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EP1252352B1 - Method for providing magnesium alloys with superplastic properties - Google Patents

Method for providing magnesium alloys with superplastic properties Download PDF

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Publication number
EP1252352B1
EP1252352B1 EP01909511A EP01909511A EP1252352B1 EP 1252352 B1 EP1252352 B1 EP 1252352B1 EP 01909511 A EP01909511 A EP 01909511A EP 01909511 A EP01909511 A EP 01909511A EP 1252352 B1 EP1252352 B1 EP 1252352B1
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Prior art keywords
temperature
alloy
magnesium
superplastic
hours
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German (de)
French (fr)
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EP1252352A2 (en
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Ulrich Draugelates
Antonia Schram
Claus-Christian Kedenburg
Talant Ryspaev
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Technische Universitaet Clausthal
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Technische Universitaet Clausthal
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Priority claimed from DE2000103970 external-priority patent/DE10003970B4/en
Priority claimed from DE2000111334 external-priority patent/DE10011334A1/en
Application filed by Technische Universitaet Clausthal filed Critical Technische Universitaet Clausthal
Priority to EP03011735A priority Critical patent/EP1342805A3/en
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    • 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
    • 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
    • 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
    • C21D2201/02—Superplasticity

Definitions

  • the present invention relates to a method for producing magnesium alloys with a superplastic structure.
  • Superplasticity means the ability of a material to Application of very low yield stresses without constrictions and practical no strain hardening to achieve degrees of deformation that the "normal plastic" Materials usual limits of about 10 to 40% by some 100 exceed over 1000%. Another characteristic of superplastic behavior of materials is the strong dependence of the yield stress on the Strain rate.
  • JP61250144A discloses a heat treatment of a cast Mg alloy to to improve the creep properties at high temperatures. According to JP61250144A, the cast parts heated at a temperature of 530 ° C for 4 hours, in water cooled, heated to 200 ° C for 20 hours and then cooled in air.
  • a disadvantage of the above processes is the fact that the alloys in each case have to be heated to above the melting temperature, and that the alloys the superplastic properties each by a very complex process (machining / sintering, melting, alloying) become, which particularly complicates their handling in industrial processes.
  • the object of the present invention is to provide a method provide a structure with that in conventional magnesium-based alloys superplastic properties can be produced inexpensively.
  • the procedure should be independent of commonly used shielding gas technologies applicable and easy to integrate into existing production.
  • the base alloy initially becomes slow, preferably at a heating rate from 0.1 to 3.0 ° C / min, more preferably 0.2 to 1.0 ° C / min and especially 0.4 to 0.6 ° C / min to a temperature of 300 to 550 ° C, more preferably 350 to 450 ° C and in particular 390 to 420 ° C heated and 1 to 100 hours, preferably 10 to 35 hours and in particular 18 to 24 hours in this Temperature maintained.
  • the heated alloy is then, preferably in air or in water to a temperature of 0 to 100 ° C, preferably 15 to 50 ° C and especially cooled to ambient temperature.
  • the cooled alloy is then brought to a temperature from 200 to 400 ° C, preferably 220 to 350 ° C and in particular 250 reheated to 310 ° C and 1 to 100 hours, preferably 10 to 35 Hours and in particular 18 to 24 hours at this temperature.
  • the alloy thus reheated is then, preferably in air or in Water to a temperature of 0 to 100 ° C, preferably 15 to 50 ° C and especially cooled to ambient temperature.
  • Preferred magnesium-based alloys for processing in the invention In addition to magnesium, processes contain aluminum, zinc, manganese, silicon, Copper, zirconium, silver and / or rare earth metals. Particularly preferred Alloys are alloys that contain zinc, zirconium and rare earth metals contain, in particular those which in addition to magnesium essentially these elements. Preferred rare earth metals are neodymium, thorium and yttrium.
  • Examples of usable magnesium base alloys are alloys from Type AM 20, AM 50, AM 60, AS 41, AS 21, AE 42, AZ 91, EZ 33, AZ 31, QE 22, QH 21, WE 54, ZC 63 and ZRE 1.
  • the alloy preheated according to the invention becomes a conventional forming process subjected to convert the alloy into a semi-finished product.
  • preferred Forming processes are pressure forming processes such as that Extrusion, rolling or forging. Extrusion is particularly preferred.
  • the magnesium alloy is preferably formed by extrusion with a compression ratio greater than 1:15, more preferred from 1:15 to 1: 100, in particular 1:25 to 1:50 at a bolt temperature and a recipient temperature of 200 to 600 ° C, more preferably 300 up to 400 ° C instead.
  • the shaping takes place the cooled alloy by extrusion at a bolt temperature and a recipient temperature of 270 to 400 ° C, more preferably 330 to 370 ° C instead.
  • the magnesium-based alloys reach the cast state according to the manufacturer's instructions an elongation at break of up to 12%.
  • the by the invention Process changed to an improved superplastic formability Magnesium-based alloys, on the other hand, achieve tensile tests on one Temperature of 380 ° C and a constant forming speed of 0.05 mm / min. an elongation at break of up to 780%.
  • the drawing shows an undeformed (a), one under the above conditions deformed tensile test of an untreated ZRE1 magnesium base alloy (b) and a tensile specimen deformed superplastically under the above conditions a ZRE1 magnesium base alloy produced according to the example according to the invention (C).

