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EP2944401B1 - Procédé de fabrication d'un composant en alliage métallique comportant une phase amorphe - Google Patents

Procédé de fabrication d'un composant en alliage métallique comportant une phase amorphe Download PDF

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Publication number
EP2944401B1
EP2944401B1 EP14168461.3A EP14168461A EP2944401B1 EP 2944401 B1 EP2944401 B1 EP 2944401B1 EP 14168461 A EP14168461 A EP 14168461A EP 2944401 B1 EP2944401 B1 EP 2944401B1
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EP
European Patent Office
Prior art keywords
powder
component
temperature
amorphous
produced
Prior art date
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EP14168461.3A
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German (de)
English (en)
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EP2944401A1 (fr
Inventor
Jürgen Wachter
Alexander Elsen
Annette Lukas
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
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Heraeus Deutschland GmbH and Co KG
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Priority to PL14168461T priority Critical patent/PL2944401T3/pl
Application filed by Heraeus Deutschland GmbH and Co KG filed Critical Heraeus Deutschland GmbH and Co KG
Priority to ES14168461T priority patent/ES2727507T3/es
Priority to EP14168461.3A priority patent/EP2944401B1/fr
Priority to CN201580027018.3A priority patent/CN106413948B/zh
Priority to KR1020167031362A priority patent/KR20160143798A/ko
Priority to JP2016567346A priority patent/JP6370925B2/ja
Priority to US15/310,263 priority patent/US20170151609A1/en
Priority to PCT/EP2015/060410 priority patent/WO2015173211A1/fr
Priority to TW104115379A priority patent/TWI557242B/zh
Publication of EP2944401A1 publication Critical patent/EP2944401A1/fr
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/006—Amorphous articles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/08—Metallic powder characterised by particles having an amorphous microstructure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/14—Both compacting and sintering simultaneously
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/14—Both compacting and sintering simultaneously
    • B22F3/15—Hot isostatic pressing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/16—Both compacting and sintering in successive or repeated steps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/002—Making metallic powder or suspensions thereof amorphous or microcrystalline
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • 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
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/045—Alloys based on refractory metals
    • C22C1/0458—Alloys based on titanium, zirconium or hafnium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C45/00—Amorphous alloys
    • C22C45/10—Amorphous alloys with molybdenum, tungsten, niobium, tantalum, titanium, or zirconium or Hf as the major constituent
    • 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
    • C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
    • 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
    • C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • C22F1/18—High-melting or refractory metals or alloys based thereon
    • C22F1/186—High-melting or refractory metals or alloys based thereon of zirconium or alloys based thereon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • B22F2003/248—Thermal after-treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/20—Refractory metals
    • B22F2301/205—Titanium, zirconium or hafnium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D2201/00—Treatment for obtaining particular effects
    • C21D2201/03—Amorphous or microcrystalline structure
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C2200/00—Crystalline structure
    • C22C2200/02—Amorphous

Definitions

  • the invention relates to a method for producing a component from an at least partially amorphous metal alloy.
  • the invention further relates to a component made of a metal alloy with amorphous phase and the use of such a component.
  • Amorphous metals and their alloys have been known for several decades. Thin tapes and their manufacture are disclosed, for example, in the disclosure DE 35 24 018 A1 described, wherein on a support by quench cooling from the molten phase, a thin metallic glass is produced. Also, for example, in the patent EP 2 430 205 B1 described a composite of an amorphous alloy, which requires a cooling rate of 102 K / s for its production. The disadvantage of this is that with such known methods only thin layers or very compact components can be constructed with a few millimeters in cross-section.
  • EP 1 593 749 A1 describes a metallic glass of an iron alloy containing 0.5-10 at% Ga, 7-15 at% P, 3-7 at% C, 3-7 at% B and 1-7 at% Si as Contains alloying elements and is present in the form of spherical particles.
  • the spherical ones Metal particles are available via gas atomization and are used for the production of a sintered body.
  • the object of the invention is therefore to overcome the disadvantages of the prior art.
  • a simple and inexpensive to implement method is to be developed with which a component can be made of a metal alloy with amorphous portion, which may have a volume of 0.1 cm 3 and more, preferably 1 cm 3 and more, and in different Even complex shapes can be generated.
