WO2015173211A1 - Verfahren zur herstellung eines bauteils aus einer metalllegierung mit amorpher phase - Google Patents
Verfahren zur herstellung eines bauteils aus einer metalllegierung mit amorpher phase Download PDFInfo
- Publication number
- WO2015173211A1 WO2015173211A1 PCT/EP2015/060410 EP2015060410W WO2015173211A1 WO 2015173211 A1 WO2015173211 A1 WO 2015173211A1 EP 2015060410 W EP2015060410 W EP 2015060410W WO 2015173211 A1 WO2015173211 A1 WO 2015173211A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- powder
- component
- temperature
- amorphous
- metal alloy
- Prior art date
Links
Classifications
-
- 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 strips and their preparation are described, for example, in the disclosure DE 35 24 018 A1, wherein a thin metallic glass is produced on a support by quench cooling from the melt phase. Also, for example, EP 2 430 205 B1 describes 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.
- WO 2008/039134 A1 discloses a method in which a larger component is produced from an amorphous metal powder. For this purpose, the component is built up in layers in the manner of a 3D printing, wherein partial areas of the layers are melted with an electron beam.
- the disadvantage of this is that the method is very expensive and expensive to implement. In addition, with such a method, it is not possible to achieve sufficient homogeneity of the physical properties of the component produced.
- the local melting and again cooling of the powder leads to a punctual exceeding of the crystallization temperature and a crystallization of the alloy if the cooling rate of the melt is too low. Specifically, it may be due to the heat input during local melting and again cooling of the near-surface powder to a punctual exceeding the crystallization temperature in deeper already amorphous solidified layers and crystallization of the alloy come. This creates an undesirable amount and an uneven distribution of crystalline phase in the component.
- 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.
- 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 objects of the invention are achieved by a method for producing a component from an at least partially amorphous metal alloy with the steps:
- the duration of the temperature treatment is selected so that the component after the heat treatment is sintered and has an amorphous content of at least 85 percent.
- the duration of the temperature treatment is selected such that the duration is at least as long that the powder is sintered after the temperature treatment, and that the duration is at most so long that the component after the temperature treatment still has an amorphous content of at least 85 percent ,
- the powder consists of powder particles of which 100% less than 125 ⁇ diameter.
- 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.
- Preferred 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 strictly geometrical or mathematical sphere is not meant by a spherical geometry.
- 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.
- the spherical particles form a flowable powder, which is particularly helpful in the layered processing on powder tanks and squeegee;
- the powder particles have similar curved surfaces, which soften in the temperature treatment under the same conditions (temperature and time or the same heat energy input) - or at least be softened to a good approximation the same conditions. As a result, 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 through the manufacturing process and be achieved 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. Unless the starting powder already has the desired properties after the manufacturing process.
- sieving can also be used to ensure that the number of powder particles having a shape that differs greatly from the spherical shape and that results from the sintering of several powder particles (so-called satellite formation) and that is 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 can be achieved.
- 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.
- Very particularly preferred embodiments of the present invention may provide that a powder of an amorphous metal alloy or an at least partially amorphous metal alloy
- 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 less than 1 weight percent of particles having a diameter smaller than 5 ⁇ or the powder is sieved or treated by air classification, so that it is less than 1 percent by weight of particles with a diameter has less than 5 ⁇ .
- powder particles having a diameter of less than 5 ⁇ m are preferably removed by air classification, or more precisely, the proportion of powder particles having 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 based on the transformation temperature T T and the crystallization temperature T K of the amorphous phase of the metallic alloy, should fulfill the following conditions:
- 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 forming component is sufficient to also the powder inside the component or the component in the interior 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. When determining the largest relevant diameter, it is possible to disregard channels or gaps in the body which do not or only slightly contribute to the heat input via a surrounding gas and / or another heat source (for example in the sum of less than 5%).
- 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 a sufficient sintering the powder takes place, but at the same time the formation of crystalline phase is kept as low as possible in the component or ideally is 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 a method according to the invention. Such methods according to the invention have 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, preferably their powder particles being smaller than 125 ⁇ m.
