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WO2018117632A1 - Alliage de magnésium présentant une excellente résistance à la corrosion et son procédé de fabrication - Google Patents

Alliage de magnésium présentant une excellente résistance à la corrosion et son procédé de fabrication Download PDF

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Publication number
WO2018117632A1
WO2018117632A1 PCT/KR2017/015112 KR2017015112W WO2018117632A1 WO 2018117632 A1 WO2018117632 A1 WO 2018117632A1 KR 2017015112 W KR2017015112 W KR 2017015112W WO 2018117632 A1 WO2018117632 A1 WO 2018117632A1
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WIPO (PCT)
Prior art keywords
corrosion resistance
magnesium alloy
secondary phase
phase
rolling
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/KR2017/015112
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English (en)
Korean (ko)
Inventor
추동균
박재신
박우진
김혜정
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.)
Research Institute of Industrial Science and Technology RIST
Posco Holdings Inc
Original Assignee
Posco Co Ltd
Research Institute of Industrial Science and Technology RIST
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Application filed by Posco Co Ltd, Research Institute of Industrial Science and Technology RIST filed Critical Posco Co Ltd
Priority to KR1020197025396A priority Critical patent/KR102306290B1/ko
Publication of WO2018117632A1 publication Critical patent/WO2018117632A1/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
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
    • 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

