic glass also comprises Cu in an atomic fraction in the range of 0.5 to 10 percent.
  • the alloy or metallic glass also comprises Cu in an atomic fraction in the range of 1 to 5 percent.
  • the alloy or metallic glass also comprises Pd in an atomic fraction in the range of up to25 percent.
  • the alloy or metallic glass also comprises Pd in an atomic fraction in the range of 0.5 to 20 percent.
  • the alloy or metallic glass also comprises Pd in an atomic fraction in the range of 1 to 15 percent.
  • the disclosure provides an alloy or a metallic glass having a composition represented by the following formula (subscripts denote atomic percentages):
  • a ranges from 0.5 to 40;
  • b ranges from 1 to 20;
  • c is up to 20;
  • b ranges from 3 to 15.
  • b ranges from 5 to 12.
  • c ranges from 0.5 to 10. In another embodiment of the alloy or metallic glass, c ranges from 1 to 5.
  • d ranges from 0.5 to 20. In another embodiment of the alloy or metallic glass, d ranges from 1 to 15.
  • the weight fraction of Au is at least 75 percent.
  • the alloy or metallic glass also comprises Sn in an atomic fraction in the range of up to 10 percent.
  • the alloy or metallic glass also comprises Sn in an atomic fraction in the range of 0.5 to 5 percent.
  • the alloy or metallic glass also comprises Mg in an atomic fraction in the range of up to20 percent.
  • the alloy or metallic glass also comprises Mg in an atomic fraction in the range of 0.5 to 10 percent.
  • the alloy or metallic glass also comprises Mg in an atomic fraction in the range of 0.5 to 5 percent.
  • the alloy or metallic glass also comprises any of Ag, Pt, Rh, Ir, Fe, Ni, Co, Ru, Cr, Mo, Mn, Ti, Zr, Hf, W, Re, Be, Ca, Si, P, S, Ge, Ga, In, Sb, and Bi, or combinations thereof, in an atomic fraction of up to 10 percent.
  • the alloy or metallic glass also comprises any of Ag, Pt, Rh, Ir, Fe, Ni, Co, Ru, Cr, Mo, Mn, Ti, Zr, Hf, W, Re, Be, Ca, Si, P, S, Ge, Ga, In, Sb, and Bi, or combinations thereof, in an atomic fraction of up to 5 percent.
  • the alloy demonstrates a critical casting thickness of at least 1 micrometer.
  • the alloy demonstrates a critical casting thickness of at least 10 micrometers.
  • the alloy demonstrates a critical casting thickness of at least 50 micrometers.
  • the alloy demonstrates a critical casting thickness of at least 100 micrometers.
  • the alloy demonstrates a critical casting thickness of at least
  • the alloy demonstrates a critical casting thickness of at least 1 millimeter.
  • the alloy demonstrates a critical casting thickness of at least 5 millimeters.
  • the metallic glass is a coating or film having a thickness of at least 100 nanometers.
  • the metallic glass is a coating or film having a thickness of at least 100 nm. In another embodiment, the metallic glass is a coating or film having a thickness of at least 1 micrometer.
  • the temperature of the melt prior to quenching is at least 100°C above the liquidus temperature of the alloy.
  • the temperature of the melt prior to quenching is at least
  • the metallic glass demonstrates a glass transition temperature of at least 150°C.
  • the metallic glass demonstrates a glass transition temperature of at least 200°C.
  • the metallic glass demonstrates a glass transition temperature of at least 250°C.
  • the metallic glass demonstrates a Vickers hardness value of at least 400 kgf/mm 2 .
  • the metallic glass demonstrates a Vickers hardness value of at least 440 kgf/mm 2 .
  • the metallic glass demonstrates a yellow color.
  • the metallic glass demonstrates a pink or rose color. In yet another embodiment, the metallic glass demonstrates a color having CIELAB coordinates with L* in the range of 65 to 120, a* in the range of -5 to 15, and b* in the range of 5 to 40.
  • the metallic glass demonstrates a color having CIELAB coordinates with L* in the range of 65 to 85, a* in the range of 0 to 3, and b* in the range of 5 to 20.
  • the disclosure is also directed to an alloy or a metallic glass having compositions selected from a group consisting of: Au74Cu2Y 8 Ali 5 Sni, Au72Cu 3 Y 8 Ali 6 Pdi,
  • FIG. 1 provides an x-ray diffractogram verifying the amorphous structure of a 68 ⁇ thick metallic glass foil with composition Au 6 9.5Cu 2 Y 9 Al 15 5 Pd 4 (Example 5).
  • FIG. 2 provides calorimetry scans for sample metallic glasses in accordance with embodiments of the disclosure.
  • the glass transition temperature T g (where detectable), crystallization temperature T x , solidus temperature T s , and liquidus temperature 7 ⁇ are indicated by arrows.
  • the following disclosure relates to Au-Al-RE based metallic glass-forming alloys and metallic glasses.
  • Au-based jewelry alloys typically contain Au at weight fractions of less than 100%. Hallmarks are used by the jewelry industry to indicate the Au metal content. Au weight fractions of about 75.0% (18 Karat), 58.3% (14 Karat), 50.0% (12 Karat), and 41.7% (10 Karat) are commonly used hallmarks in gold jewelry. In certain embodiments, this disclosure is directed to glass-forming Au-based alloys or metallic glasses that satisfy the 18 Karat hallmark. Hence, in such embodiments the Au weight fraction ranges from 74 to 90 percent.
