EP2157201B1 - Alliage à base de mg - Google Patents

Alliage à base de mg Download PDF

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Publication number
EP2157201B1
EP2157201B1 EP08752560.6A EP08752560A EP2157201B1 EP 2157201 B1 EP2157201 B1 EP 2157201B1 EP 08752560 A EP08752560 A EP 08752560A EP 2157201 B1 EP2157201 B1 EP 2157201B1
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EP
European Patent Office
Prior art keywords
alloy
heat treatment
extruded
aging
subjected
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Not-in-force
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EP08752560.6A
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German (de)
English (en)
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EP2157201A1 (fr
EP2157201A4 (fr
Inventor
Chamini Mendis
Keiichiro Oishi
Kazuhiro Houno
Yoshiaki Kawamura
Shigeharu Kamado
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National Institute for Materials Science
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National Institute for Materials Science
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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
    • C22C23/04—Alloys based on magnesium with zinc or cadmium as the next major constituent

Definitions

  • This invention relates to an Mg base alloy containing Mg as a main material, realization of which is desired as a lightweight material which is a replacement for Al.
  • Patent Documents 2, 3, 4, 6 and 8 in order to contrive to improve strength, a rare earth element, scandium or lithium is added.
  • a rare earth element is a rare element which is hardly obtainable on the earth, alloys thereof are high in the price and low in the multiplicity of use.
  • Patent Document 1 is concerned with a quinary alloy containing from 0.3 to 3 % by mass of Ca and simultaneously containing Al, Sr and Mn. In such an alloy, a precipitate (crystal) is formed on the grain boundary of Mg.
  • Patent Document 2 is concerned with an Mg alloy which contains 0.3 % or more and not more than 1.0 % of Zr and which in the case of containing Ca, contains 0.2 % or more and not more than 2.0 % of Ca (% means % by mass).
  • Patent Document 8 discloses an Mg alloy developed as a casting material, which contains from 3 to 8 % by weight of Zn and from 0.8 to 5 % by weight of Ca.
  • An alloy of Patent Document 7 is an alloy developed as a casting material. Specifically, it is disclosed that Ca is zero or 0.5 % by weight, and Zn is from 1 % by weight to 7 % by weight; and in combinations of zero, in the case where Ca is zero or 0.5 % by weight, when Zn Is zero, then the alloy has a 0.2 % proof stress of less than 75 MPa, whereas when Zn is from 1 % by weight to 7 % by weight, then the alloy has a 0.2 % proof stress of 75 MPa or more and less than 100 MPa. Thus, it is demonstrated that when such an alloy is used as a structural material, its strength is insufficient. Also, according to the foregoing knowledge obtained in the experiments of this Invention made by the present inventors, there is nothing other than estimation that an alloy containing Ca in a high concentration Is low in the ductility.
  • Patent Document 5 discloses an Mg base alloy containing Mn and Zn as main components of additive materials, and in order to obtain a high strength, it is described to perform a solution heat treatment. However, there is involved such a problem that the process is complicated because, for example, an additional heat treatment of two-stage aging is required.
  • Patent Document 8 an alloy in which not more than 10 % by weight of Cu is added is developed. However, the addition of Cu encounters a defect that the corrosion resistance of the Mg alloy is remarkably lowered.
  • Mg-Al-Zn AZ based alloy
  • Mg-Zn-Zr ZK based alloy
  • the rare earth element is expensive, its multiplicity of use is low; and furthermore, the addition of large amounts of alloying elements is accompanied with the formation of a coarse compound phase and involves such a defect that though a high strength is obtained, the ductility is impaired. Then, the development of a new wrought Mg alloy which is free from a rare earth element and which is excellent in strength and ductility by the addition of inexpensive alloying elements is being demanded.
  • an object of this invention is to provide an Mg base alloy having not only a practically sufficient strength but good ductility at room temperature to an extent that it has hitherto been unable to be desired and having small anisotropy in strength characteristics.
  • An Mg base alloy of Invention 1 is characterized in that it consists of:
  • Invention 2 is characterized in that in the Mg base alloy as set forth in Invention 1, the crystal grain size thereof is from 0.1 ⁇ m to 25 ⁇ m.
