EP3444370B1 - Alliage à base de cuivre destiné à la fabrication de verres métalliques solidifiés - Google Patents

Alliage à base de cuivre destiné à la fabrication de verres métalliques solidifiés Download PDF

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Publication number
EP3444370B1
EP3444370B1 EP17186878.9A EP17186878A EP3444370B1 EP 3444370 B1 EP3444370 B1 EP 3444370B1 EP 17186878 A EP17186878 A EP 17186878A EP 3444370 B1 EP3444370 B1 EP 3444370B1
Authority
EP
European Patent Office
Prior art keywords
alloy
glass
alloys
melt
metallic
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.)
Active
Application number
EP17186878.9A
Other languages
German (de)
English (en)
Other versions
EP3444370A1 (fr
Inventor
Ralf Busch
Alexander Elsen
Moritz Stolpe
Hans-Jürgen Wachter
Eugen Milke
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.)
Heraeus Deutschland GmbH and Co KG
Original Assignee
Heraeus Deutschland GmbH and Co KG
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Heraeus Deutschland GmbH and Co KG filed Critical Heraeus Deutschland GmbH and Co KG
Priority to EP17186878.9A priority Critical patent/EP3444370B1/fr
Priority to US16/639,236 priority patent/US11214854B2/en
Priority to KR1020207004348A priority patent/KR20200031132A/ko
Priority to PCT/EP2018/071580 priority patent/WO2019034506A1/fr
Priority to JP2020507032A priority patent/JP6997860B2/ja
Priority to CN201880052813.1A priority patent/CN110997959A/zh
Publication of EP3444370A1 publication Critical patent/EP3444370A1/fr
Application granted granted Critical
Publication of EP3444370B1 publication Critical patent/EP3444370B1/fr
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C30/00—Alloys containing less than 50% by weight of each constituent
    • C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D21/00—Casting non-ferrous metals or metallic compounds so far as their metallurgical properties are of importance for the casting procedure; Selection of compositions therefor
    • B22D21/02—Casting exceedingly oxidisable non-ferrous metals, e.g. in inert atmosphere
    • B22D21/025—Casting heavy metals with high melting point, i.e. 1000 - 1600 degrees C, e.g. Co 1490 degrees C, Ni 1450 degrees C, Mn 1240 degrees C, Cu 1083 degrees C
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D25/00—Special casting characterised by the nature of the product
    • B22D25/06—Special casting characterised by the nature of the product by its physical properties
    • 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
    • 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
    • C22C30/00—Alloys containing less than 50% by weight of each constituent
    • C22C30/04—Alloys containing less than 50% by weight of each constituent containing tin or lead
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C45/00—Amorphous alloys
    • C22C45/001—Amorphous alloys with Cu as the major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C9/00—Alloys based on copper