- the resulting molten droplets of the alloy are cooled very rapidly by the process gas stream (argon), thereby promoting the presence of an amorphous powder fraction.
- the process gas stream argon
- this powder of fine dust (particles smaller than 5 ⁇ ) and the coarse grain of greater than 125 ⁇ largely separated, for example by screening and / or by air classification of the powder is removed.
- 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 With powders produced in this way, a component with a particularly high proportion of amorphous metallic phase is obtained.
- 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 upper limit of the particle size avoids that particles which have a larger cross-section than the layers produced, these could then be removed with a doctor and thus the layer would be incomplete.
- 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 crystallize.
- 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 crystallites 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.
- Niob film 99.97% article number 002378 was 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) and melted into a water cooled Cast copper mold. From the alloy thus produced, a fine powder was produced by atomizing the melt with argon by a method known from WO 99/30858 A1, for example, in a Nanoval melt atomization apparatus (Nanoval GmbH & Co. KG, Berlin).
- the fine grain is separated, so that less than 0.1% of the particles smaller than 5 ⁇ are large, that is at least 99.9% of the particles one Have diameter or a size of 5 ⁇ or more, and by sieving through a test sieve with 125 ⁇ mesh size (Retsch GmbH, Haan Germany, Article No. 60.131 .000125) all powder particles are removed, which are greater than 125 ⁇ .
- the powder thus produced is examined by means of X-ray diffractometry and has an amorphous content greater than 95%.
- Niob film 99.97% Article number 002378 was melted 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) and poured into a water-cooled copper mold. From the alloy produced in this way, a fine powder was produced by atomizing the melt with argon by a method known from WO 99/30858 A1, for example, in a Nanoval melt atomization apparatus (Nanoval GmbH & Co. KG, Berlin).
- 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 alloy produced in this way, a fine powder was produced by atomizing the melt with argon by a method known from WO 99/30858 A1, for example, in a Nanoval melt atomization apparatus (Nanoval GmbH & Co. KG, Berlin).
- 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.
- VSG inductively heated vacuum, melting and casting plant
- argon argon 6.0, Linde AG, Pullach
- the alloy produced in this way was produced by a method, as known, for example, from WO 99/30858 A1, in a Nanoval melt atomization apparatus (Nanoval GmbH & Co. KG, Berlin) produces a fine powder by atomizing the melt with argon.
- 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 Sympatec Helos BR / R3 (Sympatec GmbH) equipped with a RODOS / M dry dispersing system with vibrating feeder VIBRI (Sympatec GmbH). Sample quantities of at least 10 g were applied dry, dispersed at a primary pressure of 1 bar and the measurement started. The starting criterion was an optical concentration of 1, 9% to 2.1%. The measuring time was 10 seconds. The evaluation was done according to the MIE theory and the d50 was used as a measure of the particle size.
- 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 now determined.
- the exact weight is determined on an analytical balance (XPE analytical balances from Mettler-Toledo GmbH). By forming the ratio of weighed weight and calculated volume, the density is obtained.
- the theoretical density of an amorphous alloy corresponds to the density at the melting point.
- each fifteen metallographic sections are made on the basis of DIN EN ISO 1463, wherein with a SiC foil 1200 (Struers GmbH, Willich) and then following polishing steps with diamond polish with 6 ⁇ , 3 ⁇ and 1 ⁇ (Struers GmbH, Willich) and finally polished with the chemo-mechanical oxide polishing suspensions OP-S (Struers GmbH, Willich).
- the ground surfaces thus obtained are examined under a light microscope (Leica DM 4000 M, Leica DM 6000 M) with a magnification of 1000 on crystalline surface portions in the micrograph.
- Leica Phase Expert software an evaluation is carried out by area percent crystalline fraction to total area of the cut, the dark areas being considered crystalline and the light areas being amorphous were.
- the amorphous matrix is defined as the reference phase and expressed as a percentage of the total measurement area.
