EP3572542A1 - Magnesiumlegierung und verfahren zur herstellung einer magnesiumlegierung - Google Patents

Magnesiumlegierung und verfahren zur herstellung einer magnesiumlegierung Download PDF

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Publication number
EP3572542A1
EP3572542A1 EP18761653.7A EP18761653A EP3572542A1 EP 3572542 A1 EP3572542 A1 EP 3572542A1 EP 18761653 A EP18761653 A EP 18761653A EP 3572542 A1 EP3572542 A1 EP 3572542A1
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EP
European Patent Office
Prior art keywords
magnesium alloy
treatment
set forth
solution
temperature
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Granted
Application number
EP18761653.7A
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English (en)
French (fr)
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EP3572542A4 (de
EP3572542B1 (de
Inventor
Ming-Zhe BIAN
Taisuke Sasaki
Kazuhiro Hono
Byeongchan SUH
Shigeharu Kamado
Taiki Nakata
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National Institute for Materials Science
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National Institute for Materials Science
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Priority claimed from PCT/JP2018/006088 external-priority patent/WO2018159394A1/ja
Publication of EP3572542A1 publication Critical patent/EP3572542A1/de
Publication of EP3572542A4 publication Critical patent/EP3572542A4/de
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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
    • 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
    • C22C—ALLOYS
    • C22C23/00—Alloys based on magnesium
    • C22C23/04—Alloys based on magnesium with zinc or cadmium 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
    • C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
    • 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 and a method for manufacturing the same.
  • the magnesium alloy of the present invention is an alloy containing 0.2 to 2 wt% of Al, 0.2 to 1 wt% of Mn, 0.2 to 2 wt% of Zn, and at least 0.2 to 1 wt% of Ca, and the remainder comprises Mg and unavoidable impurities.
  • Al content in the magnesium alloy of the present invention fall within a range from 0.2 wt% or more to 2 wt% or less. If the Al content is low, useful precipitates, which will be described later, cannot be obtained easily. Meanwhile, if it is too high, precipitated phase changes into coarse precipitates such as Al 2 Ca phase ineffective for strengthening, which is undesirable.
  • a sheet-shaped material is produced by working the homogenized ingot into a sheet material by warm rolling.
  • the rolling is performed to roll the homogenized ingot into a sheet material by setting the rolling conditions such as sample temperature, roll temperature, roll speed, circumferential rolling speed, number of passes, existence of intermediate heat treatment of the sample, and temperature and duration of intermediate heat treatment.
  • the sample temperature and rolling temperature may be made to be as low as possible, provided that the sample is not cracked during rolling.
  • the rolling rate may also be made to be as large as possible, provided that the sample is not cracked during rolling.
  • the intermediate heat treatment of the sample is a heat treatment performed in the middle of rolling, and can be performed at a high temperature within a range that does not allow cracks and incipient melting to occur.
  • the hot or warm working is not particularly limited to rolling only, but any extending processing is allowed, provided that a microstructure can be produced. Any methods including twin roll casting rolling, forging, and extrusion processing are allowed.
  • the solution treatment is performed at a temperature ranging from 350°C to 500°C depending on the material and by maintaining the solution treatment period of 15 minutes to 24 hours. Note that it is not necessary to perform the treatment for unnecessarily long period because prolonged heat treatment results in increase in the manufacturing cost.
  • process 5 by subjecting the solution treated sample to age-hardening treatment by the heat treatment, precipitates formed on the solution treated sample having undergone solution treatment are made to disperse to enhance its strength, thus producing the magnesium alloy of the present invention.
  • the aging treatment which has never been performed with conventional commercial magnesium alloys, significant enhancement in strength of the magnesium alloy can be achieved.
  • magnesium alloy and the method for manufacturing the same as described above by performing solution treatment after rolling, grains can be oriented at random, which ensures excellent formability. By randomly orienting the grains, the strength suddenly decreases, but it is possible to ensure formability, strength, and ductility at the same time by forming nano-sized precipitates by the aging treatment.
  • a highly versatile magnesium alloy that satisfies both formability and strength within a temperature range including room temperature can be obtained.
  • strength and room temperature formability which are required as applicable mechanical properties, can be achieved.
  • an alloy having the composition of Mg-1.2Al-0.3Ca-0.4Mn-0.3Zn as shown by A-1 in Table 1 was produced as a cast ingot by melting and casting it into a mold.
  • the thickness of the cast ingot was approximately 10 mm.
  • the final rolling process was performed while intermediate heat treatment was conducted by using rolling mill whose circumferential rolling speed was 2 m/min as shown in Table 1.
  • the sample temperature and the roll temperature were set to 100°C, and the sample was made to pass through the rolling mill 6 times at the 23% thickness reduction per pass.
  • FIG. 3 shows the tensile stress-strain curves of the material having undergone solution treatment in process 4 (T4), which is the solution treated sample, and the material having undergone aging treatment in process 5 (T6).
