EP0357743B1 - Hochfeste magnesiumlegierungen und verfahren, um derartige legierungen mittels rascher erstarrung zu erhalten - Google Patents

Hochfeste magnesiumlegierungen und verfahren, um derartige legierungen mittels rascher erstarrung zu erhalten Download PDF

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Publication number
EP0357743B1
EP0357743B1 EP89903172A EP89903172A EP0357743B1 EP 0357743 B1 EP0357743 B1 EP 0357743B1 EP 89903172 A EP89903172 A EP 89903172A EP 89903172 A EP89903172 A EP 89903172A EP 0357743 B1 EP0357743 B1 EP 0357743B1
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EP
European Patent Office
Prior art keywords
alloy
alloys
temperature
magnesium
extrusion
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP89903172A
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English (en)
French (fr)
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EP0357743A1 (de
Inventor
Gilles Regazzoni
Gilles Nussbaum
Haavard T. Gjestland
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Ferropem SAS
Norsk Hydro ASA
Original Assignee
Pechiney Electrometallurgie SAS
Norsk Hydro ASA
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Priority claimed from FR8802885A external-priority patent/FR2627780B1/fr
Application filed by Pechiney Electrometallurgie SAS, Norsk Hydro ASA filed Critical Pechiney Electrometallurgie SAS
Publication of EP0357743A1 publication Critical patent/EP0357743A1/de
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Classifications