  • the glass-forming ability of each alloy is quantified by the "critical casting thickness,” defined as the largest lateral dimension in which the amorphous phase can be formed when processed by a method of quenching an alloy from the high temperature melt state.
  • the glass-forming ability of each alloy can also be quantified by the "critical rod diameter,” defined as the largest rod diameter in which the amorphous phase can be formed when processed by a method of water quenching a quartz tube having 0.5 mm thick walls containing a molten alloy.
  • the critical cooling rate R c in K/s and critical casting thickness t c in mm are related via the following approximate empirical formula:
  • the critical cooling rate for an alloy having a critical casting thickness of about 1 mm is about 10 3 K/s.
  • Metal alloys having critical cooling rates in excess of 10 12 K/s are typically referred to as non-glass formers, as it is physically impossible to achieve such cooling rates over a meaningful thickness.
  • Metal alloys having critical cooling rates in the range of 10 5 to 10 12 K/s are typically referred to as marginal glass formers, as they are able to form glass over thicknesses ranging from 1 to 100 micrometers according to Eq. (2).
  • Metal alloys having critical cooling rates on the order of 10 3 or less, and as low as 1 or 0.1 K/s, are typically referred to as bulk glass formers, as they are able to form glass over thicknesses ranging from 1 millimeter to several centimeters.
  • the glass-forming ability of a metallic alloy is, to a very large extent, dependent on the composition of the alloy.
  • the compositional ranges for alloys capable of forming marginal glass formers are considerably broader than those for forming bulk glass formers.
  • alloys, and/or metallic glasses formed of alloys, with compositions with Au weight fraction of at least 75.0 percent satisfying the 18-Karat hallmark are presented in Table 1.
  • the metallic glasses may be in the form of foils.
  • Several example metallic glasses in the form of foils are presented.
  • the foil thicknesses of the example metallic glasses along with the Au weight percentages are listed in Table 1.
  • Table 1 Sample metallic glasses brmed of alloys with compositions with Au weight frac tion of at least 75.0 percent satisfying the 18-Karat ha lmark
  • FIG. 1 provides an x-ray diffractogram verifying the amorphous structure of a 68 ⁇ thick metallic glass foil with composition Au 69 .5Cu2Y 9 Al15.5Pd4 (Example 5).
  • FIG. 2 provides calorimetry scans for the sample metallic glasses listed in Table 1.
  • the glass transition temperature T g (where detectable), crystallization temperature T x , solidus temperature T s , and liquidus temperature 7 ⁇ are indicated by arrows in FIG. 2, and are listed in Table 2.
  • the enthalpy of crystallization AH X for each of the sample metallic glasses is also listed in Table 2.
  • T g is generally detectable for the Pd-bearing alloys.
  • the glass transition temperature of the rest of the alloys in Table 2 is expected to be at least 250°C. In general, the alloys according to the disclosure are expected to exhibit a T g of at least 150°C, and in some embodiments, at least 200°C.
  • the addition of Pd and Sn can decrease the liquidus temperature of the alloy as compared to the Pd-free and Sn-free alloys respectively.
  • the decrease in liquidus temperature can reduce the driving force of crystallization and can increase the critical casting thickness of the alloy.
  • Table 2 The glass transition temperature T g (where detectable), crystallization temperature T x , solidus temperature T s , and liquidus temperature ⁇ /, and enthalpy of crystallization AH X of sample metallic glasses according to the disclosure.
  • the metallic glasses of the disclosure demonstrate various colors, particularly yellow and pink/rose colors.
  • the sample metallic glasses listed in Tables 1 and 2 have a yellow color.
  • the CIELAB color coordinates of the sample metallic glasses listed in Tables 1 and 2 are listed in Table 3.
  • the Vickers hardness values of sample metallic glasses according to the current disclosure are listed in Table 4.
  • the Vickers hardness values of the sample metallic glasses are shown to be greater than 440 Kgf/mm 2 , ranging from about 447 to about 500 Kgf/mm 2 .
  • one method for producing the alloy ingots involves arc melting of the appropriate amounts of elemental constituents over a water-cooled copper hearth under inert atmosphere.
  • the alloy ingots for the sample alloys of Tables 1 and 2 were produced using this method.
  • the purity levels of the constituent elements were as follows: Au 99.99%, Al 99.999%, Y 99.9%, Cu 99.995%, Pd 99.95%, and Sn 99.999%.
  • the ingots may be produced by inductively melting the elemental constituents, where the melting crucible may be a ceramic such as alumina or zirconia, graphite, sintered crystalline silica, or a water-cooled hearth made of copper or silver.
  • one method for producing metallic glass foils from the alloy ingots involves a splat quench processing.