  • T4 the solution treated sample
  • T6 the material having undergone aging treatment in process 5
  • FIGs. 4 (a), 4 (b) and 4 (c) show images of the material having undergone aging treatment in Example 1 observed under a transmission electron microscope, wherein FIG. 4 (a) is a Bright field TEM image, FIG. 4 (b) is a selected area diffraction image obtained from [011 (bar)0], [112 (bar)0] zone axis, and FIG. 4 (c) is a chart showing a three-dimensional atom map.
  • the transmission electron microscope by FEI Tian, G2 80-200 was used.
  • process 1 as shown in A-2 in Table 1, an alloy having a structure of Mg-1.2A1-0.3Ca-0.4Mn-0.3Zn was melted and casted in a mold to create a cast ingot, with the rolling temperature in the final rolling process set to 200°C.
  • process 5 as shown in Table 3, the aging temperature was set to 450°C and the aging time was set to 2 hours.
  • a magnesium alloy was manufactured in the same manner as Example 1 except the above.
  • Tables 2 and 3 show the manufacturing conditions and the mechanical properties of the obtained solid as well as the features of the microstructure. As apparent from Tables 2 and 3, the obtained magnesium alloy was confirmed to ensure both formability and strength even if the rolling conditions and aging conditions were varied.
  • a homogenized ingot was produced by melting and casting in a mold an alloy having the composition of Mg-1.2Al-0.5Ca-0.4Mn-0.3Zn in process 1, as shown in B-1 in Table 1, maintaining the cast ingot at 300°C for 4 hours in process 2, then increasing the temperature to 450°C at the heating rate of 7.5°C/, maintaining it for 6 hours, and then water-quenching it down to a room temperature, thus performing the homogenization treatment.
  • the magnesium alloy was manufactured in the same manner as Example 1 except that the sample reheating temperature in the final rolling process in process 3 was set to 450°C, and the aging time in process 5 set to 0.25 as shown in Table 3.
  • Tables 2 and 3 and FIGs. 6 to 8 show the manufacturing conditions and the mechanical properties of the obtained solid as well as the features of the microstructure.
  • the yield strength of the material having undergone solution treatment exhibited the excellent formability at room temperature, the yield strength being 142 MPa and the Index Erichsen value being 7.5 mm.
  • the aging treatment then performed significantly increased the yield strength up to 201 MPa.
  • Tables 2 and 3 show the manufacturing conditions and the mechanical properties of the obtained solid as well as the features of the microstructure. As apparent from Tables 2 and 3, the magnesium alloy, that achieves formability in a temperature range around room temperatures, thus ensuring both formability and strength, was obtained.
  • the sample reheating temperature in process 3 was set to 450°C, the solution treatment temperature was set to 350°C, and the duration of solution treatment was set to 4 hours, as shown in Table 2, when a solution treated sample was produced by subjecting the material to solution treatment in process 4, and the aging temperature was set to 200°C and aging time was set to 2 hours in process 5 as shown in Table 3.
  • FIG. 9 shows an optical microscope image of the material having undergone solution treatment, which is the solution treated sample.
  • the grain size was calculated by the linear interception method to be 10.7 ⁇ m.
  • FIG. 10 shows the
  • the magnesium alloy that achieves both formability and strength within a temperature range around room temperatures was obtained.
  • a magnesium alloy was manufactured in the same manner as Example 10 except that the sample temperature and the rolling temperature in the final rolling process in process 1 were set to 200°C as shown in C-2 in Table 1.
  • Tables 2 and 3 show the manufacturing conditions and mechanical properties of the obtained solid as well as the features of the microstructure. As apparent from Tables 2 and 3, the formability within a temperature range around room temperatures was ensured as in the case of Example 10, meaning that the magnesium alloy that achieves both formability and strength was obtained.
  • FIG. 12 shows an optical microscope image of the material having undergone solution treatment, which is the solution treated sample.
  • the grain size was calculated by the linear interception method to be 8.5 ⁇ m.
  • FIG. 13 shows the (0002) pole figure obtained by the X-ray diffraction of the material having undergone solution treatment.
  • the basal texture intensity of the (0002) pole was 3.7 mrd.
  • FIG. 14 shows tensile stress-strain curves of the material having undergone solution treatment (T4), which is the solution treated sample in process 4, and the material having undergone aging treatment (T6) in process 5.
  • Table 3 shows the 0.2% proof strength, the tensile strength and the elongation, all of which were read from the tensile stress-strain curves, and the Index Erichsen value.
  • the material having undergone solution treatment exhibited the excellent room temperature formability, its yield strength being 160 MPa and the Index Erichsen value being 8.3 mm. The yield strength did not increase much even if the aging treatment was performed.
  • the magnesium alloy that can achieve both formability and strength in a temperature range around room temperatures was obtained.
  • FIG. 17 shows tensile stress-strain curves of the material having undergone solution treatment (T4), which is the solution treated sample in process 4 and the material having undergone aging treatment in process 5 (T6).
  • Table 3 shows the 0.2% proof strength, the tensile strength, and the elongation, all of which were read from the tensile stress-strain curves, and the Index Erichsen value.