    • 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
    • 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
    • C22C45/00—Amorphous alloys
    • C22C45/005—Amorphous alloys with Mg 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
    • C22F1/06—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 present invention relates to magnesium-based alloys with high mechanical strength, as well as a process for obtaining these alloys by rapid solidification and consolidation by spinning. It relates in particular to alloys containing Al, at least Zn and / or Ca and which can contain manganese whose weight composition is situated within the following limits: Al: 2 - 11% Zn: 0 - 12% Mn: 0 - 0.6% Ca: 0 - 7% but always with the presence of Zn and / or Ca with the following content of impurities: If: 0.1 - 0.6 Cu: ⁇ 0.2 Fe: ⁇ 0.1 Ni: ⁇ 0.01 the rest being magnesium.
  • alloys with high mechanical strength having a composition corresponding to that of the basic commercial alloys of the prior art, listed under the names AZ31, AZ61, AZ80 (wrought alloys) and AZ91, AZ92 (casting alloys), according to ASTM standard, or G-A3Z1, G-A6Z1, G-A8Z, G-A9Z1 and G-A9Z2 respectively according to French standard NE A 02-004; it also relates to alloys having a composition corresponding to those of said basic commercial alloys to which calcium is added. It should be noted that these alloys contain Mn as an addition element.
  • the alloys used comprise, on a magnesium basis, from 0 to 11 atom% of aluminum, from 0 to 4 atom% of zinc and from 0.5 to 4 atom% of an addition element such as silicon, germanium, cobalt, tin or antimony.
  • Aluminum or zinc can also be replaced up to 4% by neodymium, praseodymium, yttrium, cerium or manganese.
  • the alloys thus obtained have a breaking load of the order of 414 to 482 MPa, an elongation of up to 5% and good resistance to corrosion by aqueous solutions containing 3% NaCl.
  • magnesium alloys with high mechanical strength, obtained by rapid solidification which contain, as alloying elements, from 0 to 15 atom% of aluminum, and from 0 to 4 atom% of zinc (with a total of both between 2 and 15%) and a complementary addition of 0.2 to 3 atom% of at least one element chosen from the group comprising Mn, Ce, Nd, Pr, Y , Ag.
  • This process requires the use of non-standard magnesium alloys comprising certain elements of addition of high price and often difficult solution, and grinding of the ribbons, obtained during rapid solidification, prior to the compaction.
  • a first object of the present invention relates to magnesium-based alloys, consolidated after rapid solidification, with high mechanical characteristics, having a breaking load at least equal to 290 MPa, but more particularly at least 330 MPa and an elongation at break at least equal to 5% and having, in combination, the following characteristics: - a weight composition located within the following limits: Aluminum 2-11% Zinc 0-12%, preferably 0.2 to 12% Manganese 0-0.6%, preferably 0.1 to 0.2% Calcium 0-7% but with at least the presence of Zn and / or Ca. with the following contents of main impurities: Silicon 0.1 to 0.6% Copper ⁇ 0.2% Iron ⁇ 0.1% Nickel ⁇ 0.1% the rest being magnesium.
  • the alloy must contain at least one of the elements Zn or Ca or a mixture of the two; when Zn is present, its content is preferably at least 0.2%.
  • Mn When Mn is present, it is an at least quaternary element and its minimum weight content is preferably 0.1%.
  • the added quantities by weight are between 0.5 and 7%. This addition then makes it possible to improve the characteristics of the alloys based on Mg, in particular those containing Al and / or Zn and / or Mn, obtained after rapid quenching and consolidation by spinning, including for a spinning temperature between 250 and 350 ° C.
  • the sum of the contents of Al, Zn and / or Ca does not usually exceed 20%.
  • a second object of the present invention is a process for obtaining these alloys characterized in that said alloy, in the liquid state is added to rapid cooling, at a speed at least equal to 104 Ks-l, so as to obtain a solidified product of which at least one of the dimensions is less than 150 mm, in that this solidified product is then compacted by spinning at a temperature between 200 and 350 ° C.
  • a characteristic of the invention is that it applies to magnesium alloys of the conventional type, normally intended for foundry (casting) or for working, without any additional addition of alloying element (s) intended to modify its structure as is the case in the prior art.
  • alloys of the types G-A3Z1, G-A6Z1, G-A8Z, G-A9Z1, G-A9Z2 (according to French standard NF A 02704), including the chemical composition intervals, were preferably used. have been given previously; they contain in particular additions of Mn.
  • Ca can also be added to it to improve their mechanical characteristics obtained during consolidation at a higher temperature.
  • the magnesium ribbons can either be directly introduced into the container of a press and spun, or pre-compacted cold or warm (temperature below, for example 250 ° C.), using a press, in the form of a billet whose density is close to 99% of the theoretical density of the alloy, this billet being subsequently spun, or introduced by cold pre-compacting them to 70% the theoretical density, in a sheath made of magnesium or magnesium alloy or aluminum or aluminum alloy, itself introduced into the container of the spinning press; it is then possible, after spinning, to remove the sheath by machining.