Definitions

  • Metallic glasses also known as amorphous metals
  • amorphous metals have very high strength. Furthermore, they show little or no change in volume during solidification, so that the possibility of near-net-shape shaping without solidification shrinkage opens up.
  • metallic glasses with dimensions of at least 1 mm ⁇ 1 mm ⁇ 1 mm can be produced with an alloy, then these glasses are also referred to as bulk metallic glasses or solid metallic glasses (English: “Bulk Metallic Glasses” ( “BMG” )) .
  • metallic glasses especially metallic solid glasses, are very interesting construction materials that are in principle suitable for the production of components in series production processes such as injection molding, without the need for further processing steps after the shaping has taken place would be.
  • a measure of the ability of an alloy to form glass is therefore, for example, the maximum or "critical" diameter up to which a specimen cast from the melt still has an essentially amorphous structure. This is also referred to as the critical casting thickness.
  • Metallic glasses can not only be formed by melting metallurgical processes, but also shaped by thermoplastic forming at comparatively low temperatures in the same way as thermoplastics or silicate glasses. For this purpose, the metallic glass is first heated above the glass transition point and then behaves like a highly viscous liquid that can be deformed with relatively low forces. Following the deformation, the material is cooled back below the glass transition temperature.
  • thermoplastic forming also involves heating the metallic glass to a temperature above the gas formation temperature T g .
  • T g the crystallization temperature
  • Improved glass forming ability of an alloy upon cooling from the melt does not automatically translate to improved heat resistance (ie, higher ⁇ T x ) of the metallic glass made from that alloy. These are usually independent parameters that can even behave in opposite directions. Therefore, if it is intended to provide an alloy with as high a ⁇ T x value as possible, care must also be taken that this does not occur at the expense of the glass-forming ability on cooling from the melt.
  • the alloys most commonly used for the manufacture of metallic glasses are currently Zr-based alloys.
  • a disadvantage of these alloys is the relatively high material price for zirconium.
  • U.S. 5,618,359 describes Zr- and Cu-based alloys for the production of metallic glasses.
  • the alloys contain at least 4 alloying elements.
  • One of the Cu-based alloys has the composition Cu 45 Ti 33.8 Zr 11.3 Ni 10 and can be cast into an amorphous specimen with a thickness of 4 mm.
  • Cu- and Zr-based alloys for the production of metallic glasses. With dimensions of at least 1 mm, these are referred to as " bulk metallic glasses" .
  • the Cu and Zr alloys each contain a total of 4 alloying elements (Cu, Zr, Ti and Ni).
  • the alloy with the composition Cu 47 Ti 34 Zr 11 Ni 8 shows the best compromise between good glass-forming ability on cooling from the melt and the highest possible ⁇ T x value.
  • U.S. 2006/0231169 A1 describes alloys for the production of metallic glasses, which can be Cu-based, among other things.
  • the alloy produced in Example 3 has the composition Cu 47 Ti 33 Zr 7 Ni 8 Si 1 Nb 4 . Starting with the alloy Cu 47 Ti 34 Zr 11 Ni 8 , Ti was substituted by Si and Zr by Nb.
  • the alloy produced in Comparative Example 3 has the composition Cu 47 Ti 33 Zr 11 Ni 8 Si 1 .
  • the improved heat resistance should also not adversely affect other relevant properties such as hardness.
  • alloys with the composition defined above have high ⁇ T x values and thus improved heat resistance while still having good glass-forming ability.
  • the alloys according to the invention are therefore, for example, very well suited for thermoplastic forming.
  • the atomic ratio of Ti to Zr is defined with the values for a and b.
  • the alloy according to the invention contains oxygen, this is present in a maximum concentration of 1.7 at%, for example 0.01-1.7 at% or 0.02-1.0 at%.
  • the proportion of unavoidable impurities in the alloy is less than 0.1 at%, preferably less than 0.05 at% or even less than 0.01 at%.
  • the composition of the alloy can be determined by inductively coupled plasma optical emission spectrometry (ICP-OEC).
  • the glass transition temperature T g and the crystallization temperature T x are determined by DSC (differential scanning calorimetry). It will be the onset temperature used. The cooling and heating rates are 20 °C/min. The DSC measurement is carried out in an argon atmosphere in an aluminum oxide crucible.
  • the alloy is preferably an amorphous alloy.
  • the alloy according to the invention has a crystallinity of less than 50%, more preferably less than 25% or is even completely amorphous.
  • a completely amorphous material shows no diffraction reflections in X-ray diffraction.
  • the crystalline fraction is determined via DSC as a ratio of the maximum enthalpy of crystallization (determined by crystallization of a completely amorphous reference sample) and the actual enthalpy of crystallization in the sample.
  • the invention further relates to a method for producing the alloy described above, the alloy being obtained from a melt containing Cu, Ti, Zr, Ni, Sn and optionally Si.
  • the melt is preferably maintained under an inert gas atmosphere (e.g., an inert gas atmosphere).
  • an inert gas atmosphere e.g., an inert gas atmosphere
  • the components of the alloy can each be introduced into the melt in their elemental form (e.g. elemental Cu etc.). Alternatively, it is also possible that two or more of these metals are pre-alloyed in a starting alloy and this starting alloy is then introduced into the melt.
  • elemental form e.g. elemental Cu etc.
  • the alloy is obtained as a solid.
  • the melt can, for example, be poured into a mold or subjected to atomization.
  • the alloy can be atomized in the form of a powder, whose particles are substantially spherical in shape.
  • Suitable atomization processes are known to those skilled in the art, for example gas atomization (e.g. using nitrogen or an inert gas such as argon or helium as the atomization gas), plasma atomization, centrifugal atomization or crucible-less atomization (e.g. a "rotating electrode” process (REP) method, in particular a "Plasma Rotating Electrode” process (PREP)).
  • REP rotating electrode
  • PREP Pasma Rotating Electrode
  • EIGA electrode induction-melting gas atomization
  • inductive melting of the starting material and subsequent gas atomization.
  • the powder obtained from the atomization can then be used in an additive manufacturing process or subjected to thermoplastic molding.
  • the alloy according to the invention Due to the very good glass-forming ability of the alloy according to the invention, it can easily be obtained in the form of an amorphous alloy.
  • the present invention relates to a metallic bulk glass that contains the alloy described above or even consists of this.
  • the metallic solid glass preferably has dimensions of at least 1 mm ⁇ 1 mm ⁇ 1 mm.
  • the metallic bulk glass has a crystallinity of less than 50%, more preferably less than 25%, or is even completely amorphous.
  • the production of the metallic bulk glass can be carried out using methods that are known to those skilled in the art.
  • the alloy described above is subjected to additive manufacturing, thermoplastic forming, or is melt cast in a mold.
  • the alloy may be used in the form of a powder (e.g., a powder obtained via atomization).
  • Additive manufacturing describes a process in which a component is built up layer by layer on the basis of digital 3D design data by depositing material.
  • a thin layer of powder is first applied to the construction platform.
  • a sufficiently high energy input for example in the form of a laser or electron beam, at least partially melts the powder at the points specified by the computer-generated design data.
  • the construction platform is then lowered and another powder application takes place.
  • the further layer of powder is at least partially melted again and connects to the layer underneath at the defined points.
  • Thermoplastic forming is usually done at a temperature between the T g and T x of the alloy.
  • Alloys E4, E5 and E8 according to the invention were produced, the respective composition of which is given in Table 1 below.
  • the alloys CE1-CE5 were produced.
  • the ⁇ T x value (i.e. the distance between the crystallization temperature T x and the glass formation temperature T g ) and the critical casting thickness D c of the alloys are given in Table 1.
  • the glass transition temperature T g and the crystallization temperature T x were determined by DSC based on the onset temperatures and with cooling and heating rates of 20 °C/min.
  • the critical casting thickness D c was determined as follows: A cylinder with a length of 50mm and a specific diameter is cast. The determination of D c is done by cutting the sample about 10-15mm away from the gate (to exclude the heat affected zone) and measuring the XRD at the cutting point over the entire cross-section.
  • the alloy of comparative example CE1 has the composition Cu 47 Ti 34 Zr 11 Ni 8 .