  • the yield strength of the material having undergone solution treatment was 149 MPa and its Index Erichsen value was 6.4 mm. Therefore, the formability was insufficient as apparent from Table 2.
  • a magnesium alloy was manufactured in the same manner as Comparative Example 1 except that the solution treatment temperature was set to 450°C when the solution treated sample was produced by subjecting a material to solution treatment in process 4 as shown in Table 2 and that the duration of solution treatment was set to 0.17 hours.
  • a magnesium alloy was manufactured in the same manner as Comparative Example 1 except that the solution treatment temperature was set to 500°C when the solution treated sample was produced by subjecting a material to solution treatment in process 4 as shown in Table 2 and that the duration of solution treatment was set to 1 hour.
  • Table 2 shows the manufacturing conditions and the mechanical properties of the obtained solid as well as the features of the microstructure. As shown in Table 2, the Index Erichsen value of the material having undergone solution treatment in Comparative Example 3 was 5.6 mm, exhibiting that the formability was obviously insufficient.
  • a magnesium alloy was manufactured in the same manner as Comparative Example 1 except that the solution treatment temperature was set to 500°C when a solution treated sample was produced by subjecting the material to solution treatment in process 4 as shown in Table 2 and that the duration of solution treatment was set to 24 hours.
  • Table 2 shows the manufacturing conditions and the mechanical properties of the obtained solid as well as the features of the microstructure. As apparent from Table 2, the grain size was excessively large and the 0.2% proof strength was insufficient.
  • a magnesium alloy was manufactured in the same manner as Comparative Example 1 except that the sample temperature and the rolling temperature in the final rolling process were set to 200°C when a material was produced by subjecting a homogenized ingot to rolling treatment in process 3 as shown in A-2 in Table 1 and that the solution treatment temperature was set to 450°C and the duration of solution treatment was set to 4 hours in process 4 as shown in Table 2.
  • a magnesium alloy was manufactured in the same manner as Comparative Example 1 except that the sample temperature and the rolling temperature in the final rolling process were set to 300°C when a material is produced by subjecting a homogenized ingot to rolling treatment in process 3 as shown in A-3 in Table 1 and that the solution treatment temperature was set to 450°C and the duration of solution treatment was set to 1 hour (Comparative Example 6), 2 hours (Comparative Example 7), and 4 hours (Comparative Example 8) in process 4 as shown in Table 2.
  • Table 2 shows the manufacturing conditions and the mechanical properties of the obtained solid as well as the features of the microstructure.
  • the Index Erichsen value in each of Comparative Examples, 6, 7, and 8 was as small as 6.3 mm, 5.4 mm, and 5.3 mm respectively, exhibiting that the grain size was large and thus the formability was insufficient.
  • a magnesium alloy was produced in the same manner as Comparative Example 1 except that the sample temperature and the rolling temperature in the final rolling process were set to 300°C when a material was produced by subjecting a homogenized ingot to rolling treatment in process 3 as shown in A-4 in Table 1, hot or warm treatment was performed without reheating the sample, and that the solution treatment temperature was set to 450°C and the duration of solution treatment to 1 hour (Comparative Example 9), 2 hours (Comparative Example 10), and 4 hours (Comparative Example 11) in process 4 as shown in Table 2.
  • Table 2 shows the manufacturing conditions and the mechanical properties of the obtained solid as well as the features of the microstructure.
  • the Index Erichsen value in Comparative Examples 9, 10, and 11 was as small as 5.3 mm, 6.2 mm, and 5.9 mm respectively, exhibiting that the grain size was large and thus the formability was insufficient.
  • a homogenized ingot was produced by melting and casting in a mold an alloy having the composition of Mg-1.2Al-0.5Ca-0.4Mg-0.3Zn to produce a cast ingot in process 1 as shown in B-2 in Table 1, maintaining the cast ingot at 300°C for 4 hours, then increasing the temperature to 450°C at the heating rate of 7.5°C/h, maintaining it for 6 hours, and then water-quenching it down to a room temperature as the homogenized treatment in process 2.
  • a magnesium alloy was manufactured in the same manner as Comparative Example 1 except that the sample temperature and the rolling temperature in the final rolling process were set to 200°C in process 3 and that the solution treatment temperature was set to 350°C and the duration of solution treatment to 1 hour when a solution treated sample was produced by subjecting a material to solution treatment in process 4 as shown in Table 2.
  • Table 2 shows the manufacturing conditions and the mechanical properties of the obtained solid as well as the features of the microstructure. As shown in Table 2, the Index Erichsen value of the material having undergone solution treatment in Comparative Example 12 was 5.8 mm, exhibiting that the formability was obviously insufficient.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
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  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
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  • Shaping Metal By Deep-Drawing, Or The Like (AREA)
EP18761653.7A 2017-02-28 2018-02-20 Magnesiumlegierung und verfahren zur herstellung dieser legierung Active EP3572542B1 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP2017037769 2017-02-28
JP2018027358A JP7116394B2 (ja) 2017-02-28 2018-02-19 マグネシウム合金及びマグネシウム合金の製造方法
PCT/JP2018/006088 WO2018159394A1 (ja) 2017-02-28 2018-02-20 マグネシウム合金及びマグネシウム合金の製造方法