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  • 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)
  • Powder Metallurgy (AREA)
  • Extrusion Of Metal (AREA)
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Abstract

Production of magnesium alloys having a superplastic structure comprises heating a magnesium-based alloy to 250-600 degrees C; deforming to a semi-finished product at 250-450 degrees C; and rapidly cooling at a speed of more than 300 degrees C/minute.

Description

Die vorliegende Erfindung betrifft ein Verfahren zur Herstellung von Magnesiumlegierungen mit einer superplastischen Gefügestruktur.The present invention relates to a method for producing magnesium alloys with a superplastic structure.

Durch Nutzung des superplastischen Verhaltens von Werkstoffen kann die Produktivität bei der Weiterverarbeitung von Halbzeugen zu komplexgeformten Fertigbauteilen gegenüber konventionellen Umformverfahren wesentlich erhöht werden. Insbesondere bei der Herstellung endabmessungsgenauer Bauteile, die alternativ nur durch aufwendige Zerspan- oder Fügeprozesse hergestellt werden können, stellt die superplastische Formgebung von Metallen und deren Legierungen ein kostengünstiges Fertigungsverfahren dar.By using the superplastic behavior of materials, the Productivity in the processing of semi-finished products into complex-shaped ones Prefabricated parts significantly increased compared to conventional forming processes become. Particularly in the manufacture of components with precise dimensions alternatively, they can only be produced by complex machining or joining processes can, the superplastic shaping of metals and their Alloys represent an inexpensive manufacturing process.

Der steigende Bedarf an hoch beanspruchbaren, kostengünstig zu fertigenden Produkten hat in den letzten Jahren mit fortschreitendem Zwang zur Leichtbauweise und der damit verbundenen Material- und Energieeinsparung vor allem in den Bereichen der Luft- und Raumfahrt, des Hochgeschwindigkeitsschienenverkehrs, des Automobil- und Gerätebaus, aber auch in der Nachrichten- und Datenverarbeitungstechnik ein wachsendes Interesse an der superplastischen Formgebung hervorgerufen. Eine Ursache hierfür ist die besondere Eignung dieses Fertigungsverfahrens, möglichst dünnwandige Strukturbauteile für den Leichtbau herzustellen.The increasing need for heavy-duty, inexpensive to manufacture Products has become increasingly lightweight in the past few years and the associated material and energy savings above all in the fields of aerospace, high-speed rail transport, of automotive and device construction, but also in the news and data processing technology a growing interest in the superplastic Shape caused. One reason for this is the special one Suitability of this manufacturing process, as thin-walled structural components as possible for lightweight construction.

Während umfassende Untersuchungen über das superplastische Verhalten von Zweiphasenstählen, Titan- und Aluminiumlegierungen durchgeführt wurden, liegen über das superplastische Verhalten von Magnesiumlegierungen, die aufgrund ihrer gegenüber Aluminiumwerkstoffen um etwa 50% geringeren Dichte einen weiteren entscheidenden Beitrag zur Gewichtsreduzierung im Leichtbau leisten können, nur wenig grundlegende Erkenntnisse vor. Die Nutzung der superplastischen Eigenschaften ist jedoch gerade für die Werkstoffgruppe der Magnesiumlegierungen aufgrund ihrer eingeschränkten Kaltformbarkeit wünschenswert.During extensive studies on the superplastic behavior of Two-phase steels, titanium and aluminum alloys were carried out, lie about the superplastic behavior of magnesium alloys due to their density, which is about 50% lower than that of aluminum materials another decisive contribution to reducing weight in lightweight construction can afford little basic knowledge. The use of the However, superplastic properties are especially important for the material group Magnesium alloys desirable due to their limited cold formability.

