EP2692884B1 - Magnesiumlegierung - Google Patents

Magnesiumlegierung Download PDF

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Publication number
EP2692884B1
EP2692884B1 EP12765196.6A EP12765196A EP2692884B1 EP 2692884 B1 EP2692884 B1 EP 2692884B1 EP 12765196 A EP12765196 A EP 12765196A EP 2692884 B1 EP2692884 B1 EP 2692884B1
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Prior art keywords
mass
content
magnesium alloy
aluminum
calcium
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EP12765196.6A
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English (en)
French (fr)
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EP2692884A4 (de
EP2692884A1 (de
Inventor
Kinji Hirai
Kenji Higashi
Yorinobu Takigawa
Tokuteru Uesugi
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Advanced Technologies Inc
Osaka Prefecture University PUC
Advanced Technology Inc
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Advanced Technologies Inc
Osaka Prefecture University PUC
Advanced Technology Inc
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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
    • 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 a magnesium alloy, particularly a magnesium alloy having high strength and high heat resistance, which can be worked into a wrought material such as an extruded or forged material.
  • magnesium is the lightest and has the highest specific strength among practical metals.
  • use of a magnesium alloy is expanded in various applications, for example, application of parts which underwent weight reduction using a magnesium alloy.
  • parts of the magnesium alloy are formed by a casting or die-casting method.
  • Patent Document 1 discloses that a magnesium alloy containing 0.1 to 15% by weight of calcium and optionally containing aluminum or zinc in the amount which does not exceed two times the amount of calcium is subjected to plastic working including extrusion and rolling, thereby homogeneously dispersing a crushed intermetallic compound in crystal grains, thus leading to an enhancement in mechanical strength.
  • Patent Document 2 discloses that refining of crystal grains is suppressed by performing hot rolling or forging at a predetermined processing temperature and rolling reduction ratio using a Mg-Al-Ca-Sr-Mn based alloy, and heat resistance is improved by controlling an aspect ratio of crystal grains (length of a major axis of crystal grains/length of a minor axis of crystal grains) without causing drastic fracture of a network intermetallic compound precipitated in the grain boundary.
  • Patent Document 3 relates to the problem to provide an Mg-Al-Zn alloy material which has ⁇ 300 MPa tensile strength and uniform mechanical properties and can be easily manufactured by extrusion.
  • an Mg-Al-Zn alloy material which includes: (1) a high strength magnesium alloy extruded material which has a composition consisting of 6 to 15% Al, ⁇ 4% Zn and the balance Mg and in which solid-solution Al comprises ⁇ 40% of the Al; (2) a high strength magnesium alloy extruded material composed of the above (1), in which the average grain size of crystals constituting the alloy material in the cross-sectional central part is made to ⁇ 10 ⁇ m; and (3) a high strength magnesium alloy extruded material composed of the above (1) or (2), in which a ratio between the average grain size A of crystals constituting the alloy material in the vicinity of an outer periphery and the average grain size B of crystals constituting the alloy material in the cross-sectional central part satisfies the relation of 1.3
  • the magnesium alloy according to Patent Document 1 had a problem that it is still insufficient in heat resistance, i.e. strength at high temperature.
  • the magnesium alloy according to Patent Document 2 had a problem that it is necessary to suppress the working degree (rolling reduction ratio) of hot rolling and forging to a low value so as to obtain a defined aspect ratio of crystal grains, so that the strength at room temperature may be sometimes insufficient.
  • the magnesium alloys of Patent Documents 1 and 2 may be sometimes insufficient in high-temperature strength or room-temperature strength.
  • the environmental temperature necessarily includes a range from room temperature to high temperature. Therefore, it is necessary that tensile characteristics of the magnesium alloy are excellent in both environments at room temperature and high temperature in practical use. Accordingly, a magnesium alloy having sufficient strength at room temperature and high temperature has been required.
  • the present invention has been made so as to meet the requirements, and thus an object thereof is to provide a magnesium alloy which has sufficiently high strength at room temperature and high temperature.
  • a first aspect of the present invention is directed to a magnesium alloy including: aluminum (Al): 14.0 to 23.0% by mass, calcium (Ca) : 11.0% by mass or less (not including 0% by mass), strontium (Sr): 12.0% by mass or less (not including 0% by mass), and zinc (Zn): 0.2 to 1.0% by mass, and the balance magnesium (Mg) and inevitable impurities, wherein the content of aluminum (A1), the content of calcium (Ca), and the content of strontium (Sr) satisfy a relation shown in the following equation (1): 0.8 ⁇ ⁇ Al > ⁇ 1.35 ⁇ ⁇ Ca > + 1.23 ⁇ ⁇ Sr > + 8.5 ⁇ 1.2 ⁇ ⁇ Al > where ⁇ A1> is the content of aluminum (Al) expressed on % by mass basis, ⁇ Ca> is the content of calcium (Ca) expressed on % by mass basis, and ⁇ Sr> is the content of strontium (Sr) expressed on % by mass basis.