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EP3572542A1 true EP3572542A1 (de) 2019-11-27
EP3572542A4 EP3572542A4 (de) 2020-10-28
EP3572542B1 EP3572542B1 (de) 2023-10-11

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108570583A (zh) * 2018-06-08 2018-09-25 哈尔滨工业大学 不含稀土低合金超高强韧镁合金及其制备方法
CN111607728A (zh) * 2020-05-21 2020-09-01 东北大学 一种轻稀土元素Ce和Sm强化的低成本变形镁合金及其制备方法
EP3733889A4 (de) * 2017-12-26 2021-03-03 Posco Blech aus magnesiumlegierung und verfahren zur herstellung davon

Family Cites Families (9)

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Publication number Priority date Publication date Assignee Title
US3146096A (en) * 1962-11-23 1964-08-25 Dow Chemical Co Weldable high strength magnesium base alloy
JP2002173730A (ja) * 2000-12-01 2002-06-21 Sumitomo Light Metal Ind Ltd 展伸用マグネシウム合金
AU2007202131A1 (en) * 2007-05-14 2008-12-04 Joka Buha Method of heat treating magnesium alloys
JP2009120883A (ja) * 2007-11-13 2009-06-04 Mitsubishi Alum Co Ltd マグネシウム合金箔およびその製造方法
CN101629260A (zh) * 2008-07-18 2010-01-20 中国科学院金属研究所 医用可吸收Mg-Zn-Mn-Ca镁合金
JP5720926B2 (ja) * 2010-10-12 2015-05-20 住友電気工業株式会社 マグネシウム合金の線状体及びボルト、ナット並びにワッシャー
CN109022980A (zh) * 2012-06-26 2018-12-18 百多力股份公司 镁合金、其生产方法及其用途
US9593397B2 (en) * 2013-03-14 2017-03-14 DePuy Synthes Products, Inc. Magnesium alloy with adjustable degradation rate
WO2018117695A1 (ko) * 2016-12-22 2018-06-28 주식회사 포스코 마그네슘 합금 판재 및 이의 제조방법

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3733889A4 (de) * 2017-12-26 2021-03-03 Posco Blech aus magnesiumlegierung und verfahren zur herstellung davon
US11773472B2 (en) 2017-12-26 2023-10-03 Posco Co., Ltd Magnesium alloy sheet and method for producing same
CN108570583A (zh) * 2018-06-08 2018-09-25 哈尔滨工业大学 不含稀土低合金超高强韧镁合金及其制备方法
CN111607728A (zh) * 2020-05-21 2020-09-01 东北大学 一种轻稀土元素Ce和Sm强化的低成本变形镁合金及其制备方法

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US20200239992A1 (en) 2020-07-30
JP2018141234A (ja) 2018-09-13
JP7116394B2 (ja) 2022-08-10
EP3572542A4 (de) 2020-10-28
EP3572542B1 (de) 2023-10-11

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