Unter Superplastizität wird die Fähigkeit eines Werkstoffes verstanden, beim Aufbringen nur sehr geringer Fließspannungen ohne Einschnürungen und praktisch keiner Kaltverfestigung Umformgrade zu erzielen, die die bei "normalplastischen" Werkstoffen üblichen Grenzen von etwa 10 bis 40% um einige 100 bis über 1000% übersteigen. Ein weiteres Merkmal des superplastischen Verhaltens von Werkstoffen ist die starke Abhängigkeit der Fließspannung von der Dehngeschwindigkeit.Superplasticity means the ability of a material to Application of very low yield stresses without constrictions and practical no strain hardening to achieve degrees of deformation that the "normal plastic" Materials usual limits of about 10 to 40% by some 100 exceed over 1000%. Another characteristic of superplastic behavior of materials is the strong dependence of the yield stress on the Strain rate.

JP61250144A offenbart eine Wärmebehandlung einer gegossenen Mg-Legierung, um die Kriecheigenschaften bei Hochtemperaturen zu verbessern. Nach JP61250144A werden die gegossenen Teile bei einer Temperatur von 530°C für 4 Stunden erwärmt, in Wasser abgekühlt, auf 200°C für 20 Stunden erwärmt und anschließend in Luft abgekühlt.JP61250144A discloses a heat treatment of a cast Mg alloy to to improve the creep properties at high temperatures. According to JP61250144A, the cast parts heated at a temperature of 530 ° C for 4 hours, in water cooled, heated to 200 ° C for 20 hours and then cooled in air.

C. G. Nieh und J. Wadsworth, Scripta Metallurgica et Materialia, Band 32 (1995), Heft 8, Seiten 1133-1137, beschreiben die Herstellung von 17 Vol% SiC-partikelverstärkten ZK60-Mg-Verbundwerkstoffen durch pulvermetallurgische Verfahren. Das Vorhandensein der feinen SiC-Partikel in ZK60 kann danach scheinbar die Mikrostruktur des Verbundwerkstoffes bei hohen Temperaturen (450°C) verfeinern und stabilisieren und ist somit verantwortlich für die Verleihung der Superplastizität.C. G. Nieh and J. Wadsworth, Scripta Metallurgica et Materialia, volume 32 (1995), Issue 8, pages 1133-1137, describe the production of 17 vol% SiC particle-reinforced ZK60-Mg composites through powder metallurgical Method. The presence of the fine SiC particles in ZK60 can then apparently the microstructure of the composite at high temperatures (450 ° C) refine and stabilize and is therefore responsible for the Awarding superplasticity.

M. Mabuchi, K. Kubota und K. Higashi, Scripta Metallurgica et Materialia, Band 33 (1995), Heft 2, Seiten 331-335, beschreiben die Herstellung einer Mg-11Si-4A1-Legierung mit einer superplastischen Gefügestruktur durch Strangpressen von "schnellerstarrten" Bändern.M. Mabuchi, K. Kubota and K. Higashi, Scripta Metallurgica et Materialia, Volume 33 (1995), No. 2, pages 331-335, describe the preparation of a Mg-11Si-4A1 alloy with a superplastic structure Extrusion of "faster solid" belts.