  • a second aspect of the present invention is directed to the magnesium alloy according to the first aspect, further including at least one selected from the group consisting of silicon (Si): 0.1 to 1.5% by mass, rare earth (RE): 0.1 to 1.2% by mass, zirconium (Zr): 0.2 to 0.8% by mass, scandium (Sc): 0.2 to 3.0% by mass, yttrium (Y): 0.2 to 3.0 % by mass, tin (Sn): 0.2 to 3.0% by mass, barium (Ba): 0.2 to 3.0% by mass, and antimony (Sb): 0.1 to 1.5% by mass.
  • a third aspect of the present invention is the magnesium alloy according to the first or second aspect, in which a ratio of the content of strontium (Sr) to the content of calcium (Ca) is from 1:0.3 to 1:1.5 in terms of a mass ratio.
  • a fourth aspect of the present invention is directed to the magnesium alloy according to any one of the first to third aspects, in which precipitates containing Al 2 Ca and Al 4 Sr are formed in the grain boundary with an interval from each other.
  • the present inventors have made a study on simultaneous utilization of both solid solution strengthening and precipitation strengthening known as strengthening mechanisms of a magnesium alloy.
  • the present inventors have determined solid solubility limit of aluminum in a magnesium alloy matrix and found appropriate amounts of aluminum, calcium and strontium on the basis of the solid solubility limit, and thus completing a magnesium alloy according to the present invention, having sufficient strength at both room temperature and high temperature in which a matrix forms a solid solution with a sufficient amount of aluminum, and also an appropriate amount of intermetallic compounds Al 2 Ca and Al 4 Sr are precipitated.
  • Examples of the element capable of being solid-soluted in a magnesium alloy to lower stacking fault energy include In, Tl, Sc, Pb, Al, Y, Sn and Bi. Of these elements, aluminum (Al) is preferable from the viewpoint of safety and economy.
  • magnesium alloy is worked into a wrought material by performing plastic working including rolling, extrusion and drawing after casting so as to obtain desired shape, toughness, strength and the like, second phases containing Al 2 Ca and Al 4 Sr precipitating in the grain boundary are fractured (fragmented) and arranged in the deformation direction.
  • the precipitates containing Al 2 Ca and Al 4 Sr thus arranged in the deformation direction contribute to an enhancement in high-temperature strength.
  • second phase particles containing Al 2 Ca and Al 4 Sr can be reprecipitated and dispersed by performing a homogenization heat treatment at 350 to 450°C, leading to more enhancement in strength. It has also been found that, more preferably, second phases containing Al 2 Ca and Al 4 Sr can be homogeneously dispersed in the grain boundary by performing a homogenization heat treatment at 385°C to 415°C, and thus enabling an increase in strength more certainly.
  • the present inventors have found that the amount of aluminum of the magnesium alloy according to the present invention is appropriately from 14.0 to 23.0% by mass.
  • the amount of aluminum is 14.0% by mass or more, a sufficient amount of aluminum can form intermetallic compounds Al 2 Ca and Al 4 Sr with calcium and strontium even if about 8.5% by mass of aluminum is solid-soluted in the matrix. If the amount of aluminum is 23.0% by mass or less, it is possible to ensure ductility such as elongation.
  • the amount of aluminum is from 15.0% by mass to 20.0% by mass.
  • the content of calcium is 11.0% by mass or less (not including 0% by mass).
  • the content of calcium is from 1.0 to 8.0% by mass. This is because it is possible to form Al 2 Ca more certainly and to suppress excessiveness.
  • the content of strontium is 12.0% by mass or less (not including 0% by mass).
  • the content of strontium is from 0.5 to 8.0% by mass. This is because it is possible to form Al 4 Sr more certainly and to suppress excessiveness. More preferably, the content is from 1.0 to 6.0% by mass. This is because it is possible to maximally exert the effect of strontium.
  • the magnesium alloy according to the present invention contains 0.2 to 1.0% by mass of zinc (Zn).
  • a ratio of (content of calcium):(content of strontium) (content of strontium assumed that the content of calcium is 1) is preferably from 1:0.3 to 1:1.5 in terms of a mass ratio, and more preferably 1:0.5 to 1:1.1 in terms of a mass ratio.
  • the amount of aluminum (% by mass) indicated by the symbol y in the equation (2) is required.
  • ⁇ Ca> is the content of calcium expressed on % by mass basis and ⁇ Sr> is the content of strontium expressed on % by mass basis.
  • aluminum is contained such that the amount of aluminum (y) represented by the equation (2), which is required for entire strontium and calcium to precipitate as Al 2 Ca and Al 4 Sr, respectively, is within a range of the amount which is 0.8 to 1.2 times the content of aluminum.
  • the alloy of the present invention contains the above-mentioned aluminum, calcium, strontium and zinc, with the balance being magnesium (Mg) and inevitable impurities.
  • Al 2 Ca and Al 4 Sr are often precipitated in the grain boundary, as second phases containing Al 2 Ca and Al 4 Sr, in the form of a network.
  • the second phases containing network Al 2 Ca and Al 4 Sr precipitates
  • a magnesium alloy article obtained by plastic working (plastic deformation) also has high-temperature strength.
  • magnesium alloy according to the present invention (magnesium alloy article (wrought material)) is preferably subjected to a homogenization heat treatment at 350 to 450°C after plastic working.
  • a homogenization heat treatment at 350 to 450°C it is preferred to maintain within such temperature range for 24 to 72 hours. This is because this treatment enables redissolution (reprecipitation) of precipitates, leading to an improvement in heat stability.