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)
  • Laminated Bodies (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Claims (9)

  1. Alliage qui présente la composition suivante :
    Cu47at%-(x+y+z)(TiaZrb)cNi7at%+xSn1at%+ySiz
    dans laquelle
    c = 43 - 47 % atomique, a = 0,65-0,85, b=0,15-0,35, où a+b=1,00 ;
    x = 5-7 % atomique ;
    y = 0-2 % atomique, z = 0-2 % atomique, où y+z ≤ 4 % atomique ;
    dans lequel l'alliage contient éventuellement de l'oxygène dans une concentration d'au maximum 1,7 % atomique et le reste est constitué d'impuretés inévitables.
  2. Alliage selon la revendication 1, dans lequel a = 0,70-0,80 et b = 0,20-0,30.
  3. Alliage selon l'une quelconque des revendications précédentes, dans lequel z = 0 % atomique.
  4. Alliage selon la revendication 1 ou 2, dans lequel 0 < z ≤ 2 % atomique.
  5. Procédé pour la production de l'alliage selon l'une quelconque des revendications 1 à 4, dans lequel l'alliage est obtenu à partir d'une masse fondue qui contient du Cu, du Ti, du Zr, du Ni, du Sn et éventuellement du Si.
  6. Procédé selon la revendication 5, dans lequel la masse fondue est coulée dans un moule ou soumise à une pulvérisation.
  7. Verre massif métallique contenant l'alliage selon l'une quelconque des revendications 1 à 4.
  8. Verre massif métallique selon la revendication 7 présentant des dimensions d'au moins 1 mm x 1 mm x 1 mm.
  9. Procédé pour la fabrication d'un verre massif métallique, dans lequel l'alliage selon l'une quelconque des revendications 1 à 4 est soumis à un procédé de fabrication additif ou à un moulage thermoplastique ou est coulé dans un moule sous forme de masse fondue.
EP17186878.9A 2017-08-18 2017-08-18 Alliage à base de cuivre destiné à la fabrication de verres métalliques solidifiés Active EP3444370B1 (fr)

Priority Applications (6)

