WO2009014807A1 - Formation d'alliages de magnésium ayant une ductilité améliorée - Google Patents

Formation d'alliages de magnésium ayant une ductilité améliorée Download PDF

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Publication number
WO2009014807A1
WO2009014807A1 PCT/US2008/065252 US2008065252W WO2009014807A1 WO 2009014807 A1 WO2009014807 A1 WO 2009014807A1 US 2008065252 W US2008065252 W US 2008065252W WO 2009014807 A1 WO2009014807 A1 WO 2009014807A1
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WO
WIPO (PCT)
Prior art keywords
magnesium
cerium
billet
percent
extruded
Prior art date
Application number
PCT/US2008/065252
Other languages
English (en)
Inventor
Anil K. Gupta
Arun M. Kumar
Palle Ramarao
Anil K. Sachdev
Aihua A. Luo
Raja K. Mishra
Original Assignee
Gm Global Technology Operations, Inc.
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Gm Global Technology Operations, Inc. filed Critical Gm Global Technology Operations, Inc.
Priority to DE112008001968.1T priority Critical patent/DE112008001968B4/de
Priority to CN200880109155A priority patent/CN101809179A/zh
Publication of WO2009014807A1 publication Critical patent/WO2009014807A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C23/00—Extruding metal; Impact extrusion
    • B21C23/002—Extruding materials of special alloys so far as the composition of the alloy requires or permits special extruding methods of sequences
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C29/00—Cooling or heating work or parts of the extrusion press; Gas treatment of work
    • 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
    • C22C1/11—Making amorphous alloys
    • 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
    • C22C23/06—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

