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EP2646587B1 - Procédé de fabrication d'un alliage alscca et alliage alscca - Google Patents

Procédé de fabrication d'un alliage alscca et alliage alscca Download PDF

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Publication number
EP2646587B1
EP2646587B1 EP11831814.6A EP11831814A EP2646587B1 EP 2646587 B1 EP2646587 B1 EP 2646587B1 EP 11831814 A EP11831814 A EP 11831814A EP 2646587 B1 EP2646587 B1 EP 2646587B1
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EP
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Prior art keywords
alloy
aluminum
scandium
calcium
weight
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EP11831814.6A
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German (de)
English (en)
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EP2646587A2 (fr
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Frank Palm
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Airbus Defence and Space GmbH
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Airbus Defence and Space GmbH
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C22C1/026—Alloys based on aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/06—Alloys based on aluminium with magnesium as the next 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
    • C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
    • C22F1/047—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon of alloys with magnesium as the next major constituent

Definitions

  • US 5 211 910 describes an aluminum alloy which may contain scandium and / or calcium in a proportion of 0.5 to 4 wt.%.
  • WO 2007/102988 A2 discloses an aluminum alloy which may have calcium and / or scandium in a range of 0.01 to 6%.
  • melt-spinning describes a process by which melting, in particular molten metal, is cooled at very high speeds, ie. be deterred.
  • KBM AFFILIPS Master Alloys offers on its website aluminum base alloys, such as aluminum-magnesium alloys, aluminum-scandium alloys or aluminum-calcium alloys.
  • CN 100 402 683 C describes a process for producing an aluminum foam in which an aluminum melt is first mixed with 1 to 11% magnesium, 0.5 to 5.5% calcium and 0.1 to 1.2% rare earth metal, followed by foaming of the aluminum melt titanium hydride, zirconium hydride , Volcanic ash or the like is added.
  • the object of the invention is to propose an aluminum scandium-calcium alloy with reduced density and a simple and harmless method for producing this alloy.
  • calcium has a significantly lower volume weight than aluminum and thus contributes to a reduction in the total density of the alloy when alloyed with an aluminum scandium alloy.
  • a material made with such an alloy is lightweight and yet largely exhibits the strength properties of the aluminum scandium alloy.
  • the melt with calcium can be easily handled under atmospheric conditions, so that protective measures, such as the lining of gutters and pots with oxides or the use of inert gas, are not necessary.
  • a high-strength, low-density aluminum alloy can be produced in a simple and harmless method.
  • Calcium is added in a proportion of more than 0.5% by weight and less than 5% by weight.
  • calcium is present with a significant proportion in the alloy and significantly reduces the weight of the alloy and also of the materials produced therefrom.
  • the weight of the alloy can be reduced by about 5% over the aluminum scandium alloy.
  • the common melt is quenched by means of a rapid solidification process at a rate of 10,000 K / s to 10,000,000 K / s.
  • a rapid solidification process Through a normal metallurgical manufacturing pathway followed by cast solidification with slow cooling conditions after melting, it has hitherto been difficult to alloy calcium in significant amounts to an aluminum scandium alloy. Because it immediately forms an Al 2 Ca phase, which is excreted and embrittles the alloy.
  • the problem of limited solubility and unwanted premature coarse deterioration of calcium in aluminum alloys can be overcome and calcium remains largely in solution because rapid cooling prevents natural crystallization. This robs the atoms of mobility before they can take a crystal arrangement and thus Al 2 Ca can be formed.
  • Methods which are suitable are all solidification processes in which the heat is quickly removed from the melt, for example spin-casting, powder atomization by means of gas or in water, strip-casting or spray-compacting, but also processes in which a melt is generated at short notice and solidifies immediately, for example, welding processes for joining, surface modification or for the generative production of three-dimensional components, the so-called "layer-building process"("additivemanufacturing”).
  • the common melt is sprayed onto a substrate by means of a nozzle as a jet, wherein the substrate is cooled and rotated during the application of the common melt.
  • the substrate may be, for example, a water-cooled copper wheel.
  • the cooling results in a temperature difference between the common melt and the substrate, so that a temperature transfer from the melt takes place on the substrate. The higher the temperature difference, the faster the temperature is transferred to the substrate and dissipated by the cooling. Further, the rate of cooling, and hence the presence of rapid solidification to prevent Al 2 Ca phase formation, depends on the rate at which the melt impinges on the substrate and on the rotational speed of the rotated substrate.
  • the substrate is preferably rotated so fast that the quenched common melt is thrown off the substrate from an impact area of the nozzle jet on the substrate, the substrate is automatically freed from the solid alloy already formed by quenching and stands for subsequently sprayed common melt for cooling to disposal.
  • the centrifuged common melt forms a band which can be further processed in subsequent process steps.