  • the component produced should also have the highest possible homogeneity with regard to the physical properties and the distribution of the amorphous phase.
  • Object of the present invention is also to provide such a component.
  • the process should be easy to implement and deliver highly reproducible results.
  • the component produced should have the highest possible proportion of amorphous metallic phase. It is also desirable if the component produced is as compact as possible and has only a few pores.
  • Another object can be seen that the method can be implemented with the largest possible number of different alloys having an amorphous phase. Furthermore, it is advantageous if the method can be implemented with the simplest and most commonly used in laboratories equipment and tools.
  • the duration of the temperature treatment is chosen such that the duration is at least so long that the powder is sintered after the temperature treatment, and that the duration is at most so long that the component still has an amorphous content of at least 85 percent after the temperature treatment.
  • an amorphous material is a substance in which the atoms do not form ordered structures but form an irregular pattern and have only short-range order, but not long-range ordering. In contrast to amorphous, regularly structured materials are called crystalline.
  • Spherical particles need not be geometrically perfect spheres within the meaning of the present invention, but may also deviate from the spherical shape.
  • the spherical powder particles have a rounded at least approximately spherical shape and have a ratio of the longest cross section to the shortest cross section of at most 2 to 1.
  • a spherical geometry does not mean a strictly geometrical or mathematical sphere.
  • the cross-sections relate to running within the powder particles extremale dimensions.
  • Particularly preferred spherical powder particles may have a ratio of the longest cross section to the shortest cross section of at most 1.5 to 1, or most preferably spherical. In this case, the diameter of the largest cross-section of the powder particles is assumed according to the invention.
  • Temperature treatment under the same conditions soft - or at least under soft approximate the same conditions soft.
  • they combine or sinter these particularly well and within a short period of time, or at a known time or in a known time interval, with adjacent powder particles.
  • Another advantage of high bulk density is low shrinkage of the component during sintering. As a result, production close to the final shape is possible.
  • the component may, in accordance with a preferred embodiment of the present invention, be considered to be sintered in particular if it has a density of at least 97% of the theoretical density of the completely amorphous metal alloy.
  • sintering or sintering is understood as meaning a process in which the powder particles soften on the surface and combine with one another and remain connected after cooling. As a result, a coherent body or a coherent component is generated from the powder.
  • the transformation temperature of an amorphous phase is often referred to as the glass transition temperature or as a transformation point or glass transition point, it being understood that these are equivalent terms for the transformation temperature.
  • the powder is formed by filling the powder into a mold or into a tool and then pressing the powder in the mold or in the tool or by pressing it with the tool.
  • the heating until reaching the transformation temperature and the cooling should be carried out according to the invention as quickly as possible, since even at these temperatures below the transformation temperature crystallization takes place on the inevitable seed crystals, but still no softening of the powder particles is achieved, leading to sintering of the powder could lead. It is to be achieved according to the invention a plastic deformation of the powder particles, which leads to a compacting of the powder and thus to an accelerated sintering of the powder. An overshoot of the temperature above the desired setpoint temperature or final temperature should be as low as possible.
  • the powder particle size of the powder or the powder particle size distribution of the powder can be achieved by the manufacturing process and by sieving a starting powder.
  • the powder provided according to the invention is thus produced by sieving a starting powder before it is provided or used for the process according to the invention.
  • by sieving it can also be ensured that the number of powder particles having a shape which differs greatly from the spherical shape, which are produced by sintering several powder particles and which are contained in the starting powder, can be reduced or minimized.
  • the temperature treatment is carried out under vacuum, wherein preferably the powder is compacted by a temperature treatment at a vacuum of at least 10 -3 mbar.
  • metal oxides and other reaction products as nucleating agents for crystalline phases, have a negative effect on the purity of the amorphous phase in the produced component.
  • the invention may additionally or alternatively be provided that the temperature treatment is carried out under a protective gas, in particular under a noble gas such as argon, preferably with a purity of at least 99.99%, more preferably with a purity of at least 99.999 % he follows. It may preferably be provided in such embodiments that the atmosphere in which the pressing and the temperature treatment or only the temperature treatment takes place is largely freed of residual gases by repeated evacuation and rinsing with inert gas, in particular with argon.