  • the alloy of this invention has an average Schmid factor in the bottom slip direction against the load application direction of 0.2 or more and has uniform distribution of the Schmid factor as compared with extruded materials of the existing AZ91 alloy (Mg-9 mass % Al-1 mass % Zn alloy) which is a practical Mg alloy. Namely, the alloy of this invention is characterized in that a degree of integration of the bottom parallel to the extrusion direction is weak.
  • the alloy of this invention has such excellent mechanical properties that the compression proof stress is 75 % or more of the tensile proof stress and that anisotropy in strength is small.
  • age hardening properties are enhanced by adding trace amounts of Ag, Ca and Zr, each of which is free from a rare earth element and is relatively easily available. Also, it is noted that even by merely hot extruding the alloy, a fine grain structure having a fine precipitate dispersed therein is formed and that the subject alloy is an Mg base alloy which is excellent in not only strength but ductility and which has small anisotropy in strength as compared with the conventional alloys. Also, in view of the Examples and the technical common knowledge, it can be expected that the foregoing effects are displayed within the following ranges.
  • the maximum solubility of Zn in Mg is 2.4 at%.
  • the composition range of Zn is 0.75 at% or more, age hardening is achieved.
  • the Zn content is as high as possible, and the Zn content is preferably 1.52 at% or more.
  • the Zn content is preferably 1.92 at% or more.
  • an upper limit thereof is preferably 0.2 at%.
  • the Ag content is 0.08 at% or more
  • a work for promoting the formation of a nucleus of the precipitate is revealed, and therefore, a lower limit value thereof is 0.08 at% or more.
  • the maximum solubility of Ca in Mg is 0.82 at%.
  • an upper limit thereof is preferably 0.2 at%.
  • the Ca content is 0.08 at% or more, a work for promoting the formation of a nucleus of the precipitate is revealed, and therefore, a lower limit value thereof is 0.08 at% or more.
  • the maximum solubility of Zr in Mg is 1.04 at%.
  • the Zr content exceeds 0.17 at%, a peritectic reaction exists in the vicinity of 650°C, and a coarse precipitate is formed. Therefore, the Zr content was specified to be not more than 0.17 at%.
  • a lower limit of the Zr content is 0.08 at% or more.
  • the quenched material was aged at a temperature of 160°C and 200°C, respectively using an oil bath. Its hardness by aging was measured by a Vickers hardness meter under a condition at a load of 1 kg for a holding time of 15 seconds.
  • Figs. 2 and 3 show hardness changes in aging at 160°C and 200°C, respectively. From these figures, the hardness reaches the maximum at around 100 hours in the aging at 160°C and at around 10 hours in the aging at 200°C, respectively.
  • the age hardening properties become better by adding Ag, (Ag + Ca) or (Ag + Ca + Zr) to the Mg-2.3Zn alloy.
  • the maximum hardness of an alloy obtained by adding (Ag + Ca + Zr) to the Mg-2.3Zn alloy is the highest and reaches 100 Hv.
  • the grain size was measured by linear intercept method (ASTM standards E112).
  • the average grain size was about 100 ⁇ m in the Mg-2.3Zn binary alloy shown in Fig. 4 , about 50 ⁇ m in the Mg-2.3Zn-0.1Ag alloy shown in Fig. 5 , about 50 ⁇ m In the Mg-2.3Zn-0.1Ag-0.1Ca alloy shown in Fig. 6 and about 10 ⁇ m in the Mg-2.3Zn-0.1Ag-0.1Ca-0.17Zr alloy shown in Fig. 8 , respectively.
  • Ag or combined addition of (Ag + Ca)
  • the crystal grain size becomes small and that by the further addition of Zr, the grain size becomes finer.
  • FIG. 4 to 9 shows a TEM micrograph of each of the alloys at the peak aging stage when aged at 160°C.
  • This refinement of the precipitate is considered to cause an increase of the peak aging hardness.
  • Fig. 10 Details of experimental procedures are shown in Fig. 10 . Alloying elements were blended so as to have an alloy composition shown in Table 1 and melted and cast in a (CO 2 + SF 6 ) mixed gas atmosphere. Thereafter, the ingot was subjected to a homogenous heat treatment at 350°C for 48 hours. Thereafter, the ingot was hot extruded at 300°C and 350°C, respectively. With respect to the hot extrusion condition, an extrusion ratio was 20, and a ram rate was 0.1 mm/s. The material after extrusion was subjected to a solution heat treatment at 400°C for from 0.5 to 4 hours and then subjected to an aging treatment at a temperature of 160°C and 200°C, respectively, followed by measurement for a Vickers hardness.
  • a solution heat treatment at 400°C for from 0.5 to 4 hours and then subjected to an aging treatment at a temperature of 160°C and 200°C, respectively, followed by measurement for a Vickers hardness.
  • sample after extrusion was subjected to microstructure observation by an optical microscope and TEM.
  • Figs. 11 and 12 show an aging curve of an Mg-2.3 % Zn-0.1 % Ag-0.1 % Ca alloy at 16D°C and 200°C, respectively.
