EP3670691B1 - Alliage de magnesium et son procédé de fabrication - Google Patents

Alliage de magnesium et son procédé de fabrication Download PDF

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Publication number
EP3670691B1
EP3670691B1 EP19212085.5A EP19212085A EP3670691B1 EP 3670691 B1 EP3670691 B1 EP 3670691B1 EP 19212085 A EP19212085 A EP 19212085A EP 3670691 B1 EP3670691 B1 EP 3670691B1
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Prior art keywords
phase
magnesium
weight
based alloy
alloy
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German (de)
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EP3670691A1 (fr
Inventor
Stefan Gneiger
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LKR Leichtmetallkompetenzzentrum Ranshofen GmbH
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LKR Leichtmetallkompetenzzentrum Ranshofen GmbH
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C23/00—Alloys based on magnesium
    • C22C23/02—Alloys based on magnesium with aluminium as the next major constituent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D21/00—Casting non-ferrous metals or metallic compounds so far as their metallurgical properties are of importance for the casting procedure; Selection of compositions therefor
    • B22D21/002—Castings of light metals
    • B22D21/007—Castings of light metals with low melting point, e.g. Al 659 degrees C, Mg 650 degrees C
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D21/00—Casting non-ferrous metals or metallic compounds so far as their metallurgical properties are of importance for the casting procedure; Selection of compositions therefor
    • B22D21/02—Casting exceedingly oxidisable non-ferrous metals, e.g. in inert atmosphere
    • B22D21/04—Casting aluminium or magnesium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C23/00—Alloys based on magnesium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C23/00—Alloys based on magnesium
    • C22C23/04—Alloys based on magnesium with zinc or cadmium as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C23/00—Alloys based on magnesium
    • C22C23/06—Alloys based on magnesium with a rare earth metal 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
    • C22F1/06—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon

Definitions

  • the invention relates to a magnesium-based alloy.
  • the invention relates to a method for producing the magnesium-based alloy.
  • Mg-Al alloys are frequently used casting alloys and are particularly widely used in the automotive industry. Mg-Al alloys have proven particularly useful for die-casting processes, additive manufacturing processes or thixomolding processes because, in addition to good mechanical properties at room temperature, they are particularly suitable for castability due to the formation of a eutectic or a eutectic phase at around 437 °C exhibit.
  • the eutectic is formed with an intermetallic Mg 17 Al 12 phase ( ⁇ (Mg)+Mg 17 Al 12 ), which increases the strength of the alloy but at the same time reduces the ductility of the alloy.
  • Mg-Al alloys with an Al content of between 2% by weight and 9% by weight are common.
  • Known alloys are, for example, AZ61 (Mg-Al6%-Zn1%) or AZ91 (Mg-Al9%-Zn1%), designated according to the abbreviation customary in the trade according to the ASTM standard, the proportions being given in each case in % by weight.
  • the usual Al content of Mg -Al alloys between 2 wt. % and 9 wt Alloy is steadily further reduced.
  • Applicable Mg-Al alloys therefore generally have an Al content of less than 10.0% by weight.
  • the document WO 2018/116940 A1 relates to a high thermal resistance Mg-Al alloy.
  • the alloy has 9.0 wt% to 12.0 wt% Al to improve castability by lowering the melting temperature and above addition, Ca, Sr, rare earth elements and Mn to inhibit high-temperature formability by forming phases with aluminum.
  • the document DE 11 2017 001 307 T5 relates to a Mg-Al alloy having high heat resistance and low flammability in the molten state.
  • a Mg-Al alloy having high heat resistance and low flammability in the molten state.
  • 5.0% by weight to 15.0% by weight Al and an addition of in particular a large amount of Sr and in particular a small amount of Ca as well as Mn are provided.
  • the document EP 2 692 884 A1 relates to a Mg-Al alloy with very high strength, in particular to allow forging.
  • the alloy has 14.0% by weight to 23.0% by weight Al and also Ca, Sr and Zn.
  • the object of the invention is to specify a magnesium-based alloy which has both high strength and high ductility and is particularly suitable for die-casting processes or additive manufacturing processes.
  • the basis of the invention is the idea of using the strength-increasing effect of aluminum in a magnesium-based alloy, i.e. providing comparatively high Al proportions in the magnesium-based alloy, but at the same time reducing a proportion of the intermetallic Mg 17 Al 12 phase in order to achieve a possible To reduce reduction in ductility of the magnesium-based alloy.
  • a proportion of the aluminum is bound in the first phase and is therefore no longer fully available for the formation of a Mg 17 Al 12 phase.
  • the first phase which is formed with aluminum, contributes to the strength of the magnesium-based alloy. It is advantageous if the first phase has a favorable morphology with regard to its mechanical properties, in particular high strength or ductility. For example, it is favorable for this if the first phase is designed as a non-coherent structure, preferably in the form of predominantly isolated islands, and/or precipitations of the first phase are as small as possible and/or First phase precipitates have a round or block shape, as explained in detail below. In this way, it is accordingly achieved that the magnesium-based alloy has both high strength and high ductility.
  • the Al proportion is the highest proportion of an element in the magnesium-based alloy.
  • the formation temperature of the Mg 17 Al 12 phase or of the eutectic with the Mg 17 Al 12 phase is usually in the range of around 437 °C, as this from a binary phase diagram of Mg-Al, shown in 1 , can be removed.
  • the Mg 17 Al 12 phase and its formation temperature relate in particular to that Mg 17 Al 12 phase which occurs during the formation of a eutectic ( ⁇ (Mg)+Mg 17 Al 12 ) during cooling of the Mg-Al alloy is formed.
  • a eutectic ⁇ (Mg)+Mg 17 Al 12
  • Mg 17 Al 12 phase which occurs during the formation of a eutectic ( ⁇ (Mg)+Mg 17 Al 12 ) during cooling of the Mg-Al alloy is formed.
  • the third portion forms several different first phases with aluminum, the formation temperatures of which are greater than the formation temperature of the Mg 17 Al 12 phase.
  • This enables the desired strength and ductility of the magnesium-based alloy to be set in a differentiated manner.
  • different elements can be used to form the first phase or a plurality of first phases.
  • rare earth metals (RE) and/or calcium (Ca) have proven to be favorable for the formation of the first phase.
  • the third component forms the at least first phase with at least a component of aluminum which exceeds 10% by weight of aluminum in the second component.
  • the third part thus forms ie with at least the second proportion of aluminum minus 10.0% by weight aluminum, the at least one first phase.
  • a maximum of 10.0% by weight of aluminum is then available for the formation of an Mg 17 Al 12 phase, since the remainder of the aluminum is bound in at least the first phase. The negative influence of the Mg 17 Al 12 phase on the ductility is thus reduced to a practicable level.
  • the third portion of one or more elements can in principle be formed with all elements, apart from magnesium and aluminum, which together with aluminum form a first phase whose formation temperature is higher than that of the Mg 17 Al 12 phase, by a portion of the Mg To reduce 17 Al 12 phase or the eutectic with the Mg 17 Al 12 phase.
  • the minimum addition factor defines a minimum proportion of a respective element for binding 1.0 at % aluminum by the respective element in at least the first phase.
  • a preferably provided proportion of an element of the third proportion is thus obtained by multiplying the proportion of aluminum to be bound by the element in the first phase by the minimum addition factor of the element.