  • a protective gas in particular under a noble gas such as argon
  • the temperature treatment takes place under a reducing gas, in particular under a forming gas, in order to keep the amount of interfering metal oxides as low as possible.
  • Another measure for reducing the number of metal oxides in the component can be achieved by the use of an oxygen getter in the temperature treatment of the powder and / or in the production of the powder.
  • the powder is compacted by hot isostatic pressing or hot pressing.
  • the combination of pressure and temperature treatment results in a more compact component.
  • the compound is improved by the plastic deformation of the powder particles with each other and accelerates the sintering behavior, so that a shorter duration of the temperature treatment can be selected and the proportion of crystalline phase is reduced in the component.
  • the duration of the temperature treatment is selected such that the component has an amorphous content of at least 90 percent, preferably of more than 95 percent, particularly preferably more than 98 percent.
  • Preferred embodiments of the present invention may also provide that a powder of an amorphous metal alloy or an at least partially amorphous metal alloy having at least 50 weight percent zirconium is used.
  • Zirconium-containing amorphous metal alloys are particularly well suited for practicing methods of the present invention because many of these alloys have a large difference between the transformation temperature and the crystallization temperature, making the process easier to implement.
  • zirconium The remainder up to 100 percent by weight is zirconium. Common contaminants may be included in the alloy. These zirconium-containing amorphous metal alloys are particularly well suited for implementing inventive methods.
  • the spherical amorphous metal alloy powder is produced by melt atomization, preferably by melt atomization in a noble gas, in particular in argon, particularly preferably by melt atomization in a noble gas of purity 99.99%, 99.999% or higher purity.
  • an amorphous metal alloy is also used if the metal alloy has an amorphous phase content of at least 85% by volume.
  • melt atomization powder particles can be produced with spherical shape in a simple and cost-effective manner.
  • inert gas, in particular of argon or high-purity argon in the melt atomization causes that in the powder as few disturbing impurities as metal oxides are included.
  • the powder has less than 1 weight percent of particles less than 5 microns in diameter, or the powder is screened or air-treated so that it has less than 1 weight percent of particles less than 5 microns in diameter.
  • powder particles with a diameter of less than 5 ⁇ m are preferably removed by air classification, or more precisely, the proportion of powder particles with a diameter of less than 5 ⁇ m is reduced by air classification.
  • the temperature treatment of the powder takes place at a temperature (T) between the transformation temperature and a maximum temperature, the maximum temperature being 30% higher than the temperature difference between the transformation temperature (T T ) and the crystallization temperature (T K ) of the amorphous phase of the metallic alloy is above the transformation temperature (T T ), the maximum temperature preferably being 20% or 10% of the temperature difference between the transformation temperature (T T ) and the crystallization temperature (T K ) the amorphous phase of the metallic alloy is above the transformation temperature (T T ).
  • the temperature T at which the temperature treatment of the powder takes place should fulfill the following conditions: T T ⁇ T ⁇ T T + 300 / 100 * T K - T T or preferred T T ⁇ T ⁇ T T + 20 / 100 * T K - T T or more preferably T T ⁇ T ⁇ T T + 10 / 100 * T K - T T ,
  • a particularly advantageous embodiment of the method according to the invention results if it is provided that the duration of the temperature treatment is selected as a function of the geometric shape, in particular the thickness, of the component to be produced, preferably as a function of the largest relevant diameter of the component to be produced ,
  • the geometric shape, or the thickness, of the component to be produced is taken into account in that the heat conduction in the molded powder or molding component should be sufficient to also the powder inside the component or the component inside up to the transformation temperature or above Heat transformation temperature, so that also takes place inside the component sintering of the powder.
  • the largest relevant diameter of the component can be geometrically determined by the largest sphere that can be geometrically accommodated within the component.
