WO2012133522A1 - マグネシウム合金 - Google Patents

マグネシウム合金 Download PDF

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Publication number
WO2012133522A1
WO2012133522A1 PCT/JP2012/058113 JP2012058113W WO2012133522A1 WO 2012133522 A1 WO2012133522 A1 WO 2012133522A1 JP 2012058113 W JP2012058113 W JP 2012058113W WO 2012133522 A1 WO2012133522 A1 WO 2012133522A1
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WO
WIPO (PCT)
Prior art keywords
mass
content
magnesium alloy
aluminum
calcium
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Application number
PCT/JP2012/058113
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English (en)
French (fr)
Japanese (ja)
Inventor
勤二 平井
東　健司
順庸 瀧川
徳照 上杉
Original Assignee
株式会社新技術研究所
公立大学法人大阪府立大学
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Application filed by 株式会社新技術研究所, 公立大学法人大阪府立大学 filed Critical 株式会社新技術研究所
Priority to US14/008,280 priority Critical patent/US20140044586A1/en
Priority to EP12765196.6A priority patent/EP2692884B1/en
Priority to CN201280015541.0A priority patent/CN103635598A/zh
Publication of WO2012133522A1 publication Critical patent/WO2012133522A1/ja

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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 high-strength and high heat-resistant magnesium alloy that can be processed into a wrought material such as extrusion and forging.
  • Magnesium is known to be the lightest and highest specific strength among practical metals. For example, as a measure against global warming, parts that have been reduced in weight using a magnesium alloy to reduce the carbon dioxide emissions by reducing the weight of the vehicle and to increase the distance that can be traveled by one charge of an electric vehicle. Magnesium alloys are increasingly used in many applications, such as being applied. Magnesium alloy parts are often formed by casting or die casting.
  • Patent Document 1 discloses that a crushed intermetallic compound is uniformly dispersed in crystal grains to improve mechanical strength.
  • the magnesium alloy according to Patent Document 1 has a problem that heat resistance, that is, strength at a high temperature may still be insufficient.
  • the magnesium alloy according to the cited document 2 needs to suppress the hot rolling and forging degree of work (rolling ratio) to a low value. There was a problem that the strength may not be sufficient.
  • the present invention has been made for the purpose of meeting such a demand, and therefore an object of the present invention is to provide a magnesium alloy having a sufficiently high strength at room temperature and high temperature.
  • Embodiment 1 of the present invention aluminum (Al): 14.0 to 23.0 mass%, calcium (Ca): 11.0 mass% or less (not including 0 mass%), strontium (Sr): 12.0 A magnesium alloy characterized by containing not more than mass% (not including 0 mass%) and zinc (Zn): 0.2 to 1.0 mass%.
  • Aspect 2 of the present invention includes silicon (Si): 0.1 to 1.5 mass%, rare earth (RE): 0.1 to 1.2 mass%, zirconium (Zr): 0.2 to 0.8 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 ): 0.2-3.0% by mass and antimony (Sb): at least one selected from the group consisting of 0.1-1.5% by mass Magnesium alloy.
  • Aspect 3 of the present invention is characterized in that the ratio of the content of strontium (Sr) to the content of calcium (Ca) is 1: 0.3 to 1: 1.5 by mass ratio.
  • Aspect 4 of the present invention is characterized in that the content of aluminum (Al), the content of calcium (Ca), and the content of strontium (Sr) satisfy the relationship represented by the following formula (1).
  • a magnesium alloy according to any one of embodiments 1 to 3. 0.8 ⁇ ⁇ Al> ⁇ 1.35 ⁇ ⁇ Ca> + 1.23 ⁇ ⁇ Sr> + 8.5 ⁇ 1.2 ⁇ ⁇ Al> (1)
  • ⁇ Al> is the content of aluminum (Al) expressed in mass%
  • ⁇ Ca> is the content of calcium (Ca) expressed in mass%
  • ⁇ Sr> is expressed in mass%.
  • Aspect 5 of the present invention is the magnesium alloy according to any one of aspects 1 to 4, characterized in that precipitates containing Al 2 Ca and Al 4 Sr are precipitated at crystal grain boundaries with a space between each other. is there.
  • the present invention makes it possible to provide a magnesium alloy having sufficient room temperature strength and sufficient high temperature strength.
  • FIG. 1 shows the metal structure observed with a confocal laser microscope
  • FIG. 1 (a) shows the metal structure of the extruded material
  • FIG. 1 (b) shows the metal structure of the homogenized heat-treated material at 400 ° C. for 48 hours
  • FIG. 1 (c) shows the metal structure of the heat treatment material homogenized at 420 ° C. ⁇ 48 hours.