  • the first phase can be formed with one of the aforementioned elements, in particular in accordance with the minimum addition factor of the element, or with several of the aforementioned elements, with the proportion of aluminum to be bonded in the first phase then in particular distributed to the several elements according to their respective minimum addition factors.
  • the first phase and/or the Mg 17 Al 12 phase are each formed as a non-contiguous structure.
  • a non-cohesive structure means formation in the form of predominantly isolated islands, in contrast to formation of a net-like structure, as is often the case in conventional alloys.
  • more than 50% by weight of the first phase or Mg 17 Al 12 phase is in the form of isolated islands.
  • a high strength can be achieved if more than 70% by weight, preferably more than 90% by weight, of the first phase or Mg 17 Al 12 phase in Form of isolated islands are formed. It is favorable if precipitations of the first phase and/or precipitations of the Mg 17 Al 12 phase are as small as possible.
  • a structure of the first phase and/or Mg 17 Al 12 phase or a size of its precipitations can be adjusted in a practical way when cooling the starting materials of the magnesium-based alloy starting from a liquid phase by suitably selecting a cooling rate.
  • the main cause is a slow diffusion rate of aluminum in magnesium.
  • a cooling rate of more than 10 K/s, preferably more than 20 K/s, has proven itself.
  • a size of the precipitates can be kept small with such a cooling rate. Due to a slow diffusion rate of aluminum in magnesium, the proportion of the Mg 17 Al 12 phase is reduced even further.
  • a cooling rate of more than 20 K/s is used, particularly small and homogeneously distributed, non-contiguous precipitations of the first phase and/or Mg 17 Al 12 phase can be achieved, as a result of which particularly high strength and high ductility can be achieved.
  • strength is further increased by pronounced solid solution strengthening and corrosion resistance is improved.
  • Such cooling rates are generally used in a die-casting process or an arc process or a plasma process, which is why these methods or processes are particularly suitable for an application or production of the magnesium-based alloy according to the aforementioned effects.
  • a further improvement in the mechanical properties can be achieved if precipitations of the first phase and/or precipitations of the Mg 17 Al 12 phase have a round or block shape. This can be achieved by a coordinated choice of the elements of the third part and often also by choosing a suitable cooling rate during manufacture.
  • a similarly favorable behavior is also evident when the third portion is formed with calcium, preferably with a portion of more than 0.2 to 0.44% by weight.
  • misch metal or cerium misch metal has proven to be particularly suitable for achieving the effects provided according to the invention. Accordingly, it is favorable if the third proportion is formed with misch metal, in particular with a proportion of more than 2.5 to 3.5% by weight. In particular in combination with calcium, preferably in accordance with the aforementioned proportions, a particularly pronounced strength and high extensibility results.
  • the third portion is formed with more than 0.15 to 0.5% by weight, preferably about 0.3% by weight, of manganese. In addition to increasing strength, this also improves corrosion resistance.
  • the third portion is formed with mixed metal calcium and manganese, expediently in accordance with the aforementioned respective portions. This achieves high strength, high ductility and pronounced corrosion resistance. It is also advantageous for this if the third proportion is also formed with strontium, preferably with a proportion of between 0.2% by weight and 0.6% by weight.
  • magnesium-based alloy is formed with more than more than 0.3 to 0.6% by weight, preferably about 0.5% by weight, zinc. This further increases strength.
  • the magnesium-based alloy has more than 10.1% by weight to 11.5% by weight aluminum. It has been shown that the effects provided by the invention in terms of conventional manufacturing processes with large Cooling rates can be achieved particularly practicable when the Magnesium-based alloy has 10.1 to 11.5% by weight aluminum.
  • the further object of the invention is achieved by a method for producing a magnesium-based alloy according to the invention, starting materials of the magnesium-based alloy being cooled starting from a liquid phase or a melt in order to form the first phase and then the Mg 17 Al 12 phase.
  • a corresponding magnesium-based alloy can advantageously be produced with the method. Since the first phase has a formation temperature which is higher than the formation temperature of the Mg 17 Al 12 phase, a proportion of the aluminum is bound in the first phase and the bound amount is no longer available for formation of the Mg 17 Al 12 phase Disposal.
  • a composition of the liquid phase or melt corresponds to the general composition explained above or, if appropriate, to one of the specific compositions also explained.
  • the starting materials are cooled at a cooling rate of more than 10 K/s, preferably more than 20 K/s.
  • a cooling rate of more than 20 K/s is used, particularly small and homogeneously distributed, non-contiguous precipitations of the first phase and/or Mg 17 Al 12 phase can be achieved, as a result of which particularly high strength and high ductility can be achieved.
  • wire-arc additive manufacturing has proven itself when a die-casting process or arc welding, in particular wire-arc additive manufacturing, is used. These production techniques are operated with high cooling rates, which is why they are particularly suitable for producing or using a magnesium-based alloy according to the invention, since, as explained above, high cooling rates lead to particularly high strength and high ductility of the magnesium-based alloy. Above all, wire arc additive manufacturing (WAAM) has proven to be particularly suitable. An arc welding process is used to build up a component in layers. The high cooling rates used in wire-arc additive manufacturing lead to homogeneous and finely divided precipitations of both the first phase and the Mg 17 Al 12 phase, which means that high strength and ductility can be achieved. This makes it possible to produce complex components with the magnesium-based alloy according to the invention, which are particularly robust.