  • the belt is first chopped small, processed into granules or powder, and then bolted in a press and outgassing / annealing process compacted.
  • the bolts ie the particulate starting material, can then be extruded into extruded profiles with different cross sections.
  • the process is preferably carried out under atmospheric conditions, in particular under air contact.
  • measures for protecting the common melt against the atmosphere are no longer necessary, it can be dispensed with the use of inert gas, vacuum conditions, protection device and the like. This significantly simplifies and reduces the cost of the process compared to adding lithium.
  • step a) comprises the step of melt-bringing an aluminum-magnesium base alloy.
  • Magnesium has a density of 1.74 g / cm 3. At the same time it controls and reduces the density of the corresponding alloy. The more magnesium in the alloy, the lower the density.
  • the alloying of magnesium to aluminum is useful up to a proportion of 10 wt .-%. Due to the similar melting points of aluminum and magnesium, production of an aluminum-magnesium base alloy is particularly easy to produce.
  • Aluminum scandium alloy is a generic term for all alloys containing aluminum and scandium. This includes all compositions having the formula AlScM 1 M 2 M 3 M 4 where M 1 is a metal selected from the group consisting of copper, magnesium, manganese, silicon, iron, beryllium, lithium, chromium, zinc, silver , Vanadium, nickel, cobalt and molybdenum, and wherein M 2 is a metal selected from the group consisting of copper, magnesium, manganese, silicon, iron, beryllium, lithium, chromium, zinc, silver, vanadium, nickel, Contains cobalt and molybdenum.
  • M 3 comprises the group of elements which, with the Al 3 Sc phase, have a certain compatibility, ie metal-physical similarity (exchangeability), and can therefore form the tertiary phase Al 3 Sc 1 -xM 3 x.
  • these are zirconium, niobium, tantalum, hafnium and titanium.
  • M 4 comprises the group of the so-called rare earths (element numbers 39 and 57 to 71), which in principle are very similar to scandium. Therefore, Sc is often wrongly attributed to rare earths. In addition to the scandium of the alloy, they can also be alloyed to a considerable extent and then, in addition to solid solution hardening alone or with scandium, form a hardening phase with comparable stoichiometry as Al 3 Sc 1 -xM 3 x.
  • step a) an aluminum scandium master alloy is melted.
  • Scandium has a significantly higher melting point than aluminum, which is why a long retention time must be maintained to form an alloy. This is complicated, which is why it is advantageous if, instead of the pure elements, a master alloy is used in which the scandium is already "melted in” and thus a shorter holding time must be maintained for forming the aluminum scandium-calcium alloy.
  • an aluminum-calcium master alloy is further melted in step a).
  • calcium has a significantly higher melting point (842 ° C) than aluminum, and the pre-alloy, the required melting point and thus the holding time is preferably reduced.
  • the aluminum scandium-calcium alloy has a calcium content of more than 0.5% by weight and less than 5.0% by weight.
  • the density of the aluminum-scandium alloy can be reduced by containing an easily available and easy-to-handle metal as an alloying component in the alloy.
  • the AlScCa alloy comprises 0.3 wt% to 1.5 wt%, and preferably 0.4 wt% to 1.5 wt%, scandium.
  • scandium When scandium is contained in the specified amounts in the alloy, it increases the strength of the alloy, but does not contribute so much to an increase in density of the alloy material made from it would be too heavy for lightweight construction.
  • ytterbium instead of scandium, can also be alloyed in the stated proportions of the alloy. Ytterbium is cheaper than scandium, but has the disadvantage of not improving the strength of the alloy as well as scandium.
  • the alloy comprises from 0.1% to 1.5% and preferably from 0.2% to 0.75% zirconium by weight.
  • Zirconium in such a proportion in the alloy facilitates the temperature-enhanced processing of the alloy and stabilizes it thermally, ie it reduces the tendency to "age", which is equivalent to an unwanted coarsening of the curing phase Al 3 Sc by formation of an Al 3 ScZr phase.
  • the AlScCa alloy contains 1.0 wt% to 8.0 wt%, and preferably 2.5 wt% to 6.0 wt%, of magnesium.
  • Magnesium lowers the density of an aluminum alloy.
  • the alloying of magnesium to aluminum makes sense only up to certain amounts, since otherwise negative properties such as brittleness and corrosion sensitivity increase greatly. Therefore, magnesium is preferably contained in the stated proportions in the alloy.
  • the alloy optionally comprises further admixtures, also in multiple form, of the elements mentioned in M 1 , M 2 , M 3 and M 4 with the proportions 0.2 to 2.0% by weight, which have the mechanical, physical or chemical properties improve the alloy.
  • Unavoidable is the presence in the alloy of unwanted impurities of both metallic and non-metallic nature, such as oxides, nitrides, dissolved gases, etc., in negligible amounts, ie, less than 0.5% by weight).
  • the alloy has a density less than 2.6 g / cm 3 .
  • the alloy is particularly well suited as a basic material for lightweight construction.
  • the alloy has substantially the same strength and essentially the same elastic modulus as the pure aluminum scandium alloy in which no alloyed calcium is contained.
  • the alloy has the positive properties of the aluminum scandium base alloy, i. substantially the same strength and modulus of elasticity, but is denser reduced by the presence of calcium and thus easier.
  • An aluminum scandium-calcium material has more than 0.5 wt .-% calcium. Such a material is characterized by particularly good strength values and a high modulus of elasticity, but has a reduced density and is therefore particularly suitable for lightweight construction.
  • Fig. 1 shows how in a common crucible 10, the metals scandium 12 and calcium 14 are mixed into an aluminum-magnesium base alloy 17 containing aluminum 15 and magnesium 16.