  • FIG. 2 shows the high-temperature tensile test results (true stress-true strain diagram) at 150 ° C. of the extruded material, 400 ° C. ⁇ 48 hours homogenized heat-treated material, and 420 ° C. ⁇ 48 hours homogenized heat-treated material.
  • FIG. 3 shows the measurement results of the tensile strength at room temperature.
  • FIG. 4 shows the measurement results of the high temperature tensile strength.
  • the inventors of the present application have studied the simultaneous utilization of both solid solution strengthening and precipitation strengthening, which is known as a strengthening mechanism of magnesium alloy. That is, it was investigated that both the solid solution strengthening mechanism and the precipitation strengthening mechanism are effectively operated by appropriately controlling the contents of aluminum, strontium, and calcium.
  • the magnesium alloy according to the present invention has aluminum (Al): 14.0 to 23.0 mass%, calcium (Ca): 11 mass% or less (not including 0 mass%), strontium (Sr): 12 mass% or less. (Not including 0% by mass), zinc (Zn): 0.2 to 1.0% by mass.
  • the second phase containing Ca and Al 4 Sr breaks (breaks) and aligns in the deformation direction.
  • Such precipitates containing Al 2 Ca and Al 4 Sr aligned in the deformation direction contribute to the improvement of the high-temperature strength.
  • the present inventors have been able to reprecipitate and disperse the second phase particles containing Al 2 Ca and Al 4 Sr by performing a homogenization heat treatment at 350 to 450 ° C. It has been found that the strength can be improved. More preferably, by performing a homogenization heat treatment at 385 ° C. to 415 ° C., the second phase containing Al 2 Ca and Al 4 Sr can be uniformly dispersed in the crystal grain boundaries, and the strength is more reliably increased. It turns out that you can.
  • the inventor of the present application has further studied, and the maximum solid solution amount (solid solution limit) of aluminum in the matrix of the sample subjected to the homogenization heat treatment at 400 ° C. for 48 hours after plastic processing such as extrusion is 8.3 mass%. (7.5 at%).
  • the measurement was performed by point analysis using an electron beam microanalyzer (EPMA).
  • the amount of aluminum in the magnesium alloy according to the present invention is appropriate from 14.0 to 23.0 mass%. If aluminum is 14.0% by mass or more, even if about 8.5% by mass of aluminum is dissolved in the matrix, a sufficient amount of aluminum is sufficient for calcium, strontium, and intermetallic compounds Al 2 Ca and Al 4 Sr. It is because it can form. Moreover, if aluminum content is 23.0 mass% or less, ductility, such as elongation, is securable.
  • the amount of aluminum is 15.0% by mass to 20.0% by mass. This is because within this range, the intermetallic compounds Al 2 Ca and Al 4 Sr can be formed more reliably and the ductility can be ensured.
  • the calcium content is 11.0% by mass or less (not including 0% by mass).
  • 0% by mass is excluded so that calcium is always contained.
  • calcium is 1.0 to 8.0% by mass. This is because Al 2 Ca can be formed more reliably and can be prevented from becoming excessive.
  • strontium The content of strontium is 12.0% by mass or less (not including 0% by mass).
  • 0% by mass is excluded so that strontium is always contained.
  • the strontium is 0.5 to 8.0% by weight. This is because Al 4 Sr can be formed more reliably and the surplus can be suppressed. More preferably, the content is 1.0 to 6.0% by mass. This is because the effect of strontium can be maximized.
  • the magnesium alloy according to the present invention contains 0.2 to 1.0% by mass of zinc (Zn). This is because zinc has the effect of improving strength and improving castability.
  • the strontium and calcium contained are all precipitated as Al 2 Ca and Al 4 Sr, respectively, as shown in (2)
  • the amount of aluminum (mass%) represented by y in the formula is required.
  • ⁇ Ca> is the calcium content expressed in mass%
  • ⁇ Sr> is the strontium content expressed in mass%.
  • the physical meaning of the numbers in the formula is shown in parentheses after the numbers.
  • the amount of aluminum y represented by the formula (2) necessary for precipitation of strontium and calcium as Al 2 Ca and Al 4 Sr is 0.8 to 1.2 times the aluminum content, respectively. It is preferable to contain aluminum so that it may fall within the range.
  • Al 2 Ca and Al 4 Sr which are almost the same as the stoichiometric composition, are precipitated with almost no excess or deficiency of any element of aluminum, calcium and strontium, In addition, aluminum is sufficiently dissolved in the matrix.
  • ⁇ Al> is the aluminum content expressed in mass%.