M. Mabuchi, K. Kubota und K. Higashi, Material Transactions, JIM, Vol. 36 (10) (1995) 1249-1254, beschreiben die Herstellung von superplastischen AZ91-Magnesiumlegierungen aus maschinell gefertigten Spänen. Die Späne werden durch maschinelle Bearbeitung eines kommerziellen Gussblocks einer AZ91-Legierung in einer Drehbank hergestellt und anschließend stranggepresst. So kann bei dieser Legierung bei einer Umformtemperatur von 573 K und einer Dehnrate von 3,3 10-4s-1 eine Dehnung von 980% erzielt werden. K.U.Kainer, Metall Powder Report 44 (1990), 684-687, beschreibt die Herstellung von Magnesiumlegierungen mit einer superplastischen Gefügestruktur durch pulvermetallurgische Verfahren.M. Mabuchi, K. Kubota and K. Higashi, Material Transactions, JIM, Vol. 36 (10) (1995) 1249-1254, describe the production of superplastic AZ91 magnesium alloys from machined chips. The chips are machined from a commercial AZ91 alloy ingot in a lathe and then extruded. With this alloy, an elongation of 980% can be achieved at a forming temperature of 573 K and an elongation rate of 3.3 10 -4 s -1 . KUKainer, Metall Powder Report 44 (1990), 684-687, describes the production of magnesium alloys with a superplastic structure by powder metallurgical processes.

J. Wolfenstine, G. Gonzalez-Doncel und K. Higashi, Superplasticity and Superplastic Forming (Ed. A.K. Ghosh und T.R. Bieler), 1995, Seiten 75-82, beschreiben die Herstellung von Magnesium-Lithium-Legierungen mit einer superplastischen Gefügestruktur durch Vakuumformen und Heißwalzen. So kann bei dieser Legierung bei einer Umformtemperatur von 350°C und einer Dehnrate von 4 X 10-4s-1 eine relative Dehnung von 610% erzielt werden.J. Wolfenstine, G. Gonzalez-Doncel and K. Higashi, Superplasticity and Superplastic Forming (Ed. AK Ghosh and TR Bieler), 1995, pages 75-82, describe the production of magnesium-lithium alloys with a superplastic structure by vacuum forming and hot rolling. A relative elongation of 610% can be achieved with this alloy at a forming temperature of 350 ° C and an elongation rate of 4 X 10 -4 s -1 .

J.K. Solberg, J. Torklep, O. Bauger und H. Gjestland, Mater, Sci.Engng. A134 (1991), 1201-1203, beschreiben schließlich die Herstellung einer superplastischen AZ91-Magnesiumlegierung durch extrem rasche Erstarrung aus dem schmelzflüssigen Zustand. Die Legierung zeigte eine relative Dehnung von 1480% bei 573 K.J.K. Solberg, J. Torklep, O. Bauger and H. Gjestland, Mater, Sci.Engng. A134 (1991), 1201-1203, finally describe the production of a superplastic AZ91 magnesium alloy due to extremely rapid solidification from the molten state. The alloy showed a relative elongation of 1480% at 573 K.

Nachteilig bei den obigen Verfahren ist die Tatsache, dass die Legierungen jeweils auf oberhalb der Schmelztemperatur erwärmt werden müssen, und dass den Legierungen die superplastischen Eigenschaften jeweils durch einen sehr aufwendigen Prozess (Zerspanung / Sintern, Aufschmelzen, Legieren) verliehen werden, was insbesondere ihre Handhabung in industriellen Verfahren erschwert.A disadvantage of the above processes is the fact that the alloys in each case have to be heated to above the melting temperature, and that the alloys the superplastic properties each by a very complex process (machining / sintering, melting, alloying) become, which particularly complicates their handling in industrial processes.

Aufgabe der vorliegenden Erfindung ist es, ein Verfahren zur Verfügung zu stellen, mit dem in konventionellen Magnesiumbasislegierungen ein Gefüge mit superplastischen Eigenschaften kostengünstig erzeugt werden kann. Das Verfahren soll unabhängig von üblicherweise verwendeten Schutzgastechniken anwendbar und einfach in die bestehende Fertigung integrierbar sein.The object of the present invention is to provide a method provide a structure with that in conventional magnesium-based alloys superplastic properties can be produced inexpensively. The procedure should be independent of commonly used shielding gas technologies applicable and easy to integrate into existing production.