  • the duration of the heat treatment in a time range of 3 seconds per millimeter of the thickness or the wall thickness of the component or the largest relevant diameter of the component to be produced to 900 seconds per millimeter of thickness or the largest relevant diameter of the Component takes place, wherein preferably the duration of the temperature treatment in a time range of 5 seconds per millimeter of the thickness or the wall thickness of the component or the largest relevant diameter of the component to be produced to 600 seconds per millimeter of thickness or the largest relevant diameter of the component to be produced he follows.
  • the duration of the temperature treatment is selected so that sufficient sintering of the powder occurs, but at the same time as possible the formation of crystalline phase in the component is kept low or ideally minimal.
  • it may already be sufficient if only the edge regions of the component are completely sintered and powder that is not yet sintered is present in the interior of the component.
  • the component is sintered completely (also inside).
  • the objects underlying the present invention are also achieved by a component made of a pressed, sintered, spherical, amorphous Metal alloy powder, wherein the component has an amorphous content of at least 85 percent.
  • the component is produced by the method according to the invention.
  • the method according to the invention has been described above.
  • the invention is based on the surprising finding that by using spherical powder particles of suitable size and a temperature treatment at the suitable temperature over a suitable short period, it is also possible to produce larger and / or complex components from a powder of an amorphous metal alloy consist of a high proportion (at least 85 percent by volume) of the amorphous phase and thus have advantageous physical properties of the amorphous metal alloy.
  • the present invention thus describes for the first time a method in which a component of an amorphous metal alloy or of a metal alloy consisting of at least 85% of an amorphous phase can be produced by sintering a powder in which a high proportion of amorphous phase is retained.
  • the duration of the temperature treatment is adapted to the dimensions of the component to be produced in order to obtain the highest possible proportion of amorphous phase during sintering of the powder, or to keep the proportion of crystalline phase in the metal alloy as low as possible.
  • metal oxides and other reaction products act in particular as nuclei for the crystallization and thus reduce the proportion of amorphous phase in the component.
  • amorphous metallic powders for producing the component are produced by melt atomization and the powders are X-ray amorphous, with their powder particles preferably being smaller than 125 ⁇ m.
  • the resulting molten Droplets of the alloy cooled very rapidly through the process gas stream (argon), thereby promoting the presence of an amorphous powder fraction. From this powder, the fine dust (particles smaller than 5 microns) and the coarse grain of greater than 125 microns largely separated, for example by sieving and / or by air classification of the powder.
  • Such powder fractions are then an optimum starting material (the powder provided) to produce complex amorphous components by pressing and temperature treatment, both successive or combined pressure and temperature steps having very good results with respect to the amorphous behavior of the component.
  • the powder provided an optimum starting material
  • the powder provided to produce complex amorphous components by pressing and temperature treatment, both successive or combined pressure and temperature steps having very good results with respect to the amorphous behavior of the component.
  • the component thus produced and made of such a powder has a high degree of sintered powder particles and a low porosity, preferably a porosity of less than 5%.
  • the amorphous powder is not heated to the crystallization temperature or beyond, otherwise crystallization occurs and the amorphous character of the alloy is lost.
  • it is necessary to heat the material at least to the transformation temperature ie the temperature at which the amorphous phase of the metal alloy during the cooling from the plastic region in the rigid state passes. In this temperature range, the powder particles can connect, but without crystallizing.
  • the transformation temperature can also be referred to as the glass transition temperature and is often referred to as such.
  • the duration of the temperature treatment depends mainly on the volume of the component and should not take too long, as a rule, since each small crystal nucleus acts as a seed crystal and so crystals can grow, or so spreads the unwanted crystalline phase in the component.
  • a temperature treatment in the temperature range according to the invention with a maximum duration of 400 seconds per 1 mm component cross-section gives particularly good results.
  • the heating-up phase should also take place as quickly as possible since, in some cases, the undesired crystal growth already occurs 50 Kelvin below the transformation temperature.
  • T is the working temperature
  • T T is the transformation temperature of the amorphous metal alloy
  • T K is the crystallization temperature of the amorphous phase of the metal alloy.