  • the alloy of the present invention contains the aforementioned aluminum, calcium, strontium and zinc, and the balance may be composed of magnesium (Mg) and inevitable impurities.
  • the magnesium alloy preferably contains 40% by mass or more, more preferably 50% by mass or more, so as not to lose characteristics such as high specific strength.
  • Silicon forms an intermetallic compound with magnesium, and since the obtained intermetallic compound is stable at high temperatures, it is possible to effectively suppress grain boundary sliding and improve heat resistance in deformation at high temperatures. If the silicon content is 0.1 to 1.5% by mass, the effect can be sufficiently exerted.
  • Rare earth forms an intermetallic compound with magnesium, and since the obtained intermetallic compound is stable at high temperature, it is possible to effectively suppress grain boundary slip and improve heat resistance in deformation at high temperature. If the rare earth content is 0.1 to 1.2% by mass, the effect can be sufficiently exerted.
  • Zirconium forms an intermetallic compound with magnesium, and since the obtained intermetallic compound is stable at high temperatures, it is possible to effectively suppress grain boundary sliding and improve heat resistance in deformation at high temperatures. If the zirconium content is 0.2 to 0.8 mass%, the effect can be sufficiently exhibited.
  • Scandium when added to magnesium, has the effect of lowering stacking fault energy and reducing the deformation rate at high temperatures. If the content of scandium is 0.2 to 3.0% by mass, the effect can be sufficiently exerted.
  • Yttrium when added to magnesium, has the effect of lowering the stacking fault energy and lowering the deformation rate at high temperatures. If the yttrium content is 0.2 to 3.0% by mass, the effect can be sufficiently exerted.
  • tin When tin is added to magnesium, it has the effect of lowering stacking fault energy and reducing the deformation rate at high temperatures. If the content of tin is 0.2 to 3.0% by mass, the effect can be sufficiently exerted.
  • Barium when added to magnesium, has the effect of lowering the stacking fault energy and reducing the deformation rate at high temperatures. If the barium content is 0.2 to 3.0% by mass, the effect can be sufficiently exerted.
  • Antimony when added to magnesium, has the effect of lowering the stacking fault energy and lowering the deformation rate at high temperatures. If the content of scandium is 0.1 to 1.5% by mass, the effect can be sufficiently exerted.
  • the 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. after the plastic working. It has been found that the high temperature strength can be further improved. Accordingly, the magnesium alloy according to the present invention (magnesium alloy article (stretched material)) is preferably subjected to a homogenization heat treatment at 350 to 450 ° C. after plastic working. The homogenization heat treatment at 350 to 450 ° C. is preferably maintained in this temperature range for 24 to 72 hours. This is because the precipitate is re-dissolved (re-deposited) and the thermal stability is improved by this treatment.
  • the inventor of the present application can re-precipitate and disperse the second phase particles containing Al 2 Ca and Al 4 Sr uniformly along the grain boundaries by performing a homogenization heat treatment at 385 ° C. to 415 ° C.
  • the present inventors have found that the high temperature strength can be further improved.
  • the second phase particles (precipitates) containing Al 2 Ca and Al 4 Sr are not mesh-like but spaced apart from each other (ie, discontinuous) ) Along the grain boundaries, and this form of precipitate greatly contributes to the improvement of high-temperature strength.
  • the magnesium alloy (magnesium alloy article (stretched material)) according to the present invention is more preferably subjected to homogenization heat treatment at 385 to 415 ° C. after plastic working.
  • the homogenization heat treatment at 385 to 415 ° C. is preferably maintained in this temperature range for 24 to 72 hours. By this treatment, precipitates are re-dissolved to make the structure uniform, and the intermetallic compound structure having high thermal stability at the grain boundary can be made uniform and stabilized.
  • plastic working here includes various types of hot and cold plastic working.
  • plastic working include extrusion, rolling, forging, drawing, swaging, and combinations thereof.
  • Example 1 An alloy sample having components shown in Table 1 was prepared. About the value of y shown in the formula (2) of the example samples (Example 1 and Example 2) shown in Table 1, Example 1 is 15.5, Example is 20.9, The expression (1) is satisfied. In both Example 1 and Example 2, the ratio of calcium content: strontium content is 1: 1 by mass ratio.