  • the sample metallic glasses of Tables 1 and 2 were produced using this method.
  • a spherical alloy ingot of about 100 mg is levitated and melted inductively under a pressure of 0.05 mbar reaching a temperature of at least 1000°C, and the spherical liquid droplet was subsequently dropped and splatted between two copper platens to form a cylindrical splat foil having a diameter between 10 and 20 mm and thickness between 10 and 100 ⁇ .
  • the metallic glass can be a coating or film. In some embodiments, the metallic glass is a coating or film having a thickness of at least 100 nanometers. In still other embodiments, the metallic glass is a coating or film having a thickness of at least 1 micrometer.
  • the metallic glass can be applied using coating processes, including spray coating, chemical or electrochemical plating, thermal spraying, physical vapor deposition (PVD) processes, chemical vapor deposition (CVD) processes, sputtering or other suitable coating process.
  • coating processes including spray coating, chemical or electrochemical plating, thermal spraying, physical vapor deposition (PVD) processes, chemical vapor deposition (CVD) processes, sputtering or other suitable coating process.
  • the Au- Al-RE alloy can be applied to a substrate using a spray coating process in some
  • the Au-Al-RE alloy can be atomized by passing through a stream of gas (e.g. argon) and through a nozzle to impact a surface of the substrate.
  • a stream of gas e.g. argon
  • the Au- Al-RE alloy deposits on the surface of the substrate, it solidifies and bonds to the substrate creating a metallic glass coating or film.
  • Standard methods can be used to evaluate cosmetic appeal including color, gloss, and haze.
  • the color of objects may be determined by the wavelength of light that is reflected or transmitted without being absorbed, assuming incident light is white light.
  • the visual appearance of objects may vary with light reflection or transmission. Additional appearance attributes may be based on the directional brightness distribution of reflected light or transmitted light, commonly referred to glossy, shiny, dull, clear, and haze, among others.
  • Color measurements were taken using a Konica Minolta CM700d hand-held spectrophotometer with a 3 -mm SAV aperture, SCI specularity, 10-degree angle, and F2 light source. Color evaluation by brightness (L*), a* (between red and green) and b* (between blue and yellow) can be performed. Measurements are according to CIE/ISO standards for illuminants, observers, and the L * a * b * color scale.
  • the standards include: (a) ISO 1 1664-1 :2007(E)/CIE S 014-1/E:2006: Joint ISO/CIE Standard: Colorimetry— Part 1 : CIE Standard Colorimetric Observers; (b) ISO 11664-2 :2007(E)/CIE S 014-2/E:2006: Joint ISO/CIE Standard: Colorimetry— Part 2: CIE Standard Illuminants for Colorimetry, (c) ISO 11664-3 :2012(E)/CIE S 014-3/E:201 1 : Joint ISO/CIE Standard: Colorimetry— Part 3 : CIE Tristimulus Values; and (d) ISO 1 1664-4:2008(E)/CIE S 014-4/E:2007: Joint ISO/CIE Standard: Colorimetry— Part 4: CIE 1976 L* a* b * Colour Space. Test Methodology for Measuring Hardness
  • the Vickers hardness (FTVO. l) of sample metallic glasses was measured using a Vickers microhardness tester. Eight tests were performed where micro-indentions were inserted on -50 ⁇ - ⁇ 1 ⁇ metallic glass splats using a load of 100 g and a duel time of 10 s. A load of 100 g resulted in indentation depth of 2 to 3 ⁇ , which ensures the validity of the hardness measurements, as the indentation depth is less than 10% of the sample thickness. Measurements were performed on a metallic substrate with hardness of 607 HV0.5, which is considerably higher than the measured hardness of the Sample metallic glass.
  • the alloys, metallic glasses, and various non-limiting embodiments as described herein can be included in various products.
  • Such products can be any product known in the art.
  • the products can be a device, such as an electronic device.
  • the device can be a telephone, such as a mobile phone, and a land-line phone, or any communication device, such as a smart phone, including, for example an iPhone®, and/or an electronic email sending/receiving device.
  • the alloys, metallic glasses, and various non-limiting embodiments can be used in conjunction with a display, such as a digital display, a TV monitor, an electronic -book reader, a portable web-browser (e.g., iPad®), a watch (e.g., Apple WatchTM), and/or a computer monitor.
  • a display such as a digital display, a TV monitor, an electronic -book reader, a portable web-browser (e.g., iPad®), a watch (e.g., Apple WatchTM), and/or
  • the device can also be an entertainment device, including a portable DVD player, conventional DVD player, Blue-Ray disk player, video game console, music player, such as a portable music player (e.g., iPod®), etc.
  • Devices include control devices, such as those that control the streaming of images, videos, sounds (e.g., Apple TV®), or a remote control for a separate electronic device.
  • the device can be a part of a computer or its accessories, laptop keyboard, laptop track pad, desktop keyboard, mouse, and speaker.