- Each 10 different sample surfaces were measured and averaged.
- a calorimeter Netzsch DSC 404 F1 Pegasus (Erich NETZSCH GmbH & Co. KG) equipped with a high-temperature tube furnace with Rh meander heater, an integrated control thermocouple type S, DSC404F1 A72 sample support system, crucible made of AI 2 O 3 with lid was used , an OTS system for the removal of traces of oxygen during the measurement, including three getter rings and an evacuation system for automatic operation with a two-stage rotary pump. All measurements were carried out under protective gas (argon 6.0, Linde AG) at a flow rate of 50 ml / min. The evaluation took place by means of the software Proteus 6.1.
- the tangent method (“Glass Transition") was used in the range between 380 ° C and 420 ° C (Onset, Mid, Inflection, End)
- TK the "Complex Peak” evaluation in the temperature range 450- 500 ° C (Area, Peak, Onset, End, Width, Height) and for Tm the "Complex Peak” evaluation in the temperature range 875-930 ° C (Area, Peak, Onset, End, Width, Height)
- the measurement was carried out by weighing 25 mg +/- 0.5 mg sample into the crucible and measuring at the following heating rates and temperature ranges: 20-375 ° C: heating rate 20 K / min
- the enthalpy of crystallization was determined using the "complex peak" method, using a 100% amorphous sample (obtained by melt spinning) with a crystallization enthalpy of -47.0 J / g as reference Crystallization enthalpy of the component to crystallization enthalpy of the reference gives the proportion of the amorphous phase.
- the parameters of the ICP device were:
- Plasma gas 15.0 l / min (argon)
- Atomizing gas pressure 220 kPa (argon)
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
Description
Claims
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
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 |
US15/310,263 US20170151609A1 (en) | 2014-05-15 | 2015-05-12 | Method for producing a component from an amorphous-phase metal alloy |
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 |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP14168461.3A EP2944401B1 (de) | 2014-05-15 | 2014-05-15 | Verfahren zur Herstellung eines Bauteils aus einer Metalllegierung mit amorpher Phase |
EP14168461.3 | 2014-05-15 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2015173211A1 true WO2015173211A1 (de) | 2015-11-19 |
Family
ID=50771069
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/EP2015/060410 WO2015173211A1 (de) | 2014-05-15 | 2015-05-12 | Verfahren zur herstellung eines bauteils aus einer metalllegierung mit amorpher phase |
Country Status (9)
Country | Link |
---|---|
US (1) | US20170151609A1 (de) |
EP (1) | EP2944401B1 (de) |
JP (1) | JP6370925B2 (de) |
KR (1) | KR20160143798A (de) |
CN (1) | CN106413948B (de) |
ES (1) | ES2727507T3 (de) |
PL (1) | PL2944401T3 (de) |
TW (1) | TWI557242B (de) |
WO (1) | WO2015173211A1 (de) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE102018115815A1 (de) * | 2018-06-29 | 2020-01-02 | Universität des Saarlandes | Vorrichtung und Verfahren zur Herstellung eines aus einem amorphen oder teilamorphen Metall gebildeten Gussteils sowie Gussteil |
Families Citing this family (19)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US10987735B2 (en) | 2015-12-16 | 2021-04-27 | 6K Inc. | Spheroidal titanium metallic powders with custom microstructures |
