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WO2016117768A1 - Procédé de fabrication de billette d'alliage de magnésium pour traitement plastique et procédé de fabrication d'alliage de magnésium corroyé à haute résistance comprenant celui-ci - Google Patents

Procédé de fabrication de billette d'alliage de magnésium pour traitement plastique et procédé de fabrication d'alliage de magnésium corroyé à haute résistance comprenant celui-ci Download PDF

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Publication number
WO2016117768A1
WO2016117768A1 PCT/KR2015/005017 KR2015005017W WO2016117768A1 WO 2016117768 A1 WO2016117768 A1 WO 2016117768A1 KR 2015005017 W KR2015005017 W KR 2015005017W WO 2016117768 A1 WO2016117768 A1 WO 2016117768A1
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WO
WIPO (PCT)
Prior art keywords
magnesium alloy
alloy billet
billet
manufacturing
magnesium
Prior art date
Legal status (The legal status 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 status listed.)
Ceased
Application number
PCT/KR2015/005017
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English (en)
Korean (ko)
Inventor
박성혁
정재길
김하식
유봉선
임창동
문병기
김영민
배준호
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Korea Institute of Machinery and Materials KIMM
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Korea Institute of Machinery and Materials KIMM
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Filing date
Publication date
Application filed by Korea Institute of Machinery and Materials KIMM filed Critical Korea Institute of Machinery and Materials KIMM
Publication of WO2016117768A1 publication Critical patent/WO2016117768A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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
    • 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 method of manufacturing a magnesium alloy billet for plastic working and a method of manufacturing a high strength magnesium alloy processed material including the same.
  • Magnesium alloys have attracted attention as a very attractive material in the automotive, railroad and aviation industries because of their extremely low density compared to other metal materials, as well as their excellent strength, dimensional stability, electromagnetic shielding and heat dissipation.
  • Magnesium alloys made of such magnesium alloys are largely divided into cast Mg alloys and magnesium alloy processed materials (wrought Mg alloys).
  • the cast material is excellent in formability, but its surface is very coarse, so that after casting It requires a lot of time and cost in the post-treatment process for the surface, there are a lot of internal defects such as shrinkage pores, there is a problem that it is not suitable for manufacturing high-quality magnesium alloy products that require high strength.
  • Non-Patent Documents 0001 to 0003 have been commercialized and widely used.
  • magnesium alloy workpieces are still limited in applications and components due to their low strength compared to commercially available aluminum alloys or steels. This is an urgent situation.
  • the present invention relates to a magnesium alloy processed material having a higher strength than conventional magnesium alloyed materials including commercial magnesium alloyed materials by increasing the fraction of secondary phases produced after hot working and decreasing the average grain size of grains. Its purpose is to provide.
  • the present invention to achieve the technical problem as described above, (a) preparing a magnesium alloy billet; (b) homogenizing heat treatment of the magnesium alloy billet; And (c) aging the homogenized heat treated magnesium alloy billet.
  • step (a) is characterized in that it comprises the following steps:
  • step (b) is characterized in that the homogenization heat treatment for 0.5 to 96 hours at 350 to 550 °C.
  • the magnesium alloy billet in the step (b) is characterized in that the pre-heating (pre-heating) at a temperature of 250 to 350 °C homogenization heat treatment.
  • step (b) is characterized in that it further comprises the step of cooling after homogenizing heat treatment of the magnesium alloy billet.
  • the present invention provides a method for producing a magnesium alloy workpiece further comprising the step of hot or warm processing the magnesium alloy billet aged in step (c).
  • the hot or warm processing is characterized in that it is carried out using at least one method selected from rolling, extrusion or forging.
  • the aged magnesium alloy billet characterized in that it further comprises the step of aging treatment.