  • This invention generally relates to processed magnesium alloy compositions exhibiting improved ductility at room temperature. More specifically, magnesium alloyed with cerium is subjected to high temperature deformation to improve the alloy's formability at room temperature.
  • Magnesium is the lightest structural metal. In engineering applications it is alloyed with one or more elements, for example, aluminum, manganese, rare earth metals, lithium, zinc, and silver. Magnesium usually constitutes eighty-five percent by weight or more of these alloys. [0003] The cost of magnesium has decreased dramatically in recent years and magnesium and its alloys have become attractive structural materials for a wide range of applications due in part to desirable physical properties such as light weight, high specific strength and stiffness, machinability, and the ability to be easily recycled. However, the use of magnesium in wrought products like sheet and extrusions has been limited due to the poor workability of magnesium castings and the lower formability and ductility of magnesium in the primary fabricated stage.
  • pure magnesium At room temperature, pure magnesium is generally characterized by limited ductility as a result of its hexagonal close- packed crystal structure and resulting limited number of active slip systems. This inherent limitation often discourages widespread use of magnesium in wrought products made from sheets and extrusions because it is difficult and expensive to process the poorly workable metal into useable finished shapes. [0004] It is generally understood by those skilled in the art that metal manufacturing techniques which promote grain refinement may help to improve certain tensile properties such as work hardening and ductility in magnesium metals.
  • ECAE equal channel angular extrusion
  • a melt containing, by weight 0.2 percent cerium and the balance magnesium was cast into a round cylindrical billet for in-line extrusion.
  • the billet was preheated to 400 0 C for two hours and pushed along a straight axis (not ECAE) through a circular die with an extrusion ratio of 25:1 to produce a solid rod about fifteen millimeters in diameter.
  • a like extruded billet was produced consisting of magnesium with 0.5 weight percent cerium.
  • a billet of pure magnesium was cast and extruded in the same way.
  • cerium in amounts up to about one percent by weight is found to enhance the room temperature ductility and workability of magnesium alloys following suitable hot deformation processing.
  • the hot deformation is accomplished by extrusion at billet temperatures of about 35O 0 C to about 475 0 C with extrusion ratios in the range of about 10:1 to about 60:1 at suitable extrusion speeds.
  • the billets were suitably lubricated with graphite based lubricants or boron nitride, although this is not necessarily required.
  • the presence of the small amount of cerium favors the formation of recrystallized grains with their basal planes oriented at 40-50 degrees to the extrusion axis.
  • the magnesium-cerium alloy provides easier basal slippage during subsequent straining along the extrusion axis which is effectively precluded in the extruded rods of pure magnesium. But whatever the straining mechanism, the presence of about 0.2 to about 0.5 weight percent cerium in the hot worked magnesium matrix markedly increased the ability to further shape the extruded bar material at room temperature. And the improvement was realized whether the hot worked material was solid in cross-section or hollow. Thus, hot extruded magnesium alloy bars or tubes, for example, may then be subjected to bending or hydroforming steps, for example, at an ambient temperature to more easily form more complex shapes for automotive vehicle structures or parts, or the like.
  • magnesium in amounts up to about nine percent by weight, and/or zinc in amounts up to about three percent by weight, and/or manganese in amounts up to about one percent by weight have been used in commercial magnesium based alloys.
  • small amounts of titanium have been added for grain-refinement of magnesium alloys.
  • Cerium additions in an amount up to about one weight percent may be used to improve the room- temperature ductility of these many different magnesium alloys but the room temperature ductility may not be as high as in the magnesium-0.2-1 cerium binary alloys.
  • magnesium will constitute at least eighty-five percent by weight of the magnesium-cerium alloy when these other alloying constituents are used for other properties of the resulting alloy.
  • Figure l is a bar graph of percent elongation at ultimate load in tensile testing for extruded specimens of pure magnesium, magnesium-0.2 wt % cerium, and magnesium-0.5 wt. % cerium. The tensile tests were conducted along the extrusion axis of the workpieces.
  • Figure 2 is a bar graph of tensile strength in MPa for extruded specimens of pure magnesium, magnesium-0.2 wt. % cerium, and magnesium- 0.5 wt. % cerium.
  • Magnesium alloys comprising primarily magnesium with small additions of cerium may be formed by a hot deformation process into a wrought article that exhibits improved ductility at room temperature.
  • room temperature means a typical in-door ambient temperature of, for example, about fifteen to about thirty degrees Celsius.
  • the wrought article may be in a final product shape.
  • the room temperature ductility of the wrought article makes it useful for further deformation processing into a desired different shape.
  • the unexpected ductility of the hot deformed magnesium body is attributable to its cerium content and hot deformation processing that contribute to an alteration in slip distribution, a decrease in yield strength, an increase in work hardening, a reduction in grain size, and a recrystallized texture that favors basal dislocation activity.
  • Cerium is a preferred rare earth element for addition to magnesium for improved ductility of the magnesium-cerium combination. It may be preferred to use cerium in the form of mischmetal. Cerium mischmetal is an alloy of rare earth elements in various naturally occurring proportions. It is sometimes called cerium mischmetal or rare earth mischmetal. A representative mischmetal composition includes approximately, by weight, fifty percent cerium, forty-five percent lanthanum, with small amounts of neodymium and praseodymium. Sometimes, the alloys contain more or less cerium. An embodiment of the invention will be illustrated using cerium as the sole rare earth element additive in magnesium for markedly improving the ductility at room temperature of certain exemplary binary magnesium-cerium alloys.
  • a magnesium alloy comprising a small amount up to about one weight percent cerium may undergo a hot deformation process to fabricate a wrought metal object that exhibits enhanced room temperature ductility as compared to that of magnesium and conventional magnesium alloys.
  • the solubility of cerium in magnesium is approximately 0.1% at 500 0 C. Any excess cerium ultimately forms intermetallics with magnesium and oxide particles within the alloy.
  • a hot deformation technique suitable for improving ductility in a magnesium-cerium alloy may be a conventional in-line hot extrusion process.
  • a magnesium alloy comprising up to about one weight percent cerium may be cast as a billet.
  • the initial cast billet is suitably round in cross-section with a diameter of, for example, about 50 millimeters to typically about 300 millimeters, although larger billets are also extruded.