PL3389862T3 (pl) | 2015-12-16 | 2024-03-04 | 6K Inc. | Sferoidalne metale podlegające odwodornieniu oraz cząstki stopów metali |
GB201609141D0 (en) * | 2016-05-24 | 2016-07-06 | Metalysis Ltd | Manufacturing apparatus and method |
CN108607998B (zh) * | 2018-05-04 | 2020-09-25 | 西迪技术股份有限公司 | 一种金属烧结摩擦材料及摩擦片 |
AU2019290663B2 (en) | 2018-06-19 | 2023-05-04 | 6K Inc. | Process for producing spheroidized powder from feedstock materials |
WO2020223358A1 (en) | 2019-04-30 | 2020-11-05 | 6K Inc. | Mechanically alloyed powder feedstock |
KR20240036705A (ko) | 2019-04-30 | 2024-03-20 | 6케이 인크. | 리튬 란타넘 지르코늄 산화물(llzo) 분말 |
EP3804885A1 (de) * | 2019-10-11 | 2021-04-14 | Heraeus Additive Manufacturing GmbH | Verfahren zur herstellung eines metallischen bauteils, das einen abschnitt mit hohem aspektverhältnis aufweist |
AU2020400980A1 (en) | 2019-11-18 | 2022-03-31 | 6K Inc. | Unique feedstocks for spherical powders and methods of manufacturing |
US11590568B2 (en) | 2019-12-19 | 2023-02-28 | 6K Inc. | Process for producing spheroidized powder from feedstock materials |
EP3915701A1 (de) * | 2020-05-28 | 2021-12-01 | Heraeus Amloy Technologies GmbH | Simulationssystem zur auswahl einer legierung sowie eines fertigungsverfahrens für ein zu fertigendes werkstück mit amorphen eigenschaften |
CN116034496A (zh) | 2020-06-25 | 2023-04-28 | 6K有限公司 | 微观复合合金结构 |
US11963287B2 (en) | 2020-09-24 | 2024-04-16 | 6K Inc. | Systems, devices, and methods for starting plasma |
CA3196653A1 (en) | 2020-10-30 | 2022-05-05 | Sunil Bhalchandra BADWE | Systems and methods for synthesis of spheroidized metal powders |
SE544674C2 (en) * | 2020-12-11 | 2022-10-11 | Adrian Robert Rennie | A beam path component for use in neutron scattering equipment and method of producing such |
DE102021111186A1 (de) * | 2021-04-30 | 2022-11-03 | Haimer Gmbh | Werkzeugmaschinenkomponente sowie Verfahren zur Herstellung einer solchen Werkzeugmaschinenkomponente |
CN113249661A (zh) * | 2021-06-11 | 2021-08-13 | 北京大学口腔医学院 | 生物医用非晶合金及其应用 |
CN113737111A (zh) * | 2021-09-07 | 2021-12-03 | 东莞市无疆科技投资有限公司 | 一种高密度非晶复合材料及其制备方法 |
CN114284055B (zh) * | 2021-12-28 | 2024-02-23 | 江西大有科技有限公司 | 一种非晶粉及其制备方法 |
Citations (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE3524018A1 (de) | 1985-07-02 | 1987-01-15 | Mannesmann Ag | Verfahren und vorrichtung zum herstellen von metallglas |
US5306463A (en) * | 1990-04-19 | 1994-04-26 | Honda Giken Kogyo Kabushiki Kaisha | Process for producing structural member of amorphous alloy |
WO1999030858A1 (de) | 1997-12-17 | 1999-06-24 | Gunther Schulz | Verfahren und vorrichtung zur herstellung feiner pulver durch zerstäubung von schmelzen mit gasen |
EP1593749A1 (de) * | 2002-12-25 | 2005-11-09 | Japan Science and Technology Corporation | Kugelförmige partikel einer metallischen glaslegierung auf eisenbasis, weichmagnetisches material aus eisenbasierter sinterlegierung in loser form, hergestellt durch sintern desselben, und deren herstellungsverfahren |
EP1813694A1 (de) * | 2004-11-15 | 2007-08-01 | Nikko Materials Co., Ltd. | Sputtertarget zur herstellung eines films aus metallischem glas und herstellungsverfahren dafür |
WO2008039134A1 (en) | 2006-09-26 | 2008-04-03 | Foersvarets Materielverk | Method of producing products of amorphous metal |