  • the crucible 10 has on its underside a nozzle 18, which is separated by a closing device 19 of the crucible 10.
  • scandium 12 is added as aluminum scandium master alloy 20 and calcium 14 as aluminum calcium master alloy 21.
  • the mixture is heated with an induction heater 23.
  • induction heater 23 other suitable heating possibilities for bringing the metals 12, 14, 15, 16 into molten metal are also possible.
  • a common melt 22 has formed.
  • Fig. 2 It is shown how the common melt 22 is sprayed onto a rotating substrate 24.
  • the closing device 19 is opened between the nozzle 18 and the crucible 10, so that the common melt 22 can flow into the nozzle 18.
  • the nozzle 18 sprays the common melt 22 in a jet 30 onto a landing area 32 on a surface 33 of the substrate 24.
  • the substrate 24 is cooled on a side facing the landing area 32 via a cooling device 34.
  • the substrate 24 is rapidly rotated about the axis 35 in the direction of the arrow O.
  • the common melt 22 solidifies on the cooled substrate 24 at a high cooling rate to an aluminum-scandium-calcium alloy 36.
  • Fig. 3 shows the substrate 24 from a rear side 42, which is opposite to the surface 33.
  • the cooling device 34 is arranged in the form of a cooling coil 44. Water can be passed through the cooling coil 44, for example in the direction of the arrow, so as to cool the substrate 24.
  • Fig. 4 shows a view of the surface 33 of the substrate 24.
  • the substrate 24 is rotated in the direction of arrow P so fast that the solidified aluminum scandium calcium alloy 36 is ejected as an alloy strip 40 from the surface 38 by the resulting forces.
  • An AlMg5.4Sc1.2Zr0.6Mn0.5 alloy is alloyed with 2.0% by weight of calcium according to the method described above.
  • the alloy ribbon is chopped into granules and then degassed in a heatable device at 290 to 300 ° C with alternating rinsing with vacuum at about 10 to 2 mbar and supply of dry nitrogen and repeated vacuum suction.
  • the degassing process is carried out five times and the granules are compacted by means of a hydraulic press into a stud with 98% gross density and 31 mm diameter at 25 -30 mm length.
  • This bolt is then turned over to 30 mm and then pressed in an extrusion apparatus with a compression ratio of 25: 1 at 325 to 335 ° C to a 6 mm round rod.
  • Standard round tensile specimens EN 10001 B6 x 30 are taken from the round bar and the strength tested.
  • the microstructure hardness can be determined using the Brinell hardness test method (HB2.5 / 6.5) on small disks from the 6 mm rod
  • Fabric-based lightweight construction requires construction materials with high strength and low density, ie high specific strength, also called breaking length.
  • High-strength AlMgSc alloys have a density of 2.62 to 2.86 g / cm 3 or an Mg content of 6.0 to 2.5% by weight.
  • AlMg materials all of which are written in field AA5XXX in their American Al alloy key composition, are widely used because of their relatively low densities and are very popular for their good strength and processing properties.
  • the magnesium content of the alloy partly controls the strength via solid solution hardening, but at the same time also determines the density of the corresponding alloys, since magnesium 16 has a density of 1.74 g / cm 3 . This should be as low as possible, especially from a lightweight construction point of view. The more magnesium 16 in the alloy, the lower the density. It is known that the addition of magnesium 16 to aluminum 15, and thus the associated reduction in density, makes sense only up to certain amounts, since otherwise other negative properties such as brittleness and corrosion sensitivity increase greatly.
  • high magnesium aluminum materials have a magnesium content of less than 6 wt .-% (eg AA5059 or AA5083).
  • the alloying of lithium is state of the art, the alloying of calcium 14 in AlMgSc alloys not.
  • the alternative to lowering the density, ie the alloying of lithium with a density of 0.52 g / cm 3 was already developed in the 20s of the last century and technically implemented in Russia especially from the late 70s.
  • a further reduction in density by addition of lithium (0.5 g / cm 3 ) or only calcium 14 (1.55 g / cm 3 ) is possible.
  • the alloying of scandium 12, combined with a sufficiently rapid cooling after casting or during solidification, allows by means of defined heat conduction, eg downstream hot aging in the temperature range between 250 and 400 ° C, for these materials, a further increase in strength of precipitation hardening over a fully or partially coherent Al 3 Sc phase and / or dispersoid hardening, when the Al 3 Sc phase becomes increasingly incoherent due to overaging.
  • the density of AlMgSc sheet and more of extruded sections is determined by the amount of magnesium 16 which is added to this type of solid solution for solid solution hardening. This results in a limited minimum density for higher-strength AlMgSc alloys.
  • the alloying of calcium 14 with a density of 1.55 g / cm 3 and in an amount of more than 0.5% by weight is hitherto used in high-strength aluminum-magnesium-scandium alloy concepts for applications in the traffic or air & Space area not available.
  • the aluminum-magnesium-scandium alloys the alkaline earth element calcium 14 with a density of 1, 54 g / cm 3 alloy and thus further reduce the density of these attractive high-strength aluminum materials.
  • High-strength aluminum-magnesium scandium materials with a reduced density of less than 2.6 g / cm 3 can be obtained as profiles, but also high-strength aluminum-magnesium scandium materials with a reduced density of less than 2.6 g / cm 3 as directly generated (eg remelted by laser) close-net shape components, the components are more efficient lightweight structures with high longevity.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Continuous Casting (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Forging (AREA)