  • the cast billet is preheated to a deformation temperature in the range of about 300°C to 475 °C. Precautions may be taken to ensure that the magnesium- cerium alloy billet is sufficiently lubricated during extrusion by any known metal lubricant such as, for example, graphite or boron nitride.
  • the magnesium alloy billet may be direct extruded through a conventional circular or conical extrusion die possessing an extrusion ratio in the range of 10:1 to 60: 1 at a speed in the range of 10 mm per second to 1000 mm per second of extrudate.
  • the magnesium-cerium alloy may be hot extruded into any one of a number of sizes and shapes known to those of ordinary skill in the art, such as, but not limited to, solid or hollow rods, I-beams, or other achievable extruded shapes.
  • the enhanced ductility of these shapes may then be utilized by further working of the shapes (for example by bending or hydroforming) at a room temperature.
  • a magnesium alloy comprising 0.2 weight percent cerium and the balance magnesium that underwent a hot direct extrusion process in accordance with the specifications outlined above achieved an elongation value of approximately 30% during subsequent room temperature deformation.
  • a similarly extruded alloy comprising 0.5 weight percent cerium achieved a slightly smaller elongation value of approximately 25%.
  • a billet of substantially pure magnesium was hot extruded by the same method and extrusion die.
  • the pure magnesium extrusion had a room temperature elongation of 9% at ultimate tensile load along the extrusion axis.
  • the relatively high ductility observed in these magnesium-cerium alloys may be at least partly attributable to the dominant role attributed to slip during subsequent tensile deformation of the hot worked alloy along the extrusion axis.
  • Another factor that may be at least partly attributable to high ductility is the intense shear banding that occurs parallel to the extrusion axis which ultimately leads to a redistribution of deformation away from the shear bands and towards the matrix during continuous recrystallization at room temperature. It is contemplated that these phenomena, as well as a reduction in yield strength and grain size, are attributable to the small amount of cerium present in the magnesium-cerium alloy.
  • the billets were each preheated and maintained at a temperature of about 400°C for a period of two hours and subsequently forced through a circular die with an extrusion ration of 25:1 at a speed of 10 mm/sec.
  • Boron nitride was used as a lubricant to facilitate the hot metal extrusion.
  • the mechanical properties and microstructure of the pure Mg and Mg-0.2Ce solid rods were analyzed and compared. [0030]
  • samples of the solid extruded rods were tested to evaluate yield strength, compressibility, and elongation.
  • tensile specimens having a 25 mm gauge length and a 6.25 mm gauge diameter were tested with an Instron Universal Testing Machine at an average strain rate of 0.66 x 10 "3 s "1 . Three specimens were taken from different locations along the steady state portion of the extruded rods and the average values were reported.
  • tensile tests on the pure Mg sample revealed a yield strength of 106 MPa, an ultimate tensile strength of 170 MPa, and an elongation value 9.1%.
  • Corresponding tests performed on the Mg-0.2Ce sample revealed a yield strength of 68.6 MPa, an ultimate tensile strength of 155 MPa, and an elongation value greater than 30%.
  • the Mg-0.2Ce alloy extruded rod sample has a lower yield strength and is significantly more ductile than the pure Mg metal rod sample. Additional details pertaining to the fracture surfaces of the tensile specimens will be set out below in conjunction with the microstructure analysis of the extruded rods.
  • the compressive yield strengths of the two samples were nearly identical with the strength of pure Mg measured at 53.5 MPa and the strength of Mg-0.2Ce measured at of 55.8 MPa.
  • the similarity in compressive yield strengths arises from the fact that the threshold deformation required to nucleate the extension twins are equivalent in each sample. A noted difference, however, was observed in the way each sample transitioned from elastic behavior to plastic behavior. More specifically, the pure Mg sample abruptly transitioned from elastic to plastic mode which signals that deformation occurs almost exclusively by twinning. In the Mg-0.2Ce sample, a gradual transition between the elastic and plastic mode was observed, which suggests that deformation occurs by a combination of twinning and slip mechanisms.
  • Polished samples cut parallel and normal to the extrusion axis were fabricated from both extruded rods and examined with a NikonTM optical microscope interfaced with a LecoTM image analyzer to inspect the microstructure in both the longitudinal and transverse directions.
  • the optical micrographs show no anisotropy in grain morphology along either direction and indicate a fully recrystallized, nearly equi-axed grain structure with an average grain size of approximately 60 ⁇ m for the pure Mg sample and 45 ⁇ m for the Mg-0.2Ce sample. There was also some evidence of twinning in the Mg-0.2Ce sample sectioned parallel to the extrusion axis that was not present in the corresponding pure Mg sample.
  • the samples were also examined by electron backscattered diffraction (EBSD) in a LEOTM 1450 scanning electron microscope placed 18mm from the samples and fitted with a TSLTM EBSD camera operating at 20 KV.
  • EBSD data maps generated with TSL data analysis software from samples cut parallel to the extrusion axis indicate that both the pure Mg and Mg-0.2Ce metals underwent a fully recrystallized extrusion.
  • the data maps show that both the pure Mg metal and the Mg-0.2Ce metal contain grains having equi-axed shapes and straight grain boundaries.
  • the data maps also provided grain size measurements adjusted for twinning of approximately 34 ⁇ m for the pure Mg sample, which exhibited very little twinning, and approximately 26 ⁇ m for the Mg-0.2Ce sample, which exhibited twinning in about 2% of its grains.
  • the Mg-0.2Ce sample and accordingly the Mg-0.2Ce extruded rod, comprises a grain structure with a basal slip orientation more acquiescent to formability than the pure Mg extruded rod.
  • the addition of small amounts of cerium evidently alters the texture of the magnesium material during the recrystallization phase that follows hot extrusion.
  • the enhanced ductility of magnesium-rare earth alloys following an in-line directional hot deformation is attributed to altered metallurgical texture favoring basal slip activity, altered slip angle distribution, higher work hardening, and smaller grain size. Hot rolling with a significant reduction in cross-section may also be used as the directional hot deformation.
  • the effect is obtained by finding a suitable preferred temperature (of at least about 300 0 C) for a directional deformation of a suitably configured billet of the alloy.
  • a suitable preferred temperature of at least about 300 0 C
  • preferred extrusion ratio is particularly effective.
  • the improvement seems most pronounced in binary magnesium-cerium alloys, using cerium or a cerium mischmetal as the alloying constituent.
  • additional alloying constituents such as aluminum.
  • Other alloying constituents such as manganese, zinc, and titanium may be used for other properties but the room temperature ductility may be reduced.
  • the magnesium content of the alloy is suitably at least eighty-five percent of the alloy and preferably ninety percent by weight of the alloy or more.