  • the aging treatment after the hot or warm processing is characterized in that it is carried out at 150 to 250 °C for 1 to 360 hours.
  • the present invention also provides a magnesium alloy processing material produced by the method described above.
  • the manufacturing method of the magnesium alloy billet for plastic working before performing the plastic working of the prepared magnesium alloy billet, by performing an aging treatment (aging treatment performed after the homogenization heat treatment), a fine secondary phase (secondary phase) phase) It is possible to prepare a magnesium alloy billet in which the precipitate is formed in a large amount in the magnesium alloy grain boundary and the matrix.
  • the crystal grain boundary of the dynamic recrystallized grains formed during the plastic working of the precipitate formed in the magnesium alloy billet by hot or warm processing the magnesium alloy billet prepared by the above method By interfering through the grain boundary pinning effect, it is possible to produce a high-strength magnesium alloy workpiece by improving the strength due to grain refinement and improving the strength by precipitation hardening.
  • 1 is a flow chart showing each step of the method for producing a magnesium alloy billet for plastic working according to the present invention.
  • Figure 2 is an electron microscope (SEM or TEM) photograph showing the difference of the magnesium alloy microstructure with or without aging treatment in the present Example 1 homogenization treatment.
  • SEM scanning electron microscope
  • 4 (a) and 4 (b) are scanning electron microscope (SEM) and electron backscattering diffraction (EBSD) photographs showing the microstructure of the magnesium alloy workpiece prepared in Comparative Example 1 and Example 1, respectively.
  • SEM scanning electron microscope
  • EBSD electron backscattering diffraction
  • Example 5 is a stress-strain graph according to a room temperature tensile test (crosshead speed: 1.5 mm / min) for the magnesium alloy workpiece prepared in Example 1 and Comparative Example 1 of the present application.
  • Embodiments according to the concept of the present invention can be variously modified and can have various forms, and specific embodiments will be illustrated in the drawings and described in detail in the present specification or application. However, this is not intended to limit the embodiments in accordance with the concept of the present invention to a particular disclosed form, it should be understood to include all changes, equivalents, and substitutes included in the spirit and scope of the present invention.
  • 1 is a flow chart showing each step of the method for producing a magnesium alloy billet for plastic working according to the present invention.
  • a method of manufacturing a magnesium alloy billet for plastic working according to the present invention includes (a) preparing a magnesium alloy billet, (b) homogenizing heat treatment of the magnesium alloy billet, and (( c) aging the homogenized heat treated magnesium alloy billet.
  • a raw material including magnesium may be melted to prepare a molten magnesium alloy, and then injected into a mold to prepare a magnesium alloy billet.
  • step (a) comprises the steps of preparing a molten metal containing magnesium and alloying elements; And injecting the molten metal into a mold to form a billet, thereby preparing a magnesium alloy billet.
  • the temperature for carrying out the casting process is not particularly limited, but may be preferably cast at a temperature of 650 to 750 °C, because when casting below 650 °C the flow rate of the molten magnesium alloy may be lowered Smooth casting may not be achieved, and when casting at a temperature exceeding 750 ° C., the molten magnesium alloy may be rapidly oxidized and impurities may be mixed during casting, resulting in lower purity of the manufactured magnesium alloy billet. Because it can.
  • the molten magnesium alloy may be prepared by melting a raw material of the magnesium alloy.
  • the method of manufacturing the magnesium alloy molten metal is not limited thereto, and the method may be gravity casting, continuous casting, sand casting, or the like. Typical examples include casting methods such as pressure casting.
  • the step (b) is a step of homogenizing the magnesium alloy billet prepared in the step (a), by performing a homogenization heat treatment to form a heterogeneous structure due to segregation of alloy elements generated in the casting of magnesium alloy molten metal And high temperature processability and mechanical properties of the magnesium alloy can be improved.