Definitions

  • the present invention relates to a magnesium alloy excellent in corrosion resistance and a method of manufacturing the same.
  • Magnesium alloy is the lightest among the structural metal materials, and excellent strength, non-stiffness, vibration absorption ability, etc. is becoming more important as a lightweight material for transportation equipment as well as electronics and IT industry.
  • Pure magnesium is a very active metal electrochemically with a standard hydrogen electrode potential of -2.38V, which quickly corrodes when exposed to corrosive environments.
  • the MgO coating formed on the surface shows a level of corrosion resistance comparable to that of medium-carbon steels or ordinary aluminum alloys, whereas in the presence of water or in acidic or neutral solutions, the surface coating becomes unstable and does not form a passivation, resulting in rapid corrosion. Proceed. That is, magnesium is an electrochemically active metal, and when exposed to a corrosive environment, there is a disadvantage that corrosion proceeds at a rapid rate, and thus there is a limit to the application of material.
  • Patent Document 1 Korean Unexamined Patent Publication No. 10-2003-0096890
  • One aspect of the present invention is to provide a magnesium alloy excellent in corrosion resistance and a method of manufacturing the same.
  • One aspect of the present invention is by weight, Al: 1.0-10.0%, Zn: 0.3-3.0%, Mn: 0.05-1.5%, Ti: 0.003-1.0%, Y: 0.03-1.0%, the remaining Mg and other unavoidable It includes impurities, and the microstructure relates to a magnesium alloy having excellent corrosion resistance including 0.8 to 7.0 area% of Al-Mn-Y secondary phase and Al-Y secondary phase in total.
  • another aspect of the present invention is by weight, Al: 1.0-10.0%, Zn: 0.3-3.0%, Mn: 0.05-1.5%, Ti: 0.003-1.0%, Y: 0.03-1.0%, the remaining Mg And preparing a molten metal including other unavoidable impurities; Casting the molten metal to obtain a casting material; Homogenizing the cast material for 12 to 24 hours in a temperature range of 380 to 420 ° C .; And a step of obtaining the magnesium alloy by rolling the homogenized cast material at a temperature in a range of 200 to 350 ° C ..
  • the present invention by adding Ti and Y in combination, it is possible to provide a magnesium alloy excellent in corrosion resistance and excellent mechanical properties such as yield strength and elongation, and a method of manufacturing the same.
  • FIG. 3 is a result of measuring the element and phase distribution in atomic units by 3D-APT analysis using the radiation accelerator of Inventive Example 1.
  • the present inventors have recognized that there is a problem that corrosion proceeds rapidly when magnesium is an electrochemically active metal and exposed to a corrosive environment.
  • an Al-Mn-Y secondary phase and an Al-Y secondary phase are formed by complex addition of Ti and Y, and the formation of the Al 8 Mn 5 phase and the ⁇ phase (Mg 17 Al 12 ) is suppressed, thereby preventing the formation of the secondary phase.
  • the difference in the electrochemical potential with the ⁇ -Mg matrix can be minimized, thus confirming that the corrosion resistance is significantly improved, and thus, the present invention has been completed.
  • Magnesium alloy excellent in corrosion resistance according to an aspect of the present invention in weight% Al: 1.0 ⁇ 10.0%, Zn: 0.3 ⁇ 3.0%, Mn: 0.05 ⁇ 1.5%, Ti: 0.003 ⁇ 1.0%, Y: 0.03 ⁇ 1.0 %, Remaining Mg and other unavoidable impurities.
  • the unit of each element content hereafter means weight% unless there is particular notice.
  • Al is an element that increases the strength and hardness when added, improves the flowability of the molten alloy, and improves castability by increasing the solidification range during casting. It also serves to lower the corrosion rate.
  • Al content is less than 1.0%, the above effects are insufficient.
  • the Al content is more than 10.0%, coarse? Phase (Mg 17 Al 12 ) is excessively formed to increase brittleness, thereby reducing workability and ductility, and at the same time, forming a fine galvanic circuit with Mg base to form corrosion resistance.
  • Al is excessively added, it reacts with Mg to form coarse? Phase (Mg 17 Al 12 ), which also lowers high temperature creep characteristics. Therefore, it is preferable that Al content is 1.0-10.0%.
  • the lower limit of Al content may be 1.5%, and the lower limit may be 2.0%.
  • the more preferable upper limit of Al content may be 9.5%, and a more preferable upper limit may be 9.0%.
  • Zn is added together with Al to refine the grains and increase the strength.
  • Zn content is less than 0.3%, the above-described effects are insufficient. If the Zn content is more than 3.0%, the possibility of hot cracking during casting may increase, resulting in inferior corrosion resistance and mechanical properties of the alloy. Therefore, it is preferable that Zn content is 0.3 to 3.0%.
  • the lower limit of the Zn content may be 0.5%, and the lower limit may be 0.8%.
  • the more preferred upper limit of the Zn content may be 2.5%, and the more preferable upper limit may be 1.5%.
  • Mn improves corrosion resistance in Mg-Al and Mg-Al-Zn based alloys.
  • the corrosion resistance is improved by forming an intermetallic compound which is harmless to corrosion resistance by combining with Fe or other heavy metal elements which adversely affect the corrosion resistance.