  • an amorphous metallic powder is produced from a metallic alloy whose composition is suitable for forming an amorphous phase or which already consists of the amorphous phase. This is followed by a powder fractionation in which too small and too large powder particles or powder particles, in particular by sieving and air classification, are removed. The powder can then be pressed either with or without temperature entry in a desired shape. When the powder is pressed into the mold without the introduction of temperature, a temperature treatment is subsequently carried out, which in the context of the present invention is referred to as sintering or which causes sintering. The temperature treatment during pressing or after pressing takes place for a maximum period of 900 seconds per 1 mm component cross-section at a temperature above the transformation temperature T T and below the crystallization temperature T K of the amorphous phase of the metallic alloy used.
  • Niobium Film 99.97% Article Number 002378 was heated in an induction melting plant (VSG, inductively heated vacuum, melting and casting plant, Nürmont, Freiberg) under 800 mbar argon (argon 6.0, Linde AG, Pullach) melted and poured into a water-cooled copper mold. From the thus produced alloy was prepared by a method such as WO 99/30858 A1 is known, produced in a Nanoval Schmelzverdüsungs apparatus (Nanoval GmbH & Co. KG, Berlin) by atomizing the melt with argon, a fine powder.
  • the fine grain is separated, so that less than 0.1% of the particles are smaller than 5 microns in size, that is at least 99.9% of the particles one Diameter or a dimension of 5 microns or more, and by sieving through a test sieve with 125 microns mesh size (Retsch GmbH, Haan Germany, Article No. 60.131.000125) are removed all powder particles that are larger than 125 microns.
  • the powder thus produced is examined by means of X-ray diffractometry and has an amorphous content greater than 95%.
  • the compacted compacts are finally compacted by hot isostatic pressing under a pressure of 200 megapascal (200 MPa) under high-purity argon (Argon 6.0, Linde AG, Pullach) at a temperature of 400 ° C for 90 seconds.
  • Niobium Film 99.97% Article Number 002378 was heated in an induction melting plant (VSG, inductively heated vacuum, melting and casting plant, Nürmont, Freiberg) under 800 mbar argon (argon 6.0, Linde AG, Pullach) melted and poured into a water-cooled copper mold. From the thus produced alloy was prepared by a method such as WO 99/30858 A1 is known, produced in a Nanoval Schmelzverdüsungs apparatus (Nanoval GmbH & Co. KG, Berlin) by atomizing the melt with argon, a fine powder.
  • the fine grain was separated by separation by means of air classification Condux-Feinstsichter CFS (Netsch-Feinmahltechnik GmbH Selb Germany), so that less than 0.1% of the particles are smaller than 5 microns in size and by sieving through a test sieve with 125 microns mesh size (Retsch GmbH , Haan Germany, article number 60.131.000125), all powder particles larger than 125 ⁇ m were away.
  • the powder thus produced was examined by means of X-ray diffractometry and has an amorphous content greater than 95%.
  • niobium film 99.97% article number 002378 was used in an induction melting plant (VSG, inductively heated vacuum, melting and casting plant, Nürmont, Freiberg) under 800 mbar argon (argon 6.0, Linde AG, Pullach) melted and poured into a water-cooled copper mold. From the thus produced alloy was prepared by a method such as WO 99/30858 A1 is known, produced in a Nanoval Schmelzverdüsungs apparatus (Nanoval GmbH & Co. KG, Berlin) by atomizing the melt with argon, a fine powder.
  • the fine grain was separated by separation by means of air classification Condux-Feinstsichter CFS (Netsch-Feinmahltechnik GmbH Selb Germany), so that less than 0.1% of the particles are smaller than 5 microns in size and by sieving through a test sieve with 125 microns mesh size (Retsch GmbH , Haan Germany, article number 60.131.000125), all powder particles larger than 125 ⁇ m were removed.
  • the powder thus produced was examined by X-ray diffractometry and has an amorphous content greater than 95%.
  • niobium film 99.97% article number 002378 was used in an induction melting plant (VSG, inductively heated vacuum, melting and casting plant, Nürmont, Freiberg) under 800 mbar argon (argon 6.0, Linde AG, Pullach) melted and poured into a water-cooled copper mold. From the thus produced alloy was prepared by a method such as WO 99/30858 A1 is known, produced in a Nanoval Schmelzverdüsungs apparatus (Nanoval GmbH & Co. KG, Berlin) by atomizing the melt with argon, a fine powder.