  • Figs. 13 and 14 show an aging curve of an Mg-2.3 % Zn-0.1 % Ag-0.1 % Ca-0.17 % Zr alloy at 160°C and 200°C, respectively.
  • Fig. 15 shows an optical micrograph structure of an Mg-2.3 % Zn-0.1 % Ag-0.1 % Ca alloy when hot extruded at 350°C.
  • the crystal grain size was measured by linear intercept method using this photograph. As a result, the average crystal grain size was 20 ⁇ m.
  • Fig. 16 shows an optical micrograph of an Mg-2.3 % Zn-0.1 % Ag-0.1 % Ca-0.17 % Zr alloy when hot extruded at 350°C.
  • Figs. 17 and 18 are each a TEM micrograph of the same alloy.
  • the structure after extrusion is classified into three of (A) a coarse unrecrystallized grain, (B) a fine equi-axed recrystallized grain and (C) an obscure region.
  • the obscure region (C) is considered to be corresponding to the TEM micrograph of Fig. 17 , and it is noted that the obscure region (C) is a fine grained recrystallized grain structure in a submicron order.
  • Fig. 18 shows enlargement of the interior of the fine grain in a submicron order, and fine rod-like precipitates of several tens nm as formed along the c-axis of Mg.
  • the grain size of the hot extruded Mg-2.3 % Zn-0.1 % Ag-0.1 % Ca-0.17 % Zr alloy was measured from Figs. 16 and 17 . Since the obtained structure was not homogenous, the major axis and the minor axis were measured for crystals of the respective regions without employing the linear intercept method, and an average value thereof was defined as the grain size. Also, with respect to the unrecrystallized grain (A) and the equi-axed recrystallized grain (B), the optical micrograph of Fig. 16 was used, and with respect to the fine grain region in a submicron order (C), the TEM micrograph of Fig. 17 was used.
  • the unrecrystallized grain (A) had size distribution of from about 5 to 25 ⁇ m and had an average grain size of 11 ⁇ m; the equl-axed recrystallized grain (B) had size distribution of from about 1 to 5 ⁇ m and had an average grain size of 2.8 ⁇ m; and the fine grain region in a submicron order (C) had size distribution of from about 0.1 to 1 ⁇ m and had an average grain size of 0.75 ⁇ m.
  • a tensile test at room temperature and a compression test at room temperature were executed in parallel to the extrusion direction.
  • a tensile specimen was a JIS 14B specimen and had a gauge length of 20 mm.
  • a compression specimen had a diameter of 9.5 mm and a height of 14.3 mm. The tensile test and the compression test were performed under a condition at an initial strain rate of 10 -3 s -1 .
  • Fig. 19 shows distribution of a Schmid factor in the basal slip direction against the tensile load application direction, namely the extrusion direction. Since the degree of integration of the basal texture parallel to the extrusion direction is weak, the Schmid factors of the alloys of this invention are uniformly distributed as compared with those of extruded materials of the existing AZ91 alloy (Mg-9 mass % Al-1 mass % Zn alloy), and an average value thereof is 0.20 or more.
  • Fig. 20 shows a stress-strain curve obtained by each of a tensile test and a compression test at room temperature of an Mg-2.3 % Zn-0.1 % Ag-0.1 % Ca-0.17 % Zr alloy as extruded at 350°C.
  • Tables 3 to 7 show measurement data corresponding to the stress-strain curve in the tensile test shown in Fig. 20 ; and
  • Tables 8 to 11 show measurement data corresponding to the stress-strain curve in the compression test shown in Fig. 20 .
  • Table 12 summarizes results obtained in a tensile test and a compression test regarding an Mg-2.3 % Zn-0.1 % Ag-0.1 % Ca alloy and an Mg-2.3 % Zn-0.1 % Ag-0.1 % Ca-0.17 % Zr alloy as extruded at 300°C and 350°C, respectively.
  • the hot extruded Mg-2.3 % Zn-0.1 % Ag-0.1 % Ca alloy and Mg-2.3 % Zn-0.1 % Ag-0.1 % Ca-0.17 % Zr alloy are a material having both high strength and high ductility and having small anisotropy in proof stress.
  • the material of this invention has high strength and high ductility and can be used for transportation equipment which is expected to realize weight reduction as a replacement for Al alloys, such as automobiles, motorcycles, aircrafts, etc. Furthermore, since the mechanical properties of the material of this Invention can be obtained without necessity of an additional heat treatment after the hot working, the material of this invention is also expected as a replacement for currently used wrought Mg alloys. Also, in view of the fact that the samples after hot extrusion at 350°C display an ultrafine grain structure of about 500 nm in terms of an average grain size, there is a possibility that the material of this Invention is applicable as a superplastic material.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Extrusion Of Metal (AREA)
  • Cell Electrode Carriers And Collectors (AREA)
  • Heat Treatment Of Steel (AREA)
  • Contacts (AREA)