Zur Lösung der Aufgabe, das Verfahren insbesondere unabhängig von üblicherweise verwendeten Schutzgastechniken anwendbar zu machen, wird erfindungsgemäß ein Verfahren zur Herstellung von Magnesiumlegierungen mit einer superplastischen Gefügestruktur vorgeschlagen, das folgende Schritte umfasst:

  • a) Erwärmung einer Magnesiumbasislegierung auf eine Temperatur von 300 bis 550°C und Halten dieser Temperatur für 1 bis 100 Stunden,
  • b) Abkühlung der erwärmten Legierung auf eine Temperatur von 0 bis 100°C,
  • c) Wiedererwärmung der abgekühlten Legierung auf eine Temperatur von 200 bis 400°C und Halten dieser Temperatur für 1 bis 100 Stunden,
  • d) Abkühlung der wiedererwärmten Legierung an Luft auf eine Temperatur von 0 bis 100°C,
  • e) Umformen der abgekühlten Legierung zu einem Halbzeug bei einer Temperatur von 250 bis 450°C.
    • To solve the problem of making the method applicable, in particular, independently of the protective gas techniques commonly used, the invention proposes a method for producing magnesium alloys with a superplastic structure, which comprises the following steps:
  • a) heating a magnesium-based alloy to a temperature of 300 to 550 ° C. and maintaining this temperature for 1 to 100 hours,
  • b) cooling the heated alloy to a temperature of 0 to 100 ° C,
  • c) reheating the cooled alloy to a temperature of 200 to 400 ° C and maintaining this temperature for 1 to 100 hours,
  • d) cooling the reheated alloy in air to a temperature of 0 to 100 ° C,
  • e) Forming the cooled alloy into a semi-finished product at a temperature of 250 to 450 ° C.

    • Die Basislegierung wird zunächst langsam, vorzugsweise mit einer Heizrate von 0,1 bis 3,0°C/min, bevorzugter 0,2 bis 1,0°C/min und insbesondere 0,4 bis 0,6°C/min auf eine Temperatur von 300 bis 550°C, bevorzugter 350 bis 450°C und insbesondere 390 bis 420°C erwärmt und 1 bis 100 Stunden, vorzugsweise 10 bis 35 Stunden und insbesondere 18 bis 24 Stunden bei dieser Temperatur gehalten. Die erwärmte Legierung wird anschließend, vorzugsweise an Luft oder in Wasser auf eine Temperatur von 0 bis 100°C, vorzugsweise 15 bis 50°C und insbesondere auf Umgebungstemperatur abgekühlt.The base alloy initially becomes slow, preferably at a heating rate from 0.1 to 3.0 ° C / min, more preferably 0.2 to 1.0 ° C / min and especially 0.4 to 0.6 ° C / min to a temperature of 300 to 550 ° C, more preferably 350 to 450 ° C and in particular 390 to 420 ° C heated and 1 to 100 hours, preferably 10 to 35 hours and in particular 18 to 24 hours in this Temperature maintained. The heated alloy is then, preferably in air or in water to a temperature of 0 to 100 ° C, preferably 15 to 50 ° C and especially cooled to ambient temperature.

    In einem weiteren Schritt wird die abgekühlte Legierung dann auf eine Temperatur von 200 bis 400°C, vorzugsweise 220 bis 350°C und insbesondere 250 bis 310°C wiedererwärmt und 1 bis 100 Stunden, vorzugsweise 10 bis 35 Stunden und insbesondere 18 bis 24 Stunden bei dieser Temperatur gehalten. Die so wiedererwärmte Legierung wird danach, vorzugsweise an Luft oder in Wasser auf eine Temperatur von 0 bis 100°C, vorzugsweise 15 bis 50°C und insbesondere auf Umgebungstemperatur abgekühlt.In a further step, the cooled alloy is then brought to a temperature from 200 to 400 ° C, preferably 220 to 350 ° C and in particular 250 reheated to 310 ° C and 1 to 100 hours, preferably 10 to 35 Hours and in particular 18 to 24 hours at this temperature. The alloy thus reheated is then, preferably in air or in Water to a temperature of 0 to 100 ° C, preferably 15 to 50 ° C and especially cooled to ambient temperature.

    Bevorzugte Magnesiumbasislegierungen zur Verarbeitung im erfindungsgemäßen Verfahren enthalten neben Magnesium Aluminium, Zink, Mangan, Silicium, Kupfer, Zirkonium, Silber und/oder Seltenerdmetalle. Besonders bevorzugte Legierungen sind Legierungen, die Zink, Zirkonium und Seltenerdmetalle enthalten, insbesondere solche, die neben Magnesium im Wesentlichen aus diesen Elementen bestehen. Bevorzugte Seltenerdmetalle sind Neodym, Thorium und Yttrium.Preferred magnesium-based alloys for processing in the invention In addition to magnesium, processes contain aluminum, zinc, manganese, silicon, Copper, zirconium, silver and / or rare earth metals. Particularly preferred Alloys are alloys that contain zinc, zirconium and rare earth metals contain, in particular those which in addition to magnesium essentially these elements. Preferred rare earth metals are neodymium, thorium and yttrium.