  • Mn content is more than 1.5%, the solubility in the Mg alloy is exceeded, and mechanical properties may be degraded by formation of coarse ⁇ -Mn phase and Al 8 Mn 5 phase. Therefore, it is preferable that Mn content is 0.05 to 1.5%.
  • the lower limit of the Mn content may be 0.08%, and the lower limit may be 0.15%.
  • the more preferable upper limit of Mn content may be 1.0%, and a more preferable upper limit may be 0.3%.
  • Ti is dissolved in the ⁇ -Mg matrix and serves to improve corrosion resistance by increasing the electrochemical potential of the matrix to reduce the potential difference with the secondary phase.
  • Ti has a very large growth inhibitory factor, and contributes to the miniaturization of the cast structure and contributes to miniaturization of the final particle size and miniaturization of the ⁇ phase to inhibit corrosion.
  • it increases the Al solid solution content in the ⁇ -Mg matrix to improve the corrosion resistance.
  • the Ti content is less than 0.003%, the above effects are insufficient. Therefore, it is preferable to add 0.003% or more, and more preferably 0.07% or more, even more preferably 0.1% or more for the purpose of improving the corrosion resistance.
  • the Ti content is increased, it is effective to improve corrosion resistance, but when the Ti content is more than 1.0%, there is a fear that Ti is not dissolved in the ⁇ -Mg base and separated into Ti metal. Therefore, it is preferable to add at 1.0% or less, and more preferably at 0.5% or less.
  • Y suppresses the formation of the Al 8 Mn 5 phase and the ⁇ phase (Mg 17 Al 12 ) by forming an Al-Mn-Y secondary phase and an Al-Y secondary phase, thereby reducing the difference in electrochemical potential from the ⁇ -Mg matrix. It is an element that plays a role of minimizing and improving corrosion resistance. Further, by forming the Y 2 O 3 to improve the corrosion resistance.
  • the Y content is less than 0.03%, the above effects are insufficient.
  • the Y content is more than 1.0% (Al, Mg) 2 Y intermetallic compound is formed coarse, there is a problem that the mechanical properties such as ductility deteriorate and the manufacturing cost increases.
  • the remaining component of the present invention is magnesium (Mg).
  • Mg magnesium
  • impurities which are not intended from the raw material or the surrounding environment may be inevitably mixed, and thus cannot be excluded. Since these impurities are known to those skilled in the art, all of them are not specifically mentioned in the present specification.
  • one or more of B, Zr, Be, Sn, Sr, and Ca may be added in an amount of 0.003 to 2.0 wt% in total.
  • the total is less than 0.003%, the effect of improving corrosion resistance is insufficient. If the total amount is less than 2.0%, a large amount of the intermetallic compound is formed, which may lower the mechanical properties and the manufacturing cost increases.
  • the microstructure of the magnesium alloy according to the present invention includes an Al-Mn-Y secondary phase and an Al-Y secondary phase in a total of 0.8 to 7.0 area%.
  • the formation of the Al 8 Mn 5 phase and the ⁇ phase (Mg 17 Al 12 ) is suppressed, and the difference in the electrochemical potential from the ⁇ -Mg matrix is minimized.
  • These secondary phases are mainly formed during casting, but are controlled at a constant size and area ratio by heat treatment, rolling, cooling rate control, and the like after casting. That is, the secondary phase present in the casting material may be properly controlled in size and area ratio by rolling and heat treatment.
  • the sum is less than 0.8 area%, the above-mentioned effects are insufficient. If the total amount is more than 7.0 area%, the mechanical properties may be lowered, and the manufacturing cost increases.
  • the lower limit of the sum of the area fractions of the Al-Mn-Y secondary phase and the Al-Y secondary phase may be 1.0 area%, and even more preferably, the lower limit may be 2.0 area%.
  • the more preferable upper limit of the sum of the area fractions of the Al-Mn-Y secondary phase and the Al-Y secondary phase may be 6.8 area%, and the even more preferable upper limit may be 6.5 area%.
  • the Al-Mn-Y secondary phase may be Al 8 Mn 4 Y
  • Al-Y secondary phase may be Al 3 Y.
  • AZ-based magnesium alloys contain various secondary phases at the ⁇ -Mg matrix.
  • Representative secondary phases include Al 8 Mn 5 phase and ⁇ phase (Mg 17 Al 12 ).
  • the electrochemical potential of the representative secondary phase was determined by thermodynamic calculation.
  • the electrochemical potentials of the Al-Mn-Y secondary phase and the Al-Y secondary phase are about ⁇ 1.7 V and about ⁇ 1.8 V, respectively, which are lower than those of the Al 8 Mn 5 phase.
  • Figure 1 (a) is a Volta potential of Al 8 Mn 5 phase in Comparative Example 1 (AZ31), (b) is a result of measuring the volta potential of Al 8 Mn 4 Y secondary phase formed in Comparative Example 3 (AZ31-Y) to be.
  • Volta potential is a value measured by the SKPFM (Scanning Kelvin Probe Force Microscopy) between the secondary phase and the ⁇ -Mg base, which is not exactly equivalent to the electrochemical potential difference shown in the thermodynamic data. Shows a trend proportional to value.
  • the volta potential of the Al-Mn-Y secondary phase of the present invention may be 300 mV or less.