  • the fine grain was separated by separation by means of air classification Condux-Feinstsichter CFS (Netsch-Feinmahltechnik GmbH Selb Germany), so that less than 0.1% of the particles are smaller than 5 microns in size and by sieving through a test sieve with 125 microns mesh size (Retsch GmbH , Haan Germany, article number 60.131.000125), all powder particles larger than 125 ⁇ m were removed.
  • the powder thus produced was examined by means of X-ray diffractometry and has an amorphous content greater than 95%.
  • the component produced in this way was examined by means of several metallographic micrographs for the amorphous area fraction in the microstructure. This shows that on average 90% of the surfaces are amorphous.
  • the particle size of inorganic powders was determined by laser light scattering with a Mastersizer 2000 (Malvern Instruments Ltd., Great Britain).
  • a geometrically exact cuboid can be created by grinding the surfaces so that it can be precisely measured with a digital micrometer (PR1367, Mitutoyo Messtechnik Leonberg GmbH, Leonberg).
  • PR1367 Mitutoyo Messtechnik Leonberg GmbH, Leonberg.
  • the volume is determined and then the exact weight is determined on an analytical balance (XPE analytical balances from Mettler-Toledo GmbH).
  • XPE analytical balances from Mettler-Toledo GmbH
  • the theoretical density of an amorphous alloy corresponds to the density at the melting point.

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Claims (13)

  1. Procédé de fabrication d'un composant à partir d'un alliage métallique au moins partiellement amorphe, comprenant les étapes suivantes :
    la mise à disposition d'une poudre à partir d'un alliage métallique au moins partiellement amorphe, la poudre étant constituée par des particules de poudre sphériques, les particules de poudre sphériques présentant une forme arrondie au moins approximativement sphérique et ayant un rapport entre la section transversale la plus longue et la section transversale la plus courte d'au plus 2 sur 1, et la section transversale la plus grande des particules de poudre étant adoptée en tant que diamètre, et les particules de poudre présentant un diamètre inférieur à 125 µm, et la poudre comprenant moins de 1 pour cent en poids de particules d'un diamètre inférieur à 5 µm, ou la poudre étant tamisée ou traitée par criblage à l'air de telle sorte qu'elle comprenne moins de 1 pour cent en poids de particules d'un diamètre inférieur à 5 µm ;
    la compression de la poudre sous la forme souhaitée du composant à produire ;
    le compactage et le frittage de la poudre par un traitement thermique de la poudre pendant la compression ou après la compression à une température qui se situe entre la température de transformation et la température de cristallisation de la phase amorphe de l'alliage métallique, la durée du traitement thermique étant choisie de telle sorte que le composant soit fritté après le traitement thermique et présente une proportion amorphe d'au moins 85 pour cent.
  2. Procédé selon la revendication 1, caractérisé en ce que le traitement thermique a lieu sous vide, la poudre étant de préférence compactée par un traitement thermique sous un vide d'au moins 10-3 mbar.
  3. Procédé selon la revendication 1 ou 2, caractérisé en ce que la poudre est compactée par compression isostatique à chaud ou compression à chaud.
  4. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que la durée du traitement thermique est choisie de telle sorte que le composant présente une proportion amorphe d'au moins 90 pour cent, de préférence de plus de 95 pour cent, de manière particulièrement préférée de plus de 98 pour cent.
  5. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce qu'une poudre d'un alliage métallique amorphe contenant au moins 50 pour cent en poids de zirconium est utilisée.
  6. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce qu'une poudre d'un alliage métallique amorphe constitué par :
    a) 58 à 77 pour cent en poids de zirconium,
    b) 0 à 3 pour cent en poids d'hafnium,
    c) 20 à 30 pour cent en poids de cuivre,
    d) 2 à 6 pour cent en poids d'aluminium et
    e) 1 à 3 pour cent en poids de niobium,
    est préparée.
  7. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que la poudre d'alliage métallique amorphe sphérique est fabriquée par pulvérisation à l'état fondu, de préférence par pulvérisation à l'état fondu dans un gaz noble, notamment dans de l'argon, de manière particulièrement préférée par pulvérisation à l'état fondu dans un gaz noble d'une pureté de 99,99 %, 99,999 % ou d'une pureté supérieure.