    Beispiele für verwendbare Magnesiumbasislegierungen sind Legierungen vom Typ AM 20, AM 50, AM 60, AS 41, AS 21, AE 42, AZ 91, EZ 33, AZ 31, QE 22, QH 21, WE 54, ZC 63 und ZRE 1.Examples of usable magnesium base alloys are alloys from Type AM 20, AM 50, AM 60, AS 41, AS 21, AE 42, AZ 91, EZ 33, AZ 31, QE 22, QH 21, WE 54, ZC 63 and ZRE 1.

    Die erfindungsgemäß vorgewärmte Legierung wird konventionellen Umformverfahren unterworfen, um die Legierung in ein Halbzeug umzuwandeln. Bevorzugte Umformverfahren sind Druckumformverfahren wie beispielsweise das Strangpressen, Walzen oder Schmieden. Besonders bevorzugt ist das Strangpressen. The alloy preheated according to the invention becomes a conventional forming process subjected to convert the alloy into a semi-finished product. preferred Forming processes are pressure forming processes such as that Extrusion, rolling or forging. Extrusion is particularly preferred.

    Das Umformen der Magnesiumlegierung durch Strangpressen findet vorzugsweise mit einem Verpressungsverhältnis von größer als 1 : 15, bevorzugter von 1 : 15 bis 1 : 100, insbesondere 1 : 25 bis 1 : 50 bei einer Bolzentemperatur und einer Rezipiententemperatur von 200 bis 600°C, bevorzugter 300 bis 400°C statt. Bei dem Verfahren gemäß Anspruch 4 erfolgt das Umformen der abgekühlten Legierung durch Strangpressen bei einer Bolzentemperatur und einer Rezipiententemperatur von 270 bis 400°C, bevorzugter 330 bis 370°C statt.The magnesium alloy is preferably formed by extrusion with a compression ratio greater than 1:15, more preferred from 1:15 to 1: 100, in particular 1:25 to 1:50 at a bolt temperature and a recipient temperature of 200 to 600 ° C, more preferably 300 up to 400 ° C instead. In the method according to claim 4, the shaping takes place the cooled alloy by extrusion at a bolt temperature and a recipient temperature of 270 to 400 ° C, more preferably 330 to 370 ° C instead.

    Ohne sich an eine bestimmte Theorie binden zu wollen, wird vermutet, dass durch die oben genannte Wärmebehandlung unterhalb des Schmelzpunktes der Legierung feinverteilte Ausscheidungen im Mikrogefüge erzeugt werden, welche sich beim Umformen an den Korngrenzen anlagern und dort das für die superplastische Verformung charakteristische Korngrenzengleiten unterstützen. Zudem wirken wahrscheinlich durch die Wärmebehandlung der unterschiedlichen Magnesiumbasislegierungen erzeugten Ausscheidungen (Mg17Al12, Zr2Zn3, Mg32(Al,Zn)49, Mg9SE) als Kristallisationskeime bei der Sekundärkristallisation des Gefüges während des Umformens.Without wishing to be bound by any particular theory, it is suspected that the heat treatment mentioned below produces fine-grained precipitates in the microstructure below the melting point of the alloy, which accumulate at the grain boundaries during forming and support the grain boundary sliding characteristic of superplastic deformation. In addition, precipitates (Mg 17 Al 12 , Zr 2 Zn 3 , Mg 32 (Al, Zn) 49 , Mg 9 SE) produced by the heat treatment of the different magnesium-based alloys probably act as crystallization nuclei in the secondary crystallization of the structure during the forming.

    Die Magnesiumbasislegierungen erreichen im Gusszustand nach Herstellerangaben eine Bruchdehnung von bis zu 12%. Die durch das erfindungsgemäße Verfahren auf ein verbessertes superplastisches Umformvermögen veränderten Magnesiumbasislegierungen hingegen erreichen bei Zugversuchen bei einer Temperatur von 380°C und einer konstanten Umformgeschwindigkeit von 0,05 mm/min. eine Bruchdehnung von bis zu 780%.The magnesium-based alloys reach the cast state according to the manufacturer's instructions an elongation at break of up to 12%. The by the invention Process changed to an improved superplastic formability Magnesium-based alloys, on the other hand, achieve tensile tests on one Temperature of 380 ° C and a constant forming speed of 0.05 mm / min. an elongation at break of up to 780%.