  • the present inventors have also found that a homogenization heat treatment at 385°C to 415°C enables reprecipitation of second phase particles containing Al 2 Ca and Al 4 Sr and homogeneous dispersion of the second phase particles along the grain boundary, leading to further improvement in high-temperature strength.
  • a homogenization treatment is performed at 385°C to 415°C after plastic working, second phase particles containing Al 2 Ca and Al 4 Sr (precipitates) are precipitated in the form of particles, instead of a network, with an interval from each other (i.e. discontinuously) along the grain boundary. The thus obtained precipitates in this form remarkably contribute to an improvement in high-temperature strength.
  • the magnesium alloy according to the present invention (magnesium alloy article (wrought material)) is preferably subjected to a homogenization heat treatment at 385 to 415°C after plastic working.
  • a homogenization heat treatment at 385 to 415°C it is preferred to maintain within such temperature range for 24 to 72 hours. This is because this treatment enables redissolution of precipitates and homogenization of the structure, leading to homogenization and stabilization of an intermetallic compound structure with high heat stability of the grain boundary.
  • plastic working includes various hot and cold plastic workings.
  • examples of the plastic working include extrusion, rolling, forging, drawing, swaging, and combinations thereof.
  • Each alloy sample was melted at 700°C and then cast into a billet using a cylindrical die.
  • the casted billet was heated to 400°C at a heating rate of 0.5°C/minute, maintained for 48 hours and then water-cooled. After removing a surface oxide layer by machining, the billet was extruded at an extrusion temperature of 350°C, an extrusion rate of 0.2 mm/second and an extrusion ratio of 16 to obtain a round bar (10 mm in diameter).
  • Example 1 In order to examine an influence of a homogenization heat treatment, regarding the above-mentioned sample of Example 1 (extruded round bar), an as-extruded material, a material subjected to a homogenization heat treatment at 400°C for 48 hours, and a material subjected to a homogenization heat treatment at 420°C for 48 hours were produced.
  • Figs. 1A to 1C show metallographic structures observed by a confocal laser scanning microscope, in which Fig. 1A shows a metallographic structure of an as-extruded material, Fig. 1B shows a metallographic structure of a material subjected to a homogenization heat treatment at 400°C for 48 hours, and Fig. 1C shows a metallographic structure of a material subjected to a homogenization heat treatment at 420°C for 48 hours.
  • precipitates containing Al 2 Ca and Al 4 Sr are fragmented and arranged in the extrusion direction (up/down direction in the drawing).
  • precipitates containing Al 2 Ca and Al 4 Sr are dispersed.
  • granular precipitates containing comparatively fine Al 2 Ca and Al 4 Sr are homogeneously distributed with an interval from each other along the grain boundary.
  • Fig. 2 shows the results of a high-temperature tensile test at 150°C (true stress-strain diagram) of an as-extruded material, a material subjected to a homogenization heat treatment at 400°C for 48 hours, and a material subjected to a homogenization heat treatment at 420°C for 48 hours.
  • the tensile test was carried out at a temperature of 150°C and a tension speed of 1 ⁇ 10 -3 /second.
  • the material subjected to a homogenization heat treatment at 400°C for 48 hours has high-temperature strength which is remarkably high strength of more than 300 MPa.
  • the grain size of each alloy sample is shown in Table 2.
  • the grain size was measured by the electron back scattered diffraction patterns (EBSD) method. Crystal grains were defined by regarding deviation of orientation of 15° or more as the grain boundary.
  • Comparative Example 3 the grain size could not be measured since precipitates underwent coarsening. Except for Comparative Example 3, the grain size (both peak-top grain size and area average particle size) decreases as addition amounts of aluminum, calcium and strontium increases.
  • Fig. 3 shows the measurement results of the tensile strength at room temperature.
  • the drawing shows the measurement results of the tensile strength, 0.2% proof stress, and elongation of each alloy sample. In Comparative Examples 2 and 3, 0.2% proof stress could not be measured since the material is brittle.
  • Example 1 and Example 2 the tensile strength exhibited excellent value such as 300 MPa or more.
  • the 0.2% proof stress is less than 250 MPa, and the samples of Example 1 and Example 2 having the 0.2% proof stress of 250 MPa or more are excellent in room-temperature strength as compared with the samples of Comparative Examples. It is also apparent that the samples of Example 1 and Example 2 exhibit the elongation of 2% or more and have sufficient ductility.
  • the sample which is produced by extruding an AZ91 alloy known as a high strength magnesium alloy at an extrusion temperature of 360°C and an extrusion ratio of 22, each being the same level as that of the samples of Examples 1 and 2, exhibits the tensile strength of 295 MPa ( Hanlin Ding et al., Journal of alloys and compounds, 456(2008) 400-406 ). As is apparent from these results, the samples of Examples 1 and 2 have high room-temperature strength.
  • Fig. 4 shows the measurement results of high-temperature tensile strength.
  • the high-temperature tensile test was carried out at a measuring temperature of 175°C and a strain rate of 1 ⁇ 10 -4 /second.
  • Example 1 and Example 2 exhibited high-temperature strength which is higher than that in Comparative Examples, that is, high-temperature strength at 175°C is 210 MPa or more.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
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Claims (4)