  • the homogenization heat treatment made in this step is preferably performed at 350 to 550 ° C., which is when the homogenization heat treatment is performed at less than 350 ° C., the content of the alloying element dissolved in the magnesium matrix is small, so that the dynamic precipitation during hot or warm processing will be described later.
  • the strengthening effect of the alloy due to dynamic precipitation is not great, and when the homogenization heat treatment is performed at a temperature exceeding 550 ° C., the homogenization heat treatment temperature of the magnesium alloy is high and local dissolution of the magnesium alloy billet may occur, resulting in deterioration of physical properties. Because there is a problem that can be.
  • the homogenization heat treatment is preferably carried out for 0.5 to 96 hours, when the homogenization heat treatment is carried out in less than 0.5 hours, the diffusion of the alloying elements do not occur sufficiently, the effect of the homogenization heat treatment does not appear, more than 96 hours This is because the effect is not economical because the increase of the effect against the execution time is not large.
  • the magnesium alloy billet is preferably pre-heated at 250 to 350 ° C. prior to the homogenization heat treatment so as to prevent cracking and deformation due to rapid heat treatment of the magnesium alloy billet.
  • the homogenizing heat treatment of the magnesium alloy billet preferably configured to further comprise the step of cooling
  • the specific method for performing this cooling process is not particularly limited, magnesium made of supersaturated solid soluiont Water quenching is more preferable than air cooling in that an alloy billet can be obtained to further increase the dynamic precipitation of the secondary phase during hot or warm processing, which will be described later.
  • step (c) is a step of aging the magnesium alloy billet is homogenized heat treatment in the step (b).
  • the aging treatment of the magnesium alloy billet is preferably carried out at a temperature of 100 to 500 °C, which is inefficient when the aging treatment at a temperature of less than 100 °C slow heat-treatment is required for a long time heat treatment, 500 °C This is because when the aging treatment is carried out at the above temperature, the size of the precipitate formed is large and it is difficult to obtain the expected effect.
  • the aging treatment of the magnesium alloy billet is more preferably carried out at a temperature of 150 to 300 °C.
  • the aging treatment is preferably carried out by heat treatment for 1 to 300 hours, when the aging treatment is less than 1 hour, the amount of precipitates formed is not large, the effect of the aging treatment is less than expected, exceeding 300 hours In this case, the effect of aging treatment is no longer enhanced, so there is a problem that further heat treatment is inefficient.
  • the aging treatment of the magnesium alloy billet is more preferably heat treated for 6 to 300 hours.
  • the fine secondary phase precipitates in a large amount in the magnesium alloy grain boundary and matrix
  • the formed magnesium alloy billet can be produced.
  • the present invention provides a method for producing a magnesium alloy workpiece further comprising the step of hot or warm processing the magnesium alloy billet aged in step (c).
  • the method for producing a magnesium alloy workpiece according to the present invention is subjected to hot or warm working of the aged magnesium alloy billet as described above using at least one known plastic working method selected from rolling, extrusion or forging.
  • the plastic working method of the magnesium alloy billet is not limited by rolling, extrusion or forging, and is not limited thereto as long as it is a method commonly used in the art.
  • the aging treatment is 150 It may be carried out through a process of heat treatment for 1 to 360 hours at a temperature of to 250 °C.
  • the precipitate is formed during plastic working
  • the grain growth of the dynamic recrystallized grain By inhibiting the grain growth of the dynamic recrystallized grain through the grain boundary pinning effect, it is possible to produce a high-strength magnesium alloy workpiece through the improvement of strength due to grain refinement and the strength by precipitation hardening.
  • the magnesium alloy billet was homogenized heat treated at 400 ° C. for 15 hours, water quenched, and then processed into cylindrical specimens (diameter: 80 mm, height 200 mm) along the casting direction.