  • the alloy sample was melted at 700 ° C. and cast into a billet with a cylindrical mold.
  • the cast billet was heated to 400 ° C. at a temperature rising rate of 0.5 ° C./min, held for 48 hours, and then cooled with water.
  • extrusion was performed at an extrusion temperature of 350 ° C., an extrusion speed of 0.2 mm / second, and an extrusion ratio of 16 to obtain a round bar (diameter 10 mm).
  • Example 1 1) Homogenization heat treatment
  • the sample (extruded round bar) of Example 1 described above was subjected to a homogenization heat treatment at 400 ° C. for 48 hours while being extruded, and 420 ° C. ⁇ 48.
  • a material subjected to a homogenized heat treatment over time was produced.
  • FIG. 1 shows the metal structure observed with a confocal laser microscope
  • FIG. 1 (a) shows the metal structure of the extruded material
  • FIG. 1 (b) shows the metal structure of the homogenized heat-treated material at 400 ° C. for 48 hours
  • FIG. 1 (c) shows the metal structure of the heat treatment material homogenized at 420 ° C. ⁇ 48 hours.
  • precipitates (second phase) containing Al 2 Ca and Al 4 Sr are divided and aligned in the extrusion direction (vertical direction in the figure).
  • the 400 ° C. ⁇ 48 hour homogenized heat treatment material and the 420 ° C.
  • FIG. 2 shows the high-temperature tensile test results (true stress-true strain diagram) at 150 ° C. of the extruded material, 400 ° C. ⁇ 48 hours homogenized heat-treated material, and 420 ° C. ⁇ 48 hours homogenized heat-treated material.
  • the tensile test was performed at a temperature of 150 ° C. and a tensile speed of 1 ⁇ 10 ⁇ 3 / sec.
  • All samples show excellent high-temperature strength (heat resistance) with a tensile strength at 250 ° C. of 250 MPa.
  • the 400 ° C. ⁇ 48 hour homogenized heat treated material and the 420 ° C. ⁇ 48 hour homogenized heat treated material show higher high-temperature strength than the extruded material.
  • the heat-treated material homogenized at 400 ° C. ⁇ 48 hours has an extremely high high-temperature strength exceeding 300 MPa.
  • Crystal grain size measurement result Table 2 shows the crystal grain size of each alloy sample.
  • the crystal grain size was measured by an EBSD (Electron back scattered diffraction patterns) method.
  • a crystal grain was defined with a deviation of orientation of 15 ° or more as a grain boundary.
  • the average grain size was determined by simply dividing the total area by the number of grains.
  • FIG. 3 shows the measurement results of the tensile strength at room temperature. The measurement results of tensile strength, 0.2% proof stress and elongation of each alloy sample are shown. In Comparative Examples 2 and 3, the material was brittle and the 0.2% proof stress could not be measured.
  • Comparative Example 1 As for the tensile strength, Comparative Example 1, Example 1 and Example 2 showed excellent values of 300 MPa or more. However, it can be seen that Comparative Example 1 has a 0.2% proof stress of less than 250 MPa, and Examples 1 and 2 having a 0.2% proof stress of 250 MPa or more are superior in room temperature strength to the comparative sample. Regarding the elongation, Example 1 and Example 2 are 2% or more, and it can be seen that they have sufficient ductility. Further, the tensile strength of a sample prepared by extruding an AZ91 alloy known as a high-strength magnesium alloy at an extrusion temperature of about 360 ° C. and an extrusion ratio of about the same as those of Examples 1 and 2 is 295 MPa. (Hanlin Ding et.al, Journal of alloys and compounds, 456 (2008) 400-406), it can be seen that the samples of Examples 1 and 2 also have high room temperature strength.
  • FIG. 4 shows the measurement results of high temperature tensile strength.
  • the high temperature tensile test was performed at a measurement temperature of 175 ° C. and a strain rate of 1 ⁇ 10 ⁇ 4 / sec.
  • the sample of Comparative Example 3 was not able to measure the high-temperature strength because it was fractured soon after applying a tensile stress.
  • the high temperature strength at 175 ° C. was 210 MPa or more, which was higher than that of the comparative example.
  • the example samples exhibit high strength at both room temperature and high temperature.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
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  • Crystallography & Structural Chemistry (AREA)
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PCT/JP2012/058113 2011-03-29 2012-03-28 マグネシウム合金 WO2012133522A1 (ja)