US20120247948A1 (en) * | 2009-11-19 | 2012-10-04 | Seung Yong Shin | Sputtering target of multi-component single body and method for preparation thereof, and method for producing multi-component alloy-based nanostructured thin films using same |
EP2597166A1 (de) * | 2011-11-24 | 2013-05-29 | Universität des Saarlandes | Massives metallisches Glas bildende Legierung |
EP2430205B1 (de) | 2009-05-14 | 2014-04-02 | BYD Company Limited | Amorphes legierungsverbundmaterial und verfahren zu seiner herstellung |
Family Cites Families (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6022424A (en) * | 1996-04-09 | 2000-02-08 | Lockheed Martin Idaho Technologies Company | Atomization methods for forming magnet powders |
CN1074466C (zh) * | 1997-02-25 | 2001-11-07 | 中国科学院金属研究所 | 一种块状非晶及纳米晶合金的制备方法 |
JP3852809B2 (ja) * | 1998-10-30 | 2006-12-06 | 独立行政法人科学技術振興機構 | 高強度・高靭性Zr系非晶質合金 |
TW200722532A (en) * | 2005-12-14 | 2007-06-16 | Jin P Chu | Annealing-induced solid-state amorphization in a metallic film |
JP2009097084A (ja) * | 2007-09-25 | 2009-05-07 | Sanyo Special Steel Co Ltd | 微細形状、微細表面性状を有する精密金属部材の製造方法 |
JP5515539B2 (ja) * | 2009-09-09 | 2014-06-11 | 日産自動車株式会社 | 磁石成形体およびその製造方法 |
CN102383067A (zh) * | 2010-08-27 | 2012-03-21 | 比亚迪股份有限公司 | 一种非晶合金粉体及其制备方法、以及一种非晶合金涂层及其制备方法 |
CN110977144B (zh) * | 2013-04-10 | 2022-09-23 | 斯凯孚公司 | 通过扩散焊接接合两种材料的方法 |
-
2014
- 2014-05-15 PL PL14168461T patent/PL2944401T3/pl unknown
- 2014-05-15 EP EP14168461.3A patent/EP2944401B1/de active Active
- 2014-05-15 ES ES14168461T patent/ES2727507T3/es active Active
-
2015
- 2015-05-12 CN CN201580027018.3A patent/CN106413948B/zh active Active
- 2015-05-12 US US15/310,263 patent/US20170151609A1/en not_active Abandoned
- 2015-05-12 KR KR1020167031362A patent/KR20160143798A/ko active Search and Examination
- 2015-05-12 JP JP2016567346A patent/JP6370925B2/ja active Active
- 2015-05-12 WO PCT/EP2015/060410 patent/WO2015173211A1/de active Application Filing
- 2015-05-14 TW TW104115379A patent/TWI557242B/zh active
Patent Citations (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE3524018A1 (de) | 1985-07-02 | 1987-01-15 | Mannesmann Ag | Verfahren und vorrichtung zum herstellen von metallglas |
US5306463A (en) * | 1990-04-19 | 1994-04-26 | Honda Giken Kogyo Kabushiki Kaisha | Process for producing structural member of amorphous alloy |
WO1999030858A1 (de) | 1997-12-17 | 1999-06-24 | Gunther Schulz | Verfahren und vorrichtung zur herstellung feiner pulver durch zerstäubung von schmelzen mit gasen |
EP1593749A1 (de) * | 2002-12-25 | 2005-11-09 | Japan Science and Technology Corporation | Kugelförmige partikel einer metallischen glaslegierung auf eisenbasis, weichmagnetisches material aus eisenbasierter sinterlegierung in loser form, hergestellt durch sintern desselben, und deren herstellungsverfahren |
EP1813694A1 (de) * | 2004-11-15 | 2007-08-01 | Nikko Materials Co., Ltd. | Sputtertarget zur herstellung eines films aus metallischem glas und herstellungsverfahren dafür |
WO2008039134A1 (en) | 2006-09-26 | 2008-04-03 | Foersvarets Materielverk | Method of producing products of amorphous metal |
EP2430205B1 (de) | 2009-05-14 | 2014-04-02 | BYD Company Limited | Amorphes legierungsverbundmaterial und verfahren zu seiner herstellung |
US20120247948A1 (en) * | 2009-11-19 | 2012-10-04 | Seung Yong Shin | Sputtering target of multi-component single body and method for preparation thereof, and method for producing multi-component alloy-based nanostructured thin films using same |