  • the specimens were aged at 200 ° C. for 64 hours and cooled with water.
  • FIG. 2 is an electron micrograph showing the difference between the magnesium alloy microstructure with or without aging treatment after the homogenization treatment, in the microstructure of the specimen before the aging treatment from Figure 2 by the homogenization heat treatment secondary phase (Mg 17 Al 12 ) are all dissolved in the magnesium matrix so that no secondary phase particles are observed (see FIG. 2 (a)), whereas in the microstructure of the aged specimen after homogenization heat treatment, a large number of Mg 17 Al 12 particles are found in the grain boundary as well as the grain boundary (See FIG. 2 (b)), it can be seen that plate-like Mg 17 Al 12 precipitates in the grains have a specific orientation with respect to the magnesium matrix (see FIG. 2 (c)). .
  • the pre-heated specimen was preheated to 250 ° C. and then extruded (ram speed: 1 mm / sec, extrusion ratio: 25) at 250 ° C. and air cooled to prepare a magnesium alloy workpiece.
  • a cast billet made of a magnesium alloy (TAZ711) having the composition shown in Table 2 below was prepared. Specifically, magnesium alloy molten metal obtained by dissolving a raw metal such as magnesium under an inert atmosphere containing carbon dioxide (CO 2 ) and sulfur hexafluoride (SF 6 ) and a temperature of 800 ° C. is poured into a steel mold preheated to 210 ° C. Alloy billets were prepared.
  • a raw metal such as magnesium under an inert atmosphere containing carbon dioxide (CO 2 ) and sulfur hexafluoride (SF 6 ) and a temperature of 800 ° C.
  • the magnesium alloy billet was homogenized heat treated at 500 ° C. for 12 hours, water quenched, and then processed into cylindrical specimens (diameter: 80 mm, height 200 mm) along the casting direction.
  • the specimen was subjected to aging treatment under different conditions (Example 2-1: 200 ° C., 64 hours; Example 2-2: 200 ° C., 128 hours; Example 2-3: 400 ° C., 4 hours) and water cooled. It was.
  • FIG. 3 is a scanning electron microscope (SEM) photograph showing the difference of magnesium alloy microstructures according to the conditions of aging treatment after homogenization treatment, and the fine grains of Mg 2 Sn precipitates were formed by performing aging treatment before hot working from FIG. 3. It is formed in a large amount and the base, it can be seen that the particle size of the precipitate increases as the heat treatment temperature or time increases.
  • a magnesium alloy workpiece was prepared in the same manner as in Example 1 except that the extrusion process was performed immediately after the homogenization heat treatment without aging treatment.
  • a magnesium alloy workpiece was manufactured in the same manner as in Example 2-1, except that the aging treatment was not performed before the extrusion process.
  • 4 (a) and 4 (b) are scanning electron microscope (SEM) and electron backscattering diffraction (EBSD) photographs showing the microstructure of the magnesium alloy workpiece prepared in Comparative Example 1 and Example 1, respectively.
  • SEM scanning electron microscope
  • EBSD electron backscattering diffraction
  • the magnesium alloy workpiece of Example 1 was 57% more than the magnesium alloy workpiece of Comparative Example 1 having a fraction of 49% fine DRX region, thus leading to plastic working.
  • the aging treatment resulted in the reduction of the average grain size from 9.9 ⁇ m to 8.4 ⁇ m.
  • the magnesium alloy workpiece of Example 1 has a band-shaped Mg 17 which adversely affects mechanical properties compared to the magnesium alloy workpiece of Comparative Example 1 It was confirmed that the fraction of Al 12 particles decreased from 2.3% to 0.5%. This result led to the improvement of the strength of the magnesium alloy workpiece as shown below.
  • Example 1 of the present application when the aging treatment is performed before the plastic working, it can be seen that the elongation is also increased.
  • Table 4 shows the results of room temperature tensile test (1.5 mm / min) of magnesium alloy workpieces prepared in Examples 2-1 to 2-3 and Comparative Example 2 of the present application.
  • the magnesium alloy workpiece prepared in Examples 2-1 to 2-3 in the present application was aged before the plastic working was performed, compared with the magnesium alloy workpiece of Comparative Example 2 that did not undergo preaging treatment. It can be seen that it has improved strength through grain refinement and precipitation hardening effect through grain boundary pinning effect of the secondary phase (Mg 2 Sn) precipitated particles thus formed.