Priority Applications (3)

Application Number Priority Date Filing Date Title
US14/008,280 US20140044586A1 (en) 2011-03-29 2012-03-28 Magnesium alloy
EP12765196.6A EP2692884B1 (en) 2011-03-29 2012-03-28 Magnesium alloy
CN201280015541.0A CN103635598A (zh) 2011-03-29 2012-03-28 镁合金

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JP2011072505A JP5729081B2 (ja) 2011-03-29 2011-03-29 マグネシウム合金
JP2011-072505 2011-03-29

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EP (1) EP2692884B1 (zh)
JP (1) JP5729081B2 (zh)
CN (1) CN103635598A (zh)
TW (1) TWI519649B (zh)
WO (1) WO2012133522A1 (zh)

Cited By (1)

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Publication number Priority date Publication date Assignee Title
WO2018012602A1 (ja) * 2016-07-15 2018-01-18 住友電気工業株式会社 マグネシウム合金

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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
US10947609B2 (en) * 2015-12-28 2021-03-16 Korea Institute Of Materials Science Magnesium alloy having excellent mechanical properties and corrosion resistance and method for manufacturing the same
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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Cited By (3)

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Publication number Priority date Publication date Assignee Title
WO2018012602A1 (ja) * 2016-07-15 2018-01-18 住友電気工業株式会社 マグネシウム合金
JP6329714B1 (ja) * 2016-07-15 2018-05-23 住友電気工業株式会社 マグネシウム合金
US10808302B2 (en) 2016-07-15 2020-10-20 Sumitomo Electric Industries, Ltd. Magnesium alloy

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JP5729081B2 (ja) 2015-06-03
EP2692884A4 (en) 2014-11-19
TWI519649B (zh) 2016-02-01
US20140044586A1 (en) 2014-02-13
CN103635598A (zh) 2014-03-12
TW201307580A (zh) 2013-02-16
EP2692884A1 (en) 2014-02-05
EP2692884B1 (en) 2017-05-03
JP2012207253A (ja) 2012-10-25

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