    Die Zeichnung zeigt eine unverformte (a), eine bei den obigen Bedingungen verformte Zugprobe einer unbehandelten ZRE1-Magnesiumbasislegierung (b) sowie eine bei den obigen Bedingungen superplastisch verformte Zugprobe einer gemäß Beispiel erfindungsgemäß hergestellten ZRE1-Magnesiumbasislegierung (c). The drawing shows an undeformed (a), one under the above conditions deformed tensile test of an untreated ZRE1 magnesium base alloy (b) and a tensile specimen deformed superplastically under the above conditions a ZRE1 magnesium base alloy produced according to the example according to the invention (C).

    Beispiel:Example: Herstellung einer ZRE1-Magnesiumbasislegierung mit superplastischer GefügestrukturProduction of a ZRE1 magnesium base alloy with superplastic structure

    Eine kommerziell erhältliche ZRE1-Magnesiumbasislegierung wurde mit einer Heizrate von 0,5°C/min langsam auf 415°C erwärmt und 20 Stunden bei dieser Temperatur gehalten. Anschließend wurde die Probe an Luft auf Umgebungstemperatur abgekühlt. Die abgekühlte Probe wurde anschließend durch Erwärmen auf 300°C und Halten der Probe bei dieser Temperatur für 20 Stunden überaltert. Daraufhin wurde die überalterte Probe an Luft auf Umgebungstemperatur wieder abgekühlt. Die Probe wurde mit einem Verpressungsverhältnis von 1 : 29 bei einer Bolzentemperatur und Rezipiententemperatur von 350°C durch Strangpressen verformt. Es wurde gefunden, dass ihre Mikrostruktur auf einer Korngröße von d = 10 µm gefeint war. Die Basislegierung erreicht im Gusszustand nach Herstellerangaben eine Bruchdehnung von 3%. Die durch das erfindungsgemäße Verfahren bearbeitete Magnesiumlegierung hingegen erreichte bei Zugversuchen bei einer Temperatur von 380°C und einer Umformgeschwindigkeit von 0,05 mm/min eine Bruchdehnung von 780% (siehe Zeichnung).A commercially available ZRE1 magnesium base alloy was used with a Heating rate of 0.5 ° C / min slowly heated to 415 ° C and 20 hours at this Temperature maintained. The sample was then exposed to ambient temperature in air cooled. The cooled sample was then run through Warm to 300 ° C and hold the sample at this temperature for 20 hours out of date. The aged sample was then exposed to ambient temperature in air cooled down again. The sample was made with a compression ratio of 1:29 at a bolt temperature and recipient temperature of 350 ° C deformed by extrusion. It was found that their Microstructure was fine-tuned to a grain size of d = 10 microns. The base alloy achieves an elongation at break of 3%. The magnesium alloy processed by the method according to the invention however, reached in tensile tests at a temperature of 380 ° C and a forming speed of 0.05 mm / min an elongation at break of 780% (see drawing).

    Claims (9)

    1. Method for producing magnesium alloys having a superplastic microstructure, which comprises the following steps:
      a) heating a magnesium-based alloy to a temperature of 300 to 550°C and holding this temperature for 1 to 100 hours,
      b) cooling the heated alloy to a temperature of 0 to 100°C,
      c) reheating the cooled alloy to a temperature of 200 to 400°C and holding this temperature for 1 to 100 hours,
      d) cooling the reheated alloy in air to a temperature of 0 to 100°C,
      e) forming the cooled alloy to form a semi-finished product at a temperature of 250 to 450°C.
    2. Method according to Claim 1, characterized in that in step a) the alloy is heated to a temperature of 390 to 420°C.
    3. Method according to Claim 1 or 2, characterized in that in step c) the alloy is heated to a temperature of 250 to 310°C.
    4. Method according to Claim 1, 2 or 3, characterized in that in step b) and/or d) the alloy is cooled to ambient temperature.
    5. Method according to one of Claims 1 to 4, characterized in that in step a) and/or c) the heated alloy is held at the final temperature for 12 to 24 hours.
    6. Method according to one of the preceding claims, characterized in that the magnesium-based alloy in addition to magnesium also contains aluminium, zinc, manganese, silicon, copper, zirconium, silver and/or rare earth metals.
    7. Method according to one of the preceding claims, characterized in that the alloy is formed by extrusion.
    8. Method according to Claim 7, characterized in that the pressing ratio during the extrusion is 1:25 to 1:50.
    9. Method according to Claim 7 or 8, characterized in that the billet temperature and the receptacle temperature during the extrusion is 300 to 400°C.
    EP01909511A 2000-01-25 2001-01-23 Method for providing magnesium alloys with superplastic properties Expired - Lifetime EP1252352B1 (en)