EP2597166A1 (de) * | 2011-11-24 | 2013-05-29 | Universität des Saarlandes | Massives metallisches Glas bildende Legierung |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE102018115815A1 (de) * | 2018-06-29 | 2020-01-02 | Universität des Saarlandes | Vorrichtung und Verfahren zur Herstellung eines aus einem amorphen oder teilamorphen Metall gebildeten Gussteils sowie Gussteil |
Also Published As
Publication number | Publication date |
---|---|
CN106413948B (zh) | 2019-08-02 |
TW201610187A (zh) | 2016-03-16 |
US20170151609A1 (en) | 2017-06-01 |
ES2727507T3 (es) | 2019-10-16 |
PL2944401T3 (pl) | 2019-08-30 |
EP2944401B1 (de) | 2019-03-13 |
EP2944401A1 (de) | 2015-11-18 |
JP6370925B2 (ja) | 2018-08-08 |
CN106413948A (zh) | 2017-02-15 |
KR20160143798A (ko) | 2016-12-14 |
JP2017520677A (ja) | 2017-07-27 |
TWI557242B (zh) | 2016-11-11 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
WO2015173211A1 (de) | Verfahren zur herstellung eines bauteils aus einer metalllegierung mit amorpher phase | |
WO2016008674A1 (de) | Verfahren zur hestellung eines bauteils aus einer metalllegierung mit amorpher phase | |
WO2019068117A1 (de) | Additiv gefertigtes bauteil und herstellungsverfahren davon | |
EP3360627B1 (de) | Pulver zur verwendung in einem additiven fertigungsverfahren | |
CH522038A (de) | Wolframcarbid enthaltender Sinterhartmetallkörper | |
EP3802898B1 (de) | Dichteoptimierte molybdänlegierung | |
WO2016004448A1 (de) | Verfahren zur herstellung eines bauteils | |
WO2014044429A1 (de) | Herstellen eines refraktärmetall-bauteils | |
EP2736431B1 (de) | Implantat | |
DE102014114830A1 (de) | Verfahren zum Herstellen eines thermoelektischen Gegenstands für eine thermoelektrische Umwandlungsvorrichtung | |
DE60317582T2 (de) | Verfahren zum sintern von aluminium- und aluminiumlegierungsteilen | |
WO2019034506A1 (de) | Kupfer-basierte legierung für die herstellung metallischer massivgläser | |
JP2023502935A (ja) | 三次元物体製造用の球状粉末 | |
JP6815574B1 (ja) | 炭化タングステン粉末 | |
DE102019104492B4 (de) | Verfahren zur herstellung einer kristallinen aluminium-eisen-silizium-legierung | |
DE102018205893B3 (de) | Werkstoff bestehend aus einem dreidimensionalen Gerüst, das mit SiC oder SiC und Si3N4 gebildet ist und einer Edelmetalllegierung, in der Silicium enthalten ist, sowie ein Verfahren zu seiner Herstellung | |
DE2030666A1 (de) | Hartmetallkorper und Verfahren zur Herstellung desselben | |
EP4247578A1 (de) | Isotropes, rissfreies stahldesign mittels additiver fertigungsverfahren |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
121 | Ep: the epo has been informed by wipo that ep was designated in this application |
Ref document number: 15720349 Country of ref document: EP Kind code of ref document: A1 |
|
ENP | Entry into the national phase |
Ref document number: 20167031362 Country of ref document: KR Kind code of ref document: A |
|
ENP | Entry into the national phase |
Ref document number: 2016567346 Country of ref document: JP Kind code of ref document: A |
|
WWE | Wipo information: entry into national phase |
Ref document number: 15310263 Country of ref document: US |
|
NENP | Non-entry into the national phase |
Ref country code: DE |
|
122 | Ep: pct application non-entry in european phase |
Ref document number: 15720349 Country of ref document: EP Kind code of ref document: A1 |