Claims (10)

  1. Alliage à base d'aluminium - scandium - calcium (36), constitué de :
    - 0,3 % en poids à 1,5 % en poids de scandium (12),
    - 1,0 % en poids à 8,0 % en poids de magnésium (16),
    - entre 0,5 et 5 % en poids de calcium (14),
    - 0,1 % en poids à 1,5 % en poids de zirconium,
    - le reste étant de l'aluminium et des impuretés inévitables d'une somme inférieure à 0,5 % en poids,
    et d'autres additifs optionnels, également sous forme multiple, des éléments M1, M2, M3, M4 avec les proportions de 0,2 à 2,0 % en poids, dans lequel
    - M1 est choisi parmi le groupe comprenant le cuivre, le magnésium, le manganèse, le silicium, le fer, le béryllium, le lithium, le chrome, le zinc, l'argent, le vanadium, le nickel, le cobalt et le molybdène,
    - M2 est choisi parmi le groupe comprenant le cuivre, le magnésium, le manganèse, le silicium, le fer, le béryllium, le lithium, le chrome, le zinc, l'argent, le vanadium, le nickel, le cobalt et le molybdène,
    - M3 est choisi parmi le groupe comprenant le zirconium, le niobium, le tantale, le hafnium et le titane,
    - M4 est choisi parmi le groupe des terres rares.
  2. Alliage selon la revendication 1, dans lequel le scandium (12) est contenu en une proportion quantitative de 0,4 % en poids à 1,5 % en poids et/ou le magnésium (16) est contenu en une proportion quantitative de 2,5 à 6,0 % en poids.
  3. Alliage selon la revendication 1 ou 2, dans lequel le zirconium est contenu en une proportion quantitative de 0,2 à 0,75 % en poids.
  4. Alliage selon l'une des revendications précédentes, caractérisé en ce que l'alliage présente une densité inférieure à 2,6 g/cm3.
  5. Procédé de réalisation d'un alliage à base d'aluminium - scandium - calcium selon l'une des revendications 1 à 4 en ajoutant du calcium aux autres composantes de l'alliage, comprenant les étapes suivantes :
    a) la mise en fusion commune des composantes de l'alliage; et
    b) la trempe de la fonte commune (22) au moyen d'un processus de solidification rapide à une vitesse de plus de 100 K/s.
  6. Procédé selon la revendication 5, dans lequel la trempe s'effectue à une vitesse dans la plage de 10 000 K/s à 10 000 000 K/s.
  7. Procédé selon l'une des revendications 5 et 6, caractérisé en ce que la fonte commune (22) est pulvérisée en tant que jet (30) sur un substrat (24) au moyen d'une buse (18), le substrat (24) étant refroidi et tourné pendant l'application de la fonte commune (22).
  8. Procédé selon la revendication 7, caractérisé en ce que le substrat (24) est tourné aussi rapidement que la fonte commune trempée (22) est éjectée du substrat (25) à partir d'une zone d'impact (32) du jet (30) sur le substrat (24).
  9. Procédé selon l'une des revendications précédentes, caractérisé en ce que le procédé est mis en oeuvre dans des conditions atmosphériques, en particulier au contact avec l'air.
  10. Procédé selon l'une des revendications précédentes, caractérisé en ce que l'étape a) comprend l'étape de la mise en fusion d'un alliage de base (17) d'aluminium - magnésium et/ou de la mise en fusion un pré-alliage (20) d'aluminium - scandium et/ou la mise en fusion d'un pré-alliage (21) d'aluminium - calcium.
EP11831814.6A 2010-12-02 2011-11-30 Procédé de fabrication d'un alliage alscca et alliage alscca Active EP2646587B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102010053274A DE102010053274A1 (de) 2010-12-02 2010-12-02 Verfahren zum Herstellen einer AlScCa-Legierung sowie AlScCa-Legierung
PCT/DE2011/002050 WO2012075993A2 (fr) 2010-12-02 2011-11-30 Procédé de fabrication d'un alliage alscca et alliage alscca