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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)
  • Extrusion Of Metal (AREA)
  • Forging (AREA)

Abstract

Un alliage de magnésium comprenant jusqu'à environ un pour cent en poids de cérium peut être travaillé à chaud pour produire une pièce à travailler en alliage intermédiaire ou final qui présente une ductilité améliorée à la température ambiante. L'addition d'une petite quantité de cérium peut affecter l'alliage de magnésium par réduction de la résistance à la déformation, affinage de la dimension du grain et amélioration du comportement de durcissement d'écoulement. Une recristallisation pendant une déformation à chaud de la matière de magnésium contenant un métal des terres rares modifie la texture de l'alliage et oriente les grains d'une manière qui favorise une activité de glissement basal. L'alliage se déforme ainsi à la température ambiante par une combinaison de mécanismes d'hémitropie et de glissement.
PCT/US2008/065252 2007-07-26 2008-05-30 Formation d'alliages de magnésium ayant une ductilité améliorée WO2009014807A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
DE112008001968.1T DE112008001968B4 (de) 2007-07-26 2008-05-30 Bilden von Magnesiumlegierungen mit verbesserter Duktilität
CN200880109155A CN101809179A (zh) 2007-07-26 2008-05-30 形成具有改善的延展性的镁合金

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US95201807P 2007-07-26 2007-07-26
US60/952,018 2007-07-26

Publications (1)

Publication Number Publication Date
WO2009014807A1 true WO2009014807A1 (fr) 2009-01-29

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US (1) US20090028743A1 (fr)
CN (1) CN101809179A (fr)
DE (1) DE112008001968B4 (fr)
WO (1) WO2009014807A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102009048450A1 (de) * 2008-10-20 2010-06-10 GM Global Technology Operations, Inc., Detroit Hochduktile und hochfeste Magnesiumlegierungen

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KR101139879B1 (ko) 2009-07-17 2012-05-02 포항공과대학교 산학협력단 선압축변형을 이용하여 저주기 피로 수명이 향상된 마그네슘 합금 가공재의 제조방법
CN103597104B (zh) * 2011-06-23 2017-03-15 延世大学校产学协力团 分散有氧化物颗粒的氧原子和金属元素的合金材料及其制造方法
EP2727667B1 (fr) * 2011-06-28 2018-05-09 The University of Electro-Communications Procédé de production d'un matériau en alliage de magnésium à haute résistance
CN103911569A (zh) * 2012-12-28 2014-07-09 北京有色金属研究总院 一种弱化变形镁合金产品各向异性的方法
WO2014138027A1 (fr) * 2013-03-05 2014-09-12 Arcanum Alloy Design Inc. Alliages ultra-minces
CN107012376B (zh) * 2016-01-27 2019-06-11 中国科学院金属研究所 一种低稀土含量的高速挤压镁合金变形材及其制备工艺
WO2017201418A1 (fr) 2016-05-20 2017-11-23 Arcanum Alloys, Inc. Procédés et systèmes de revêtement de substrat en acier
CN110940686B (zh) * 2019-11-18 2021-12-21 中国科学院金属研究所 通过ebsd技术和维氏硬度计来计算孪晶临界分切应力的方法
CN117161116A (zh) * 2022-05-27 2023-12-05 通用汽车环球科技运作有限责任公司 挤出粗晶粒、低铝含量的镁合金的方法

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DE102009048450A1 (de) * 2008-10-20 2010-06-10 GM Global Technology Operations, Inc., Detroit Hochduktile und hochfeste Magnesiumlegierungen

Also Published As

Publication number Publication date
US20090028743A1 (en) 2009-01-29
CN101809179A (zh) 2010-08-18
DE112008001968B4 (de) 2019-12-05
DE112008001968T5 (de) 2010-06-02

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