  • the sheath can be thin-walled (less than 1 mm) or thick (up to 4 mm). In all cases, it is preferable that the alloy constituting the sheath has a flow limit not exceeding the order of magnitude of that of the product to be spun, at the spinning temperature.
  • a rotating electrode is melted by an electron beam or an electric arc (atomization by rotating electrode), or a liquid jet is mechanically divided in contact with a rotating body and the fine droplets are projected onto a strongly cooled, renewed, or fixed surface, but kept clear, that is to say without adhesion of the solidified metal particles on said surface; the droplets can also be projected into a stream of inert gas, at low temperature (centrifugal atomization).
  • the parameters of the operation must be chosen so that at least one of the dimensions of the metal particles is less than 150 ⁇ m.
  • the alloy particles are obtained by atomization of liquid alloy in a jet of inert gas. This operation is also well known in itself and is not part of the invention. It makes it possible to provide particles of dimensions less than a hundred microns. These particles are generally spherical in shape, while those obtained in the previous variant are rather in the form of thin plates. The compaction of these particles is also carried out according to the same scheme as in the first and the second embodiment.
  • the products obtained can, before spinning, be degassed at a temperature not exceeding 350 ° C.
  • the procedure can be as follows: the ribbons are cold pre-compacted in a box and all placed in a vacuum oven. The box is vacuum sealed and then spun. But degassing can also be done dynamically: the divided products are degassed and then compacted under vacuum in the form of a billet with closed porosities which is then spun.
  • Table II gives the characteristics of alloys of equivalent compositions, obtained in a conventional manner: TABLE II Test No. Alloy type (1) Method of obtaining Hv kg / mm2 TYS (0.2) MPa UTS MPa e% 14 AZ 31 Gross spinning 170 250 5
  • AZ31 has 2.5-3.5% Al and 0.5-1.5% Zn, and AZ91 8.3-10.3% Al and 0.2-1% Zn as main elements, and 0.15% from Mn.
  • the hardness, the elastic limit and the breaking load very strongly depend on the spinning conditions.
  • Table III brings together a certain number of mechanical characteristics of products in AZ91 alloys solidified quickly then compacted by spinning, according to the invention. The parameters were varied: spinning ratio (from 12 to 30), temperature and spinning speed (resp. 200-350 ° C and 0.5-3 mm / s). TABLE III Mechanical characteristics of the AZ91 treated according to the invention T. Wire ° C R. Wire V Wire. mm / sec Hardness Hv kg / mm2 Elast.limit. Charge rupt. UTS, MPa All.
  • the mechanical characteristics decrease when the spinning temperature increases, that the hardness increases when the spinning ratio increases to reach a plateau, more or less quickly, depending on the temperature.
  • a spinning ratio 20.
  • the elastic limit CYS in compression is at least equal (and sometimes higher) to the elastic limit in tension, which is quite exceptional since the same alloys, in classical transformation, have a limit in compression about 0.7 times the tensile limit. This means that, in the design of parts added to compressive stresses, the alloys according to the invention will bring a significant gain of around 30%.
  • the remarkable mechanical properties of the alloys according to the invention are essentially due to the fact that the process used leads to a very fine grain structure, of the order of a micrometer (0.7 to 1.5 on average).
  • the optical microscope does not make it possible to resolve the structure and it is only by electron microscopy that it can be verified that the products according to the invention are in fact constituted by a homogeneous matrix reinforced by particles of intermetallic compounds Mg17Al12 of size less than 0.5 mum, precipitated at the grain boundaries and also of Al2Ca, under certain conditions mentioned above.
  • the presence, in the grains, of precipitates ⁇ 0.2 mum of compound based on Al Mn Zn is also noted.
  • the general structure is granular equiaxed.
  • the precipitates do not have the same morphology as the structural hardening precipitates observed on samples of the same alloys obtained by conventional metallurgy.
  • This structure also has remarkable thermal stability, since it remains unchanged after 24 hours of holding at 200 ° C for alloys containing no Ca and up to 350 ° C for those containing it. No softening or hardening is manifested, which is not the case for conventional magnesium alloys with structural hardening.
  • the corrosion resistance is evaluated by a measurement of weight loss in an aqueous solution at 5% (by weight) of NaCl, the result of which is expressed in "mcd" (milligrams per square centimeter per day).
  • the tests carried out on a set of products according to the invention give results of between 0.4 and 0.6 while the same alloys, transformed into conventional metallurgy, give results of between 0.6 and 2 mcd. It can therefore be said that the corrosion resistance of the alloys according to the invention is at least equal to that of conventional alloys, and is in fact placed at the level of the resistance of high purity alloys, such as AZ91E produced by the Company DOW CHEMICAL. It is found that the alloys according to the invention generally exhibit corrosion without pitting and more homogeneous than that of said AZ91E alloys.
  • the presence of Ca further improves the resistance to corrosion; it becomes very slow and extremely homogeneous.
  • the weight loss is 0.075 mg / cm2.day while for an AZ91 without calcium in test 4 it is 0.4 mg / cm2.day.