  1. Magnesiumlegierung, umfassend:
    Aluminium (Al): 14,0 bis 23,0 Massen-%,
    Calcium (Ca): 11,0 Massen-% oder weniger (ausschließlich 0 Massen-%),
    Strontium (Sr): 12,0 Massen-% oder weniger (ausschließlich 0 Massen-%),
    Zink (Zn): 0,2 bis 1,0 Massen-%, und gegebenenfalls Si, RE, Zr, Sc, Y, Sn, Ba, Sb,
    den Rest Magnesium (Mg) und unvermeidbare Verunreinigungen, wobei der Gehalt an Aluminium (Al), der Gehalt an Calcium (Ca) sowie der Gehalt an Strontium (Sr) der in der folgenden Gleichung (1) gezeigten Beziehung genügen: 0 , 8 × < Al > ≤ 1 , 35 × < Ca > + 1 , 23 × < Sr > + 8 , 5 ≤ 1 , 2 × < Al >
    Figure imgb0005
     wobei <Al> der Gehalt an Aluminium (Al) ist, ausgedrückt auf Massenprozentbasis, <Ca> der Gehalt an Calcium (Ca) ist, ausgedrückt auf Massenprozentbasis und <Sr> der Gehalt an Strontium (Sr) ist, ausgedrückt auf Massenprozentbasis.
  2. Magnesiumlegierung gemäß Anspruch 1, des Weiteren umfassend wenigstens eines, ausgewählt aus der Gruppe, bestehend aus:
    Silicium (Si): 0,1 bis 1,5 Massen-%,
    seltene Erden (RE): 0,1 bis 1,2 Massen-%,
    Zirkonium (Zr): 0,2 bis 0,8 Massen-%,
    Scandium (Sc): 0,2 bis 3,0 Massen-%,
    Yttrium (Y): 0,2 bis 3,0 Massen-%,
    Zinn (Sn): 0,2 bis 3,0 Massen-%,
    Barium (Ba): 0,2 bis 3,0 Massen-% und
    Antimon (Sb): 0,1 bis 1,5 Massen-%.
  3. Magnesiumlegierung gemäß Anspruch 1 oder 2, wobei das Verhältnis des Gehalts an Strontium (Sr) zu dem Gehalt an Calcium (Ca) von 1:0,3 bis 1:1,5 als Massenverhältnis reicht.
  4. Magnesiumlegierung gemäß einem der Ansprüche 1 bis 3, wobei Präzipitate, welche Al2Ca und Al4Sr enthalten, an der Korngrenze mit einem Abstand voneinander gebildet sind.
EP12765196.6A 2011-03-29 2012-03-28 Magnesiumlegierung Not-in-force EP2692884B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2011072505A JP5729081B2 (ja) 2011-03-29 2011-03-29 マグネシウム合金
PCT/JP2012/058113 WO2012133522A1 (ja) 2011-03-29 2012-03-28 マグネシウム合金