  • WAAM wire arc additive manufacturing
  • a starting material, semi-finished product or component is advantageously produced with a magnesium-based alloy according to the invention or according to a method according to the invention. According to the above statements, features and effects of the magnesium-based alloy according to the invention or a magnesium alloy produced using a method according to the invention, a starting material, semi-finished product or component formed with the magnesium-based alloy also has an advantageously high strength and high ductility.
  • phase diagram 1 shows a phase diagram known from the prior art for an alloy composition of Mg and aluminum, shown up to an aluminum content of 60% by weight.
  • a conventional alloy with Mg-Al9% (in % by weight) known from the prior art is drawn in the phase diagram with a vertical dashed line.
  • Mg-Al9% alloy cools down, starting from a liquid phase L, only a mixed-crystal phase ⁇ (Mg) initially solidifies.
  • a eutectic or a eutectic phase formed with an Mg 17 Al 12 phase, is finally precipitated, as can be seen from the phase diagram.
  • This brittle intermetallic Mg 17 Al 12 phase usually leads to an increase in strength of an Mg-Al alloy, in particular also of the Mg-Al9% alloy shown, but at the same time reduces its ductility.
  • an Al content of both the AEX11-1 alloy and the AEX11-2 alloy was selected in a range slightly above 10.0% by weight in order to achieve advantageous effects of the two alloys compared to conventional Mg Show Al alloys, which usually have Al shares of up to about 9.0 wt .-%.
  • phase 2 shows a comparison of the AEX11-1 alloy with that of a standard AZ91 alloy, showing different phase fractions of the two alloys, which were calculated using the Thermocalc simulation software.
  • Phase portions of the AEX11-1 alloy are shown as solid lines, phase portions of the AZ91 alloy as dashed lines.
  • the proportions of the liquid phase L, the ⁇ (Mg) and the Mg 17 Al 12 phase are shown for both the AEX11-1 alloy and the AZ91 alloy.
  • RE is an abbreviation for rare earth metals.
  • FIG. 12 clearly shows that the AEX11-1 alloy has a lower proportion of the Mg 17 Al 12 phase compared to the AZ91 alloy despite a higher Al content.
  • a formation temperature of the Mg 17 Al 12 phase is between 360°C and 370°C in both AEX11-1 and AZ91.
  • a formation temperature of the Al 11 RE 3 phase of the AEX11-1 alloy is around 560°C.
  • the formation temperature of the Al 11 RE 3 phase is significantly higher than the formation temperature of the Mg 17 Al 12 phase
  • cooling of an initial composition of the AEX11-1 alloy starting from the liquid phase results in the formation of the Al 11 RE 3 -Phase bound an Al proportion, so that when the formation temperature of the Mg 17 Al 12 phase is reached, only a reduced Al proportion is available for the formation of the Mg 17 Al 12 phase.
  • the Al 11 RE 3 phase contributes to the high strength of the AEX11-1 alloy, the reduced proportion of the Mg 17 Al 12 phase leads to high ductility in the AEX11-1 alloy.
  • phase of the AEX11-1 alloy such as an Al-Mn phase, are in 2 not shown as this have negligibly small proportions compared to the Al 11 RE 3 phase.
  • the AEX11-2 alloy shows a behavior analogous to the AEX11-1 alloy.
  • Alloy samples for AEX11-1 and AEX11-2 were gravity cast into billets and extruded into wires. Finally, sample parts made of the AEX11-1 alloy and the AEX11-2 alloy were manufactured from the wires using an arc welding process using Wire-Arc-Additive-Manufacturing.
  • FIG. 3 shows a representative microstructure image of an AEX11-1 sample portion.
  • a relatively fine, homogeneous microstructure can be seen, which shows needle-shaped Al-RE precipitation phases (in dark grey) and Mg 17 Al 12 precipitation phases (in light grey).
  • isolated Al-Mn phases in dark gray and block-shaped
  • the phases shown are each formed as a non-contiguous structure, in particular as isolated islands, as a result of which a particularly pronounced strength can be achieved.
  • the AEX11-2 specimens show analogous microstructure images.
  • the Mg 17 Al 12 phase or the eutectic phase formed with it can be dissolved by heat treatment and, if necessary, can then be separated out again to increase strength.
  • figure 5 shows a stress-strain diagram as a result of dilatometer tensile tests of the sample parts before and after a heat treatment. Shown are stress-strain curves for an AEX11-1 sample part prior to its heat treatment, denoted in figure 5 denoted by reference numeral 1 and after its heat treatment, denoted by reference numeral 2, and stress-strain curves for an AEX11-2 sample part before its heat treatment, denoted by reference numeral 3, and after its heat treatment, denoted by reference numeral 4. For comparison, also a stress-strain curve, for a typical AZ61 alloy sample, identified in figure 5 shown with reference number 5, which is manufactured with a method corresponding to the manufacturing method of the two AEX11 sample parts.
  • the AEX11-1 specimen and AEX11-2 specimen have very high yield strengths, which are higher than a yield strength of the AZ61 alloy specimen.
  • ductility of the AEX11-1 sample part and AEX11-2 sample part before the heat treatment of the sample parts are lower than that of the AZ61 alloy sample.
  • both the AEX11-1 specimen and the AEX11-2 specimen exhibit high strength and high ductility.
  • a heat treatment thus makes it possible to adjust the strength and extensibility.
  • heat treatment does not improve strength or ductility. This is by looking at a microstructure image of the AZ61 alloy sample shown in 6 , also understandable.
  • a magnesium-based alloy according to the invention thus advantageously has both high strength and high ductility and in particular offers the possibility of adjusting strength and ductility by heat treatment.