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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)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)
  • Forging (AREA)
  • Extrusion Of Metal (AREA)

Claims (13)

  1. Legierung auf Magnesiumbasis, erhalten durch rasche Erstarrung und Verfestigung, mit einer Bruchfestigkeit von mindestens 290 MPa, einer Bruchdehnung von mindestens 5 % und der Kombination der folgenden Elemente:
    Sie hat eine in den folgenden Grenzen liegende Gewichtszusammensetzung:
    - Aluminium: 2 - 11 %
    - Zink: 0 - 12 %
    - Mangan: 0 - 0,6 %
    - Calcium: 0 - 7 %,
    aber mit mindestens der Anwesenheit von Zn und/oder Ca,
    mit den folgenden Gehalten an Hauptverunreinigungen:
    - Silizium: 0,1 - 0,6 %
    - Kupfer: < 0,2 %
    - Eisen: < 0,1 %
    - Nickel: < 0,01 %
    Rest Magenesium;
    sie hat eine mittlere Kornabmessung unter 3 µm;
    sie besteht aus einer homogenen Matrix, die durch Teilchen intermetallischer Verbindungen Mg₁₇Al₁₂, die an den Korngrenzen ausgeschieden sind, eventuell Mg₃₂ (Al, Zn)₄₉ und Al₂Ca einer mittleren Größe unter 1 µm verstärkt ist, welches Gefüge nach Halten von 24 Stunden bei 200 °C unverändert bleibt;
    und im Fall, wo sie kein Ca enthält, wird die Verfestigung durch Strangpressen bei einer Temperatur im Bereich von 200 bis 350 °C mit einem Reduktionsverhältnis im Bereich von 10 bis 40 und einer Vorrückgeschwindigkeit des Kolbens von 0,5 bis 3 mm/s durchgeführt.
  2. Legierung nach dem Anspruch 1,
    dadurch gekennzeichnet,
    daß die Teilchen intermetallischer Verbindungen eine mittlere Größe unter 0,5 µm haben.
  3. Legierung nach irgendeinem der Ansprüche 1 oder 2,
    dadurch gekennzeichnet,
    daß der Gehalt an Zn zwischen 0,2 und 12 Gew.% und der Gehalt an Mn zwischen 0,1 und 0,6 Gew.% liegen.
  4. Legierung nach irgendeinem der Ansprüche 1 oder 2,
    dadurch gekennzeichnet,
    daß der Gehalt an Ca zwischen 0,5 und 7 Gew.% liegt.
  5. Verfahren zur Herstellung einer Legierung nach den Ansprüchen 1 bis 4,
    dadurch gekennzeichnet,
    daß die Legierung im flüssigen Zustand einer raschen Abkühlung mit einer Geschwindigkeit von mindestens 10⁴·K·s⁻¹ derart ausgesetzt wird, um ein erstarrtes Produkt zu erhalten, dessen wenigstens eine der Abmessungen unter 150 µm ist und das dann durch Strangpressen bei einer Temperatur im Bereich von 200 bis 350 °C direkt kompaktiert wird.
  6. Verfahren nach Anspruch 5,
    dadurch gekennzeichnet,
    daß die rasche Abkühlung durch Gießen eines Endlosbandes einer Dicke unter 150 µm auf eine stark gekühlte bewegliche Oberfläche bewirkt wird.
  7. Verfahren nach Anspruch 5,
    dadurch gekennzeichnet,
    daß die rasche Abkühlung durch Zerstäuben der flüssigen Legierung auf eine freigehaltene stark gekühlte Oberfläche bewirkt wird.
  8. Verfahren nach Anspruch 5,
    dadurch gekennzeichnet,
    daß die rasche Abkühlung durch Versprühen der flüssigen Legierung mittels eines Inertgasstrahls bewirkt wird.
  9. Verfahren nach irgendeinem der Ansprüche 5 bis 8,
    dadurch gekennzeichnet,
    daß das rasch erstarrte Produkt, wenn es Calcium enthält, durch Strangpressen in der Presse bei einer Temperatur im Bereich von 200 bis 350 °C mit einem Strangpreßverhältnis von 10 bis 40 und vorzugsweise von 10 bis 20 und mit einer Vorrückgeschwindigkeit des Stempels der Presse von 0,5 bis 3 mm je Sekunde kompaktiert wird.
  10. Verfahren nach irgendeinem der Ansprüche 5 bis 9,
    dadurch gekennzeichnet,
    daß das rasch abgekühlte Produkt direkt in den Preßtopf der Strangpresse eingeführt wird.
  11. Verfahren nach irgendeinem der Ansprüche 5 bis 9,
    dadurch gekennzeichnet,
    daß das rasch abgekühlte Produkt vorab in eine aus Aluminium, aus Magnesium oder aus einer Legierung auf Basis des einen oder anderen dieser beiden Metalle bestehende Metallhülle eingeführt wird.
  12. Verfahren nach irgendeinem der Ansprüche 5 bis 11,
    dadurch gekennzeichnet,
    daß das rasch erstarrte Produkt vorab in Form eines Barrens bei einer Temperatur von höchstens 200 °C vorkompaktiert wird.
  13. Verfahren nach irgendeinem der Ansprüche 5 bis 12,
    dadurch gekennzeichnet,
    daß das rasch abgekühlte Produkt unter Vakuum bei einer Temperatur unter oder gleich 350 °C vor der Verfestigung entgast wird.
EP89903172A 1988-02-26 1989-02-23 Hochfeste magnesiumlegierungen und verfahren, um derartige legierungen mittels rascher erstarrung zu erhalten Expired - Lifetime EP0357743B1 (de)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
FR8802885A FR2627780B1 (fr) 1988-02-26 1988-02-26 Alliages de magnesium a haute resistance mecanique et procede d'obtention de ces alliages par solidification rapide
FR8802885 1988-02-26
FR8901913 1989-02-01
FR898901913A FR2642439B2 (de) 1988-02-26 1989-02-01

Publications (2)

Publication Number Publication Date
EP0357743A1 EP0357743A1 (de) 1990-03-14
EP0357743B1 true EP0357743B1 (de) 1993-09-29

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EP89903172A Expired - Lifetime EP0357743B1 (de) 1988-02-26 1989-02-23 Hochfeste magnesiumlegierungen und verfahren, um derartige legierungen mittels rascher erstarrung zu erhalten

Country Status (6)

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US (1) US4997622A (de)
EP (1) EP0357743B1 (de)
JP (1) JPH02503331A (de)
DE (1) DE68909544T2 (de)
FR (1) FR2642439B2 (de)
WO (1) WO1989008154A1 (de)

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US4997622A (en) 1991-03-05
WO1989008154A1 (fr) 1989-09-08
DE68909544T2 (de) 1994-01-27
JPH02503331A (ja) 1990-10-11
DE68909544D1 (de) 1993-11-04
FR2642439A2 (de) 1990-08-03
FR2642439B2 (de) 1993-04-16
EP0357743A1 (de) 1990-03-14

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