  • the magnesium alloy of the present invention has a tensile strength of 180 MPa or more, an elongation of 15% or more, and an LDH of 2.0 to 3.5 mm.
  • the magnesium alloy of the present invention has a corrosion rate of 0.7 mm / year or less. More preferably, it is 0.5 mm / year or less.
  • Another aspect of the present invention provides a method for producing a magnesium alloy excellent in corrosion resistance comprising the steps of preparing a melt that satisfies the alloy composition of the present invention; Casting the molten metal to obtain a casting material; Homogenizing the cast material for 12 to 24 hours in a temperature range of 380 to 420 ° C .; And rolling the homogenized cast material at a temperature range of 275 to 325 ° C. to obtain a magnesium alloy.
  • a molten metal that satisfies the alloy composition of the present invention described above is prepared. It does not need to specifically limit, According to the general preparation of the molten metal for magnesium alloys.
  • pure magnesium is charged into a low carbon steel crucible and dissolved by heating to 720 ° C. under a protective gas atmosphere.
  • alloy elements are added in order of Al-B, Al-Ti, Al-Mn, Al, Mg-Y, and Zn in order from high melting point alloy element to dissolve the alloy elements evenly in the molten metal. It can stir for about a minute and can hold about 10 minutes so that an inclusion may fully settle.
  • the molten metal is cast to obtain a casting material.
  • the casting step need not be particularly limited as in the molten metal preparation step. For example, it may be cast using gravity casting, pressure casting, continuous casting, twin roll type sheet casting machine. In addition, the step of extruding the cast material to produce an extruded material may be further performed.
  • the cast material is homogenized for 12 to 24 hours in the temperature range of 380 ⁇ 420 °C. This is to homogenize the composition and texture segregation and non-uniformity present in the Mg alloy matrix structure during casting. Secondary phases such as ⁇ phase (Mg 17 Al 12 ) dispersed in the base can be sufficiently employed in the base, and appropriately control the heat treatment temperature and time within a range that does not cause economic deterioration due to excessive increase of the heat treatment temperature and time. shall.
  • the homogenization temperature is less than 380 ° C. or the holding time is less than 12 hours, sufficient homogenization is not achieved, and segregation and non-uniformity of the composition and the tissue remain, which may adversely affect the corrosion resistance.
  • the homogenization temperature is more than 420 °C or the holding time is more than 24 hours, the corrosion resistance is rather deteriorated due to abnormal growth of the tissue, there is a fear that the economic efficiency is lowered.
  • the homogenized cast material is rolled in a temperature range of 200 ⁇ 350 °C to obtain a magnesium alloy. Since the Mg alloy has an HCP structure, it must be warm rolled at 200 ° C. or higher, and a rolling crack may occur when the rolling temperature is lower than 200 ° C. On the other hand, if the rolling temperature is greater than 350 °C there is a risk that hot tearing (rolling) occurs during rolling. Therefore, it is preferable that rolling temperature is 200-350 degreeC.
  • the more preferable minimum of rolling temperature may be 250 degreeC, and a more preferable upper limit may be 325 degreeC.
  • the rolling can be performed so that the reduction ratio per pass is 10 to 20%.
  • the manufacturing cost is increased because a number of passes must be rolled to a desired thickness, and if it exceeds 20%, there may be a rolling crack due to excessive reduction ratio.
  • the corrosion rate of the magnesium alloy was measured and listed in Table 1 below.
  • Corrosion rate was used by the Salt Immersion Test, in which the specimen was immersed in brine, and the brine used was a 3.5% NaCl solution at 25 ° C and the specimen was immersed in brine for 75 hours to lose weight in mg / cm 2. It was measured in units of / day, and this was divided by the sample area and expressed in terms of the annual corrosion rate in mm / y.
  • the total fractions of the Al-Mn-Y secondary phase and the Al-Y secondary phase were measured in area% using an image analyzer after measuring the microstructure with a scanning electron microscope, and the results are shown in Table 1.
  • Formability Limit Dome Height is one of the test methods for measuring the formability of the material, by measuring the limit dome height (Limit Dome Height) is formed without breaking the material measured by the Ericsson test (Table 2) It is described in.
  • Comparative Example 3 in which only Y was added, also exhibited a corrosion rate of 0.86 mm / y, indicating poor corrosion resistance.
  • 3 is a result of 3D-APT analysis using an emission accelerator for Inventive Example 1, and is a result of measuring elemental and phase distribution in atomic units for the internal microstructure.
  • the unit of the Z axis is nm.
  • Ti is finely and uniformly dissolved in the ⁇ -Mg matrix, and it is possible to identify the Al-Mn-Y secondary phase finely formed in several tens of nm in size.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Continuous Casting (AREA)
  • Prevention Of Electric Corrosion (AREA)