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EP2692884A1 EP2692884A1 (de) 2014-02-05
EP2692884A4 EP2692884A4 (de) 2014-11-19
EP2692884B1 true EP2692884B1 (de) 2017-05-03

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US (1) US20140044586A1 (de)
EP (1) EP2692884B1 (de)
JP (1) JP5729081B2 (de)
CN (1) CN103635598A (de)
TW (1) TWI519649B (de)
WO (1) WO2012133522A1 (de)

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CN104109827B (zh) * 2014-08-11 2016-04-13 重庆科技学院 Mg-Zn系镁合金板材的轧制工艺
CN108431261A (zh) * 2015-12-28 2018-08-21 韩国机械研究院 具有优异的机械性能和耐腐蚀性的镁合金及其制造方法
US10808302B2 (en) 2016-07-15 2020-10-20 Sumitomo Electric Industries, Ltd. Magnesium alloy
CN108220724A (zh) * 2017-12-22 2018-06-29 中山市榄商置业发展有限公司 一种镁合金新材料及其制备工艺
CN109182860A (zh) * 2018-11-08 2019-01-11 中信戴卡股份有限公司 一种高强韧镁合金及制备方法
AT522003B1 (de) * 2018-12-18 2021-10-15 Lkr Leichtmetallkompetenzzentrum Ranshofen Gmbh Magnesiumbasislegierung und Verfahren zur Herstellung derselben
CN109913720B (zh) * 2019-03-27 2020-11-24 东北大学 一种高钙高铝含量的高弹性模量镁基复合材料及制备方法
CN110438380B (zh) * 2019-08-13 2021-02-26 中南大学 一种耐热阻燃镁合金及其形变热处理方法

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JPH08269609A (ja) * 1995-03-27 1996-10-15 Toyota Central Res & Dev Lab Inc ダイカスト性に優れたＭｇ−Ａｌ−Ｃａ合金
JP3030338B1 (ja) 1998-10-05 2000-04-10 工業技術院長 高強度難燃性マグネシウム合金の製造方法
JP3603706B2 (ja) * 1999-12-03 2004-12-22 株式会社日立製作所 高強度Ｍｇ基合金とＭｇ基鋳造合金及び物品
CN1225565C (zh) * 2001-08-24 2005-11-02 三菱铝株式会社 模铸镁合金
JP4208649B2 (ja) * 2003-06-06 2009-01-14 株式会社新技術研究所 成形仕上り性に優れたマグネシウム合金およびその成形品
KR101127113B1 (ko) * 2004-01-09 2012-03-26 켄지 히가시 다이캐스트용 마그네슘 합금 및 이것을 사용한 마그네슘다이캐스트 제품
JP4803357B2 (ja) 2005-09-06 2011-10-26 独立行政法人産業技術総合研究所 熱間加工により作製される耐熱マグネシウム合金及びその製造方法
JP4864413B2 (ja) * 2005-10-18 2012-02-01 株式会社神戸製鋼所 高強度マグネシウム合金押出し材
JP2010242146A (ja) * 2009-04-03 2010-10-28 Toyota Central R&D Labs Inc マグネシウム合金およびマグネシウム合金部材
JP4987936B2 (ja) 2009-09-30 2012-08-01 京楽産業．株式会社 遊技機

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JP2012207253A (ja) 2012-10-25
WO2012133522A1 (ja) 2012-10-04
TW201307580A (zh) 2013-02-16
CN103635598A (zh) 2014-03-12
TWI519649B (zh) 2016-02-01
EP2692884A4 (de) 2014-11-19
JP5729081B2 (ja) 2015-06-03
US20140044586A1 (en) 2014-02-13
EP2692884A1 (de) 2014-02-05

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