  8. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que le traitement thermique de la poudre a lieu à une température (T) comprise entre la température de transformation et une température maximale, la température maximale étant située 30 % de la différence de température entre la température de transformation (TT) et la température de cristallisation (TK) de la phase amorphe de l'alliage métallique au-dessus de la température de transformation (TT), la température maximale étant de préférence située 20 % ou 10 % de la différence de température entre la température de transformation (TT) et la température de cristallisation (TK) de la phase amorphe de l'alliage métallique au-dessus de la température de transformation (TT).
  9. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que la durée du traitement thermique est choisie en fonction de la forme géométrique, notamment de l'épaisseur, du composant à produire, de préférence en fonction du diamètre pertinent le plus grand du composant à produire.
  10. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que la durée du traitement thermique est dans une plage temporelle de 3 secondes par millimètre d'épaisseur ou de diamètre pertinent le plus grand du composant à produire à 900 secondes par millimètre d'épaisseur ou de diamètre pertinent le plus grand du composant à produire, la durée du traitement thermique étant de préférence dans une plage temporelle de 5 secondes par millimètre d'épaisseur ou de diamètre pertinent le plus grand du composant à produire à 600 secondes par millimètre d'épaisseur ou de diamètre pertinent le plus grand du composant à produire.
  11. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que les particules de poudre sont déformées plastiquement par le traitement thermique.
  12. Composant en une poudre d'alliage métallique amorphe, sphérique, frittée, comprimée, le composant présentant une proportion amorphe d'au moins 85 pour cent et étant fabriqué par un procédé selon l'une quelconque des revendications 1 à 11.
  13. Utilisation d'un composant selon la revendication 12 pour la fabrication d'une roue dentée, d'une roue de friction, d'un composant résistant à l'usure, d'un boîtier, d'un boîtier d'horloge, d'une partie d'une transmission ou d'un produit semi-fini.
EP14168461.3A 2014-05-15 2014-05-15 Procédé de fabrication d'un composant en alliage métallique comportant une phase amorphe Active EP2944401B1 (fr)

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Application Number Priority Date Filing Date Title
ES14168461T ES2727507T3 (es) 2014-05-15 2014-05-15 Procedimiento para la producción de un componente a partir de una aleación metálica con fase amorfa
EP14168461.3A EP2944401B1 (fr) 2014-05-15 2014-05-15 Procédé de fabrication d'un composant en alliage métallique comportant une phase amorphe
PL14168461T PL2944401T3 (pl) 2014-05-15 2014-05-15 Sposób wytwarzania elementu konstrukcyjnego ze stopu metali zawierającego fazę amorficzną
KR1020167031362A KR20160143798A (ko) 2014-05-15 2015-05-12 비정질상 금속 합금으로부터 부품을 제조하기 위한 방법
CN201580027018.3A CN106413948B (zh) 2014-05-15 2015-05-12 用于由非晶相金属合金制造构件的方法
JP2016567346A JP6370925B2 (ja) 2014-05-15 2015-05-12 非晶質相を有する金属合金からなる部品の製造方法
US15/310,263 US20170151609A1 (en) 2014-05-15 2015-05-12 Method for producing a component from an amorphous-phase metal alloy
PCT/EP2015/060410 WO2015173211A1 (fr) 2014-05-15 2015-05-12 Procédé de production d'un élément à partir d'un alliage métallique comprenant une phase amorphe
TW104115379A TWI557242B (zh) 2014-05-15 2015-05-14 製造非晶相金屬合金組件之方法

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CN106413948A (zh) 2017-02-15
CN106413948B (zh) 2019-08-02
US20170151609A1 (en) 2017-06-01
TW201610187A (zh) 2016-03-16
EP2944401A1 (fr) 2015-11-18
ES2727507T3 (es) 2019-10-16
KR20160143798A (ko) 2016-12-14
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JP6370925B2 (ja) 2018-08-08
JP2017520677A (ja) 2017-07-27
TWI557242B (zh) 2016-11-11

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