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

Claims (7)

  1. Alliage à base de magnésium, comportant (en % en poids) dans un premier composant, du magnésium,
    dans un deuxième composant, plus de 10,1 % à 11,5 % d'aluminium,
    un troisième composant, d'un ou de plusieurs éléments formant avec l'aluminium au moins une première phase, ledit troisième composant étant formé en mettant en oeuvre :
    0,15 % en poids à 0,5 % en poids de manganèse,
    2,5 % en poids à 3,5 % en poids de mischmétal,
    0,2 % en poids à 0,44 % en poids de calcium,
    optionnellement, 0,2 % en poids à 0,6 % en poids de strontium
    plus de 0,3 % à 0,6 % de zinc,
    le reste étant du magnésium et des impuretés issues du processus de fabrication,
    ledit alliage à base de magnésium contenant une phase Mg17Al12 et une température de formation de la première phase étant supérieure à une température de formation de la phase Mg17Al12.
  2. Alliage à base de magnésium selon la revendication 1, caractérisé en ce que ledit troisième composant forme l'au moins une première phase avec au moins une telle proportion d'aluminium que celle-ci sera, dans le deuxième composant, supérieure à 10 % en poids d'aluminium.
  3. Alliage à base d'aluminium selon les revendications 1 ou 2, caractérisé en ce que le troisième composant forme avec l'aluminium plusieurs premières phases différentes dont les températures de formation sont supérieures à la température de formation de la phase Mg17Al12.
  4. Alliage à base d'aluminium selon l'une des revendications 1 à 3, caractérisé en ce que la première phase et/ou la phase Mg17Al12 sont chacune formée de manière à ne pas constituer de structure contiguë.
  5. Procédé de fabrication d'un alliage à base de magnésium selon l'une des revendications 1 à 4, les matières de départ dudit alliage à base de magnésium étant refroidies à partir d'une phase liquide, pour ainsi former la première phase et ensuite la phase Mg17Al12, le refroidissement des matières de départ étant réalisé avec un taux de refroidissement supérieur à 10 K/s, de préférence supérieur à 20 K/s.
  6. Procédé selon la revendication 5 caractérisé en ce que l'on met en œuvre un procédé de coulée sous pression ou du soudage à l'arc, notamment du Wire Arc Additive Manufacturing.
  7. Matériau précurseur, produit semi-fini ou élément constitutif comportant un alliage à base de magnésium selon l'une des revendications 1 à 4 ou pouvant être obtenu conformément à un procédé selon l'une des revendications 5 ou 6.
EP19212085.5A 2018-12-18 2019-11-28 Alliage de magnesium et son procédé de fabrication Active EP3670691B1 (fr)

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ATA51127/2018A AT522003B1 (de) 2018-12-18 2018-12-18 Magnesiumbasislegierung und Verfahren zur Herstellung derselben

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EP3670691B1 true EP3670691B1 (fr) 2023-01-25

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AT521500B1 (de) * 2018-12-18 2020-02-15 Lkr Leichtmetallkompetenzzentrum Ranshofen Gmbh Verfahren zur Erhöhung einer Korrosionsbeständigkeit eines mit einer Magnesiumbasislegierung gebildeten Bauteiles gegen galvanische Korrosion sowie damit erhältliches korrosionsbeständiges Bauteil

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JP2001247926A (ja) * 2000-03-03 2001-09-14 Japan Steel Works Ltd:The 流動性に優れたマグネシウム合金およびマグネシウム合金材
KR101127113B1 (ko) * 2004-01-09 2012-03-26 켄지 히가시 다이캐스트용 마그네슘 합금 및 이것을 사용한 마그네슘다이캐스트 제품
DE102005033835A1 (de) * 2005-07-20 2007-01-25 Gkss-Forschungszentrum Geesthacht Gmbh Magnesiumsekundärlegierung
JP4539572B2 (ja) * 2006-01-27 2010-09-08 株式会社豊田中央研究所 鋳造用マグネシウム合金および鋳物
TWI427158B (zh) * 2009-06-26 2014-02-21 Foxconn Tech Co Ltd 鎂合金及其製備方法
JP5729081B2 (ja) * 2011-03-29 2015-06-03 株式会社新技術研究所 マグネシウム合金
US10808302B2 (en) * 2016-07-15 2020-10-20 Sumitomo Electric Industries, Ltd. Magnesium alloy
WO2018116940A1 (fr) * 2016-12-21 2018-06-28 住友電気工業株式会社 Alliage de magnésium

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EP3670691A1 (fr) 2020-06-24
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AT522003A3 (de) 2021-07-15

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