Claims (2)

  1. Alliage à base de Mg constitué de :
    Zn en une quantité de 0,75 % at. à 2,4 % at. ;
    Ag en une quantité de 0,08 % at. à 1,98 % at. ;
    Ca en une quantité de 0,08 % at. à 0,61 % at. ;
    Zr en une quantité de 0,08 % at. à 0,17 % at., et
    le reste étant constitué de Mg et d'impuretés inévitables.
  2. Alliage à base de Mg tel que revendiqué dans la revendication 1, qui est caractérisé en ce qu'une granulométrie de celui-ci est de 0,1 µm à 25 µm.
EP08752560.6A 2007-05-09 2008-05-09 Alliage à base de mg Not-in-force EP2157201B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2007124879A JP2010047777A (ja) 2007-05-09 2007-05-09 Ｍｇ基合金
PCT/JP2008/058677 WO2008140062A1 (fr) 2007-05-09 2008-05-09 ALLIAGE À BASE DE Mg

Publications (3)

Publication Number Publication Date
EP2157201A1 EP2157201A1 (fr) 2010-02-24
EP2157201A4 EP2157201A4 (fr) 2014-07-09
EP2157201B1 true EP2157201B1 (fr) 2015-11-18

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EP08752560.6A Not-in-force EP2157201B1 (fr) 2007-05-09 2008-05-09 Alliage à base de mg

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US (1) US20100202916A1 (fr)
EP (1) EP2157201B1 (fr)
JP (2) JP2010047777A (fr)
KR (1) KR101561147B1 (fr)
WO (1) WO2008140062A1 (fr)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101899600B (zh) * 2010-08-13 2012-04-25 上海交通大学 骨科用镁合金内植入材料及其制备方法
KR101252784B1 (ko) * 2010-11-09 2013-04-11 도쿠리츠교세이호징 붓시쯔 자이료 겐큐키코 고강도 고성형성 마그네슘 합금 판재 및 그 제조방법
KR101303585B1 (ko) * 2010-11-23 2013-09-11 포항공과대학교 산학협력단 상온성형성이 우수한 마그네슘 합금 판재 및 그 제조방법
US9510932B2 (en) * 2011-10-06 2016-12-06 University Of Pittsburgh-Of The Commonwealth System Of Higher Education Biodegradable metal alloys

Family Cites Families (19)

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GB544351A (en) * 1940-10-04 1942-04-09 Dow Chemical Co Improved magnesium base alloys
GB987515A (en) * 1963-04-03 1965-03-31 Magnesium Elektron Ltd Improvements in or relating to magnesium base alloys
US4765954A (en) * 1985-09-30 1988-08-23 Allied Corporation Rapidly solidified high strength, corrosion resistant magnesium base metal alloys
JP2725112B2 (ja) 1992-03-25 1998-03-09 三井金属鉱業株式会社 高強度マグネシウム合金
JPH08134581A (ja) * 1994-11-14 1996-05-28 Mitsui Mining & Smelting Co Ltd マグネシウム合金の製造方法
JP2001239326A (ja) 2000-02-28 2001-09-04 Mitsui Mining & Smelting Co Ltd マグネシウム材製品の製造方法
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JP2002212662A (ja) 2001-01-19 2002-07-31 Aisin Takaoka Ltd マグネシウム合金
JP2003226929A (ja) 2002-02-01 2003-08-15 Kasatani:Kk マグネシウム合金材の冷間プレス成形方法
JP2003328064A (ja) 2002-05-10 2003-11-19 Toyo Kohan Co Ltd 成形性に優れる展伸用マグネシウム薄板およびその製造方法
JP4064720B2 (ja) 2002-05-10 2008-03-19 東洋鋼鈑株式会社 成形性に優れる展伸用マグネシウム薄板およびその製造方法
WO2004085689A1 (fr) * 2003-03-25 2004-10-07 Yoshihito Kawamura Alliage de magnesium de haute resistance et tenacite, et son procede de production
JP2005113235A (ja) 2003-10-09 2005-04-28 Toyota Motor Corp 高強度マグネシウム合金およびその製造方法
EP1690954B1 (fr) * 2003-11-26 2014-10-08 KAWAMURA, Yoshihito Alliage de magnesium haute resistance et haute tenacite et son procede de production
JP4840751B2 (ja) 2004-06-30 2011-12-21 独立行政法人物質・材料研究機構 高強度マグネシウム合金及びその製造方法
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Also Published As

Publication number Publication date
US20100202916A1 (en) 2010-08-12
KR101561147B1 (ko) 2015-10-16
EP2157201A1 (fr) 2010-02-24
JPWO2008140062A1 (ja) 2010-08-05
KR20100021563A (ko) 2010-02-25
JP2010047777A (ja) 2010-03-04
WO2008140062A1 (fr) 2008-11-20
EP2157201A4 (fr) 2014-07-09
JP5404391B2 (ja) 2014-01-29

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