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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)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Forging (AREA)
  • Extrusion Of Metal (AREA)

Abstract

La présente invention concerne un procédé de fabrication d'une billette d'alliage de magnésium comprenant les étapes de : (a) préparation d'une billette d'alliage de magnésium ; (b) conduite d'un traitement thermique d'homogénéisation sur la billette d'alliage de magnésium ; et (c) vieillissement de la billette d'alliage de magnésium thermiquement traitée, et concerne un procédé de fabrication d'un alliage de magnésium corroyé qui comprend en outre une étape de conduite d'un travail à chaud ou tiède sur la billette d'alliage de magnésium fabriquée par le procédé. Selon la présente invention, en effectuant le vieillissement avant de conduire le traitement plastique, il est possible de fabriquer une billette d'alliage de magnésium dans laquelle une grande quantité de précipités de phase secondaire fins est contenue dans un joint de grain d'alliage de magnésium et la matrice, et en effectuant le travail à chaud ou à froid sur la billette d'alliage de magnésium, les précipités formés dans la billette d'alliage de magnésium obstruent la croissance de grains recristallisés de façon dynamique formés dans le traitement plastique de sorte qu'il soit possible d'induire un effet de durcissement par précipitation et un effet d'augmentation de la résistance en fonction de l'affinage de grain, de manière à fabriquer un alliage de magnésium corroyé à haute résistance.
PCT/KR2015/005017 2015-01-20 2015-05-19 Procédé de fabrication de billette d'alliage de magnésium pour traitement plastique et procédé de fabrication d'alliage de magnésium corroyé à haute résistance comprenant celui-ci Ceased WO2016117768A1 (fr)

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KR10-2015-0009455 2015-01-20
KR1020150009455A KR101680046B1 (ko) 2015-01-20 2015-01-20 소성 가공 전 시효 처리에 의한 고강도 마그네슘 합금 가공재 제조방법 및 이에 의해 제조된 고강도 마그네슘 합금 가공재

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115874126A (zh) * 2022-12-09 2023-03-31 哈尔滨工业大学（威海） 一种可时效强化镁合金强韧化处理及制备工艺

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107557706B (zh) * 2017-09-04 2019-05-21 河北工业大学 一种提高镁合金强度的处理方法
KR102469771B1 (ko) 2020-04-22 2022-11-23 경북대학교 산학협력단 시효처리 시간의 단축을 위한 공정을 포함하는 고강도 석출 경화형 Mg-Al계 마그네슘 합금 가공재의 제조방법

Citations (5)

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KR19990071071A (ko) * 1998-02-27 1999-09-15 신광선 알루미늄 함유 마그네슘합금의 내식성 향상방법
JP2006176873A (ja) * 2004-11-26 2006-07-06 Aisin Seiki Co Ltd マグネシウム合金及びマグネシウム合金部材の製造方法
KR100994812B1 (ko) * 2010-04-05 2010-11-16 한국기계연구원 고강도 고연성 마그네슘 합금 압출재 및 그 제조방법
KR20120095184A (ko) * 2011-02-18 2012-08-28 한국기계연구원 이방성이 낮은 고강도 고연성 마그네슘 합금 압출재 및 그 제조방법
KR101400140B1 (ko) * 2013-07-16 2014-05-30 한국기계연구원 마그네슘 합금 압출재의 제조방법 및 이에 따라 제조되는 마그네슘 합금 압출재

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR19990071071A (ko) * 1998-02-27 1999-09-15 신광선 알루미늄 함유 마그네슘합금의 내식성 향상방법
JP2006176873A (ja) * 2004-11-26 2006-07-06 Aisin Seiki Co Ltd マグネシウム合金及びマグネシウム合金部材の製造方法
KR100994812B1 (ko) * 2010-04-05 2010-11-16 한국기계연구원 고강도 고연성 마그네슘 합금 압출재 및 그 제조방법
KR20120095184A (ko) * 2011-02-18 2012-08-28 한국기계연구원 이방성이 낮은 고강도 고연성 마그네슘 합금 압출재 및 그 제조방법
KR101400140B1 (ko) * 2013-07-16 2014-05-30 한국기계연구원 마그네슘 합금 압출재의 제조방법 및 이에 따라 제조되는 마그네슘 합금 압출재

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115874126A (zh) * 2022-12-09 2023-03-31 哈尔滨工业大学（威海） 一种可时效强化镁合金强韧化处理及制备工艺

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