Abstract

Un mode de réalisation de la présente invention concerne un alliage de magnésium présentant une excellente résistance à la corrosion, comprenant : de 1,0 à 10,0 % en poids d'Al ; de 0,3 à 3,0 % en poids de Zn ; de 0,05 à 1,5 % en poids de Mn ; de 0,003 à 1,0 % en poids de Ti ; de 0,03 à 1,0 % en poids d'Y ; et un complément constitué de Mg et d'autres impuretés inévitables, la microstructure comprenant de 0,8 à 7,0 % de surface, en tant que somme d'une phase secondaire d'Al-Mn-Y et d'une phase secondaire d'Al-Y.
PCT/KR2017/015112 2016-12-23 2017-12-20 Alliage de magnésium présentant une excellente résistance à la corrosion et son procédé de fabrication Ceased WO2018117632A1 (fr)

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KR1020197025396A KR102306290B1 (ko) 2016-12-23 2017-12-20 내식성이 우수한 마그네슘 합금 및 그 제조방법

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112424385A (zh) * 2018-07-18 2021-02-26 株式会社Posco 镁合金板材及其制造方法
CN113025858A (zh) * 2021-03-05 2021-06-25 吉林大学 具有细化基体相和共晶相Mg-Al-Zn系镁合金及其制备方法和应用
CN116926391A (zh) * 2023-07-25 2023-10-24 上海交通大学 一种高亮高耐蚀镁合金及其制备方法
WO2024208130A1 (fr) * 2023-04-06 2024-10-10 上海交通大学 Alliage de magnésium super résistant à la corrosion et son procédé de préparation

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* Cited by examiner, † Cited by third party
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JPH07316713A (ja) * 1994-05-25 1995-12-05 Kobe Steel Ltd 高強度高耐食性Ｍｇ基合金及び該合金よりなる鋳物の製法
KR20030044997A (ko) * 2003-05-23 2003-06-09 연우인더스트리(주) 성형성이 우수한 마그네슘합금 및 이를 이용한마그네슘합금 제품의 제조방법
JP2006144059A (ja) * 2004-11-18 2006-06-08 Mitsubishi Alum Co Ltd プレス成形性に優れたマグネシウム合金板およびその製造方法
KR20100106137A (ko) * 2009-03-23 2010-10-01 주식회사 지알로이테크놀로지 저온에서 고속 성형능이 우수한 가공재 마그네슘-아연계 마그네슘 합금과 그 합금 판재의 제조방법
KR20150017143A (ko) * 2013-08-06 2015-02-16 이인영 소성가공성이 우수한 압출용 마그네슘합금 빌렛 및 그 제조방법

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KR100452452B1 (ko) 2002-06-18 2004-10-12 현대자동차주식회사 내식성이 향상된 고강도 마그네슘 합금 및 이의 제조방법
KR100605741B1 (ko) * 2004-04-06 2006-08-01 김강형 내식성과 도금성이 우수한 마그네슘합금 단련재

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Publication number Priority date Publication date Assignee Title
JPH07316713A (ja) * 1994-05-25 1995-12-05 Kobe Steel Ltd 高強度高耐食性Ｍｇ基合金及び該合金よりなる鋳物の製法
KR20030044997A (ko) * 2003-05-23 2003-06-09 연우인더스트리(주) 성형성이 우수한 마그네슘합금 및 이를 이용한마그네슘합금 제품의 제조방법
JP2006144059A (ja) * 2004-11-18 2006-06-08 Mitsubishi Alum Co Ltd プレス成形性に優れたマグネシウム合金板およびその製造方法
KR20100106137A (ko) * 2009-03-23 2010-10-01 주식회사 지알로이테크놀로지 저온에서 고속 성형능이 우수한 가공재 마그네슘-아연계 마그네슘 합금과 그 합금 판재의 제조방법
KR20150017143A (ko) * 2013-08-06 2015-02-16 이인영 소성가공성이 우수한 압출용 마그네슘합금 빌렛 및 그 제조방법

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112424385A (zh) * 2018-07-18 2021-02-26 株式会社Posco 镁合金板材及其制造方法
EP3825429A4 (fr) * 2018-07-18 2021-10-27 Posco Tôle d'alliage de magnésium et son procédé de fabrication
JP2021529888A (ja) * 2018-07-18 2021-11-04 ポスコＰｏｓｃｏ マグネシウム合金板材およびその製造方法
CN112424385B (zh) * 2018-07-18 2022-07-26 株式会社Posco 镁合金板材及其制造方法
JP7138229B2 (ja) 2018-07-18 2022-09-15 ポスコ マグネシウム合金板材およびその製造方法
US11542577B2 (en) 2018-07-18 2023-01-03 Posco Holdings Inc. Magnesium alloy sheet and manufacturing method thereof
CN113025858A (zh) * 2021-03-05 2021-06-25 吉林大学 具有细化基体相和共晶相Mg-Al-Zn系镁合金及其制备方法和应用
CN113025858B (zh) * 2021-03-05 2022-03-04 吉林大学 具有细化基体相和共晶相Mg-Al-Zn系镁合金及其制备方法和应用
WO2024208130A1 (fr) * 2023-04-06 2024-10-10 上海交通大学 Alliage de magnésium super résistant à la corrosion et son procédé de préparation
CN116926391A (zh) * 2023-07-25 2023-10-24 上海交通大学 一种高亮高耐蚀镁合金及其制备方法

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KR20190120227A (ko) 2019-10-23

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