    Priority Applications (1)

    Application Number Priority Date Filing Date Title
    EP03011735A EP1342805A3 (en) 2000-01-25 2001-01-23 Method for providing magnesium alloys with superplastic properties

    Applications Claiming Priority (5)

    Application Number Priority Date Filing Date Title
    DE10003970 2000-01-25
    DE2000103970 DE10003970B4 (en) 2000-01-25 2000-01-25 Process for producing magnesium alloys having a superplastic microstructure
    DE2000111334 DE10011334A1 (en) 2000-03-10 2000-03-10 Production of magnesium alloys used as a material for the construction of airplanes, spacecraft, high speed trains and cars comprises heating a magnesium-based alloy, deforming to a semi-finished product and rapidly cooling
    DE10011334 2000-03-10
    PCT/DE2001/000256 WO2001055467A2 (en) 2000-01-25 2001-01-23 Method for providing magnesium alloys with superplastic properties

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    EP1252352B1 true EP1252352B1 (en) 2004-04-21

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    Cited By (2)

    * Cited by examiner, † Cited by third party
    Publication number Priority date Publication date Assignee Title
    CN100382905C (en) * 2003-04-15 2008-04-23 彼德·施托尔菲希 Method and apparatus for manufacturing profiled sheet parts
    DE102005027258B4 (en) * 2005-06-13 2013-01-31 Daimler Ag High carbon steel with superplasticity

    Families Citing this family (2)

    * Cited by examiner, † Cited by third party
    Publication number Priority date Publication date Assignee Title
    DE102005027259B4 (en) * 2005-06-13 2012-09-27 Daimler Ag Process for the production of metallic components by semi-hot forming
    RU2376397C1 (en) * 2008-09-22 2009-12-20 Федеральное государственное унитарное предприятие "Всероссийский научно-исследовательский институт авиационных материалов" (ФГУП "ВИАМ") Method of treatment of magnesium alloys

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    GB1187305A (en) * 1967-05-22 1970-04-08 Dow Chemical Co Process for production of Extruded Magnesium-Lithium Alloy Articles
    US3709745A (en) * 1970-10-19 1973-01-09 Dow Chemical Co Thermal process for improving the mechanical forming of magnesium alloys
    JPS61250144A (en) * 1985-04-26 1986-11-07 Ube Ind Ltd Magnesium alloy for casting
    JP3719525B2 (en) * 1994-11-14 2005-11-24 三井金属鉱業株式会社 Manufacturing method of superplastic magnesium alloy material
    US5620537A (en) * 1995-04-28 1997-04-15 Rockwell International Corporation Method of superplastic extrusion

    Cited By (2)

    * Cited by examiner, † Cited by third party
    Publication number Priority date Publication date Assignee Title
    CN100382905C (en) * 2003-04-15 2008-04-23 彼德·施托尔菲希 Method and apparatus for manufacturing profiled sheet parts
    DE102005027258B4 (en) * 2005-06-13 2013-01-31 Daimler Ag High carbon steel with superplasticity

    Also Published As

    Publication number Publication date
    EP1252352A2 (en) 2002-10-30
    ATE264928T1 (en) 2004-05-15
    CA2398125A1 (en) 2001-08-02
    AU2001237234A1 (en) 2001-08-07
    WO2001055467A3 (en) 2002-04-25
    WO2001055467A2 (en) 2001-08-02
    DE50102051D1 (en) 2004-05-27
    US20030140992A1 (en) 2003-07-31
    EP1342805A2 (en) 2003-09-10
    EP1342805A3 (en) 2004-03-17

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