Application Number Priority Date Filing Date Title
EP17186878.9A EP3444370B1 (fr) 2017-08-18 2017-08-18 Alliage à base de cuivre destiné à la fabrication de verres métalliques solidifiés
US16/639,236 US11214854B2 (en) 2017-08-18 2018-08-09 Copper-based alloy for the production of bulk metallic glasses
KR1020207004348A KR20200031132A (ko) 2017-08-18 2018-08-09 벌크 금속 유리의 생산을 위한 구리계 합금
PCT/EP2018/071580 WO2019034506A1 (fr) 2017-08-18 2018-08-09 Alliage à base de cuivre pour la fabrication de verres massifs métalliques
JP2020507032A JP6997860B2 (ja) 2017-08-18 2018-08-09 バルク金属ガラスの製造のための銅に基づく合金
CN201880052813.1A CN110997959A (zh) 2017-08-18 2018-08-09 用于生产块体金属玻璃的铜基合金

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP17186878.9A EP3444370B1 (fr) 2017-08-18 2017-08-18 Alliage à base de cuivre destiné à la fabrication de verres métalliques solidifiés

Publications (2)

Publication Number Publication Date
EP3444370A1 EP3444370A1 (fr) 2019-02-20
EP3444370B1 true EP3444370B1 (fr) 2022-03-09

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EP17186878.9A Active EP3444370B1 (fr) 2017-08-18 2017-08-18 Alliage à base de cuivre destiné à la fabrication de verres métalliques solidifiés

Country Status (6)

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US (1) US11214854B2 (fr)
EP (1) EP3444370B1 (fr)
JP (1) JP6997860B2 (fr)
KR (1) KR20200031132A (fr)
CN (1) CN110997959A (fr)
WO (1) WO2019034506A1 (fr)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111360276A (zh) * 2020-03-24 2020-07-03 上海材料研究所 一种tc4高氧粉末改性后用于3d打印原料的方法
EP3895827B1 (fr) 2020-04-17 2023-11-15 Heraeus Amloy Technologies GmbH Procédé de fabrication d'un corps creux en métal amorphe
WO2024046742A1 (fr) 2022-08-29 2024-03-07 Universität des Saarlandes Alliage pour produire des verres métalliques massifs et corps façonnés à partir de ceux-ci
KR20240065910A (ko) 2022-11-07 2024-05-14 정지원 상체 체중 분리 견인 허리보호 장치

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RU2009254C1 (ru) * 1952-04-01 1994-03-15 Научно-производственное объединение "Гамма" Аморфный сплав на основе железа с улучшенным состоянием поверхности
US5618359A (en) 1995-02-08 1997-04-08 California Institute Of Technology Metallic glass alloys of Zr, Ti, Cu and Ni
US20060102315A1 (en) * 2002-09-27 2006-05-18 Lee Jung G Method and apparatus for producing amorphous alloy sheet, and amorphous alloy sheet produced using the same
CN1219905C (zh) 2002-12-30 2005-09-21 中国科学院物理研究所 铜基大块非晶合金
KR100530040B1 (ko) 2003-06-23 2005-11-22 학교법인연세대학교 구리계 비정질 합금
KR100701027B1 (ko) 2005-04-19 2007-03-29 연세대학교 산학협력단 연성이 우수한 단일상 비정질 합금
CN101538690B (zh) * 2008-03-21 2011-04-20 比亚迪股份有限公司 一种非晶合金及其制备方法
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KR20150141103A (ko) * 2014-06-09 2015-12-17 삼성전자주식회사 비정질 금속 기지 복합 재료
CN104117672B (zh) 2014-07-31 2017-01-18 华中科技大学 一种制备/成形非晶合金及其复合材料的方法
KR101532409B1 (ko) 2014-09-22 2015-06-30 서울대학교산학협력단 가공경화가 가능한 비정질 금속 기지 복합재료
WO2016112507A1 (fr) 2015-01-14 2016-07-21 东莞帕姆蒂昊宇液态金属有限公司 Boîtier de montre en alliage amorphe, montre et procédé de fabrication associé
KR101752976B1 (ko) * 2015-10-07 2017-07-11 서울대학교산학협력단 가공경화능 제어 비정질 합금 기지 복합재의 제조 방법 및 그에 따라 제조된 복합재

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Also Published As

Publication number Publication date
JP6997860B2 (ja) 2022-02-04
KR20200031132A (ko) 2020-03-23
US11214854B2 (en) 2022-01-04
JP2020531683A (ja) 2020-11-05
CN110997959A (zh) 2020-04-10
EP3444370A1 (fr) 2019-02-20
US20200208243A1 (en) 2020-07-02
WO2019034506A1 (fr) 2019-02-21

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