Publications (2)

Publication Number Publication Date
EP2646587A2 EP2646587A2 (fr) 2013-10-09
EP2646587B1 true EP2646587B1 (fr) 2017-10-11

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US (2) US9725790B2 (fr)
EP (1) EP2646587B1 (fr)
DE (1) DE102010053274A1 (fr)
WO (1) WO2012075993A2 (fr)

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EP4159344A1 (fr) 2021-09-30 2023-04-05 Airbus (S.A.S.) Alliage aluminium-nickel pour la fabrication d'une pièce thermoconductrice, tel qu'un échangeur de chaleur
US11802325B2 (en) 2018-05-21 2023-10-31 Obshchestvo S Ogranichennoy Otvetstvennost'yu Obedinennaya Kompaniya Rusal “Inzherno-Tekhnologicheskiy Tsentr” Aluminum alloy for additive technologies

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WO2021025531A1 (fr) * 2019-08-07 2021-02-11 액츠테크놀러지스 주식회사 Alliage d'aluminium pour impression 3d ou fabrication additive, procédé d'impression 3d ou de fabrication additive utilisant celui-ci, et produit ou composant d'alliage d'aluminium fabriqué par impression 3d ou fabrication additive
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Publication number Priority date Publication date Assignee Title
US11802325B2 (en) 2018-05-21 2023-10-31 Obshchestvo S Ogranichennoy Otvetstvennost'yu Obedinennaya Kompaniya Rusal “Inzherno-Tekhnologicheskiy Tsentr” Aluminum alloy for additive technologies
EP4159344A1 (fr) 2021-09-30 2023-04-05 Airbus (S.A.S.) Alliage aluminium-nickel pour la fabrication d'une pièce thermoconductrice, tel qu'un échangeur de chaleur
US12139778B2 (en) 2021-09-30 2024-11-12 Airbus Sas Aluminium-nickel alloy for manufacturing a heat conducting part, such as a heat exchanger

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US20130312876A1 (en) 2013-11-28
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US9725790B2 (en) 2017-08-08
EP2646587A2 (fr) 2013-10-09
WO2012075993A3 (fr) 2012-08-23
US20170298477A1 (en) 2017-10-19

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