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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)
  • Glass Compositions (AREA)

Abstract

L'invention concerne des alliages formant du verre métallique et des verres métalliques, à base de Au-Al et de terres rares, qui comprennent divers autres verres métalliques des éléments ajoutés y compris mais pas exclusivement Cu, Pd, Sn et Mg. Dans certains modes de réalisation, les verres métalliques selon l'invention satisfont à l'alliage d'or estampillé 18 carats et présentent des couleurs incluant le jaune et rose.
PCT/US2015/033496 2014-05-30 2015-06-01 Verres or-aluminium portant des métaux de terres rares WO2015184438A1 (fr)

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Cited By (2)

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WO2018001564A1 (fr) * 2016-06-30 2018-01-04 Universität des Saarlandes Alliage d'or blanc générateur de verre massif
CN108315673A (zh) * 2018-03-02 2018-07-24 华中科技大学 一种不含非金属元素的金基非晶合金及其制备方法

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CN105522137B (zh) * 2014-10-24 2018-09-11 比亚迪股份有限公司 一种金属陶瓷复合体及其制备方法
US10895004B2 (en) 2016-02-23 2021-01-19 Glassimetal Technology, Inc. Gold-based metallic glass matrix composites
US10801093B2 (en) 2017-02-08 2020-10-13 Glassimetal Technology, Inc. Bulk palladium-copper-phosphorus glasses bearing silver, gold, and iron
CN112708797A (zh) * 2020-11-25 2021-04-27 西安汇创贵金属新材料研究院有限公司 一种紫色金合金及其制备方法
CN115011833B (zh) * 2021-12-21 2023-08-29 昆明理工大学 一种改善紫色18k金铝合金韧性的配方及其制备方法
US12054819B1 (en) * 2023-09-15 2024-08-06 Chow Sang Sang Jewellery Company Limited Amorphous alloy

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WO2018001564A1 (fr) * 2016-06-30 2018-01-04 Universität des Saarlandes Alliage d'or blanc générateur de verre massif
DE102016008074A1 (de) * 2016-06-30 2018-01-04 Universität des Saarlandes Massivglasbildende Weißgoldlegierung
CN108315673A (zh) * 2018-03-02 2018-07-24 华中科技大学 一种不含非金属元素的金基非晶合金及其制备方法
CN108315673B (zh) * 2018-03-02 2019-06-18 华中科技大学 一种不含非金属元素的金基非晶合金及其制备方法

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