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WO2018117713A1 - Alliage de magnésium de résistance élevée présentant une excellente ininflammabilité, et son procédé de production - Google Patents

Alliage de magnésium de résistance élevée présentant une excellente ininflammabilité, et son procédé de production Download PDF

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Publication number
WO2018117713A1
WO2018117713A1 PCT/KR2017/015291 KR2017015291W WO2018117713A1 WO 2018117713 A1 WO2018117713 A1 WO 2018117713A1 KR 2017015291 W KR2017015291 W KR 2017015291W WO 2018117713 A1 WO2018117713 A1 WO 2018117713A1
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WIPO (PCT)
Prior art keywords
magnesium alloy
flame retardancy
intermetallic compound
strength
excellent flame
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/KR2017/015291
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English (en)
Korean (ko)
Inventor
박우진
엄형섭
최대환
김상진
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
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Posco Co Ltd, Research Institute of Industrial Science and Technology RIST filed Critical Posco Co Ltd
Priority to CN201780079314.7A priority Critical patent/CN110114485A/zh
Priority to JP2019533182A priority patent/JP2020509196A/ja
Priority to US16/471,939 priority patent/US20200087757A1/en
Priority to EP17883943.7A priority patent/EP3561097A4/fr
Publication of WO2018117713A1 publication Critical patent/WO2018117713A1/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
    • 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
    • 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
    • C22C1/02—Making non-ferrous alloys by melting
    • C22C1/03—Making non-ferrous alloys by melting using master alloys
    • 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 high strength magnesium alloy excellent in flame retardancy and a method of manufacturing the same.
  • Magnesium is one of the lightest metals in practical metals, so it can be applied as a structural material for portable electronic products such as smartphones, tablet PCs, and laptops, as well as for transportation of automobiles, trains, aircrafts, etc. Is spotlighted as an eco-friendly lightweight metal material.
  • Magnesium alloys are excellent in castability, so cast products manufactured through mold casting methods such as high pressure casting, low pressure casting and gravity casting have been mainly applied to practical products, and recently, they have been manufactured through processing processes such as rolling or extrusion. The development of products for the whole body materials and market expansion are also being promoted.
  • the alloying elements added to the casting magnesium alloy and the magnesium alloy for the whole material are similar, and the most commonly used magnesium alloys are AZ-based alloys containing Al and Zn or AM containing Al and Mn. A system alloy is mentioned.
  • the two kinds of alloys commonly contain Al, in order to improve the castability and tensile strength of magnesium.
  • AZ and AM-based magnesium alloys which occupy most of commercial magnesium alloys, are suitable for manufacturing various mold casting products by improving the flowability of molten metal by Al addition, and also have advantages in billet casting and sheet casting for whole body materials.
  • yield strength or tensile strength is significantly lower than that of competing aluminum alloys, so there is a problem in that the thickness of the product or the product shape should be modified and applied.
  • magnesium alloy has a problem that the use conditions are limited because of the high possibility of ignition due to high oxygen affinity.
  • Patent Document 1 Korean Unexamined Patent Publication No. 10-2015-0077494
  • One aspect of the present invention is to provide a high-strength magnesium alloy excellent in flame retardancy and a method of manufacturing the same.
  • Mg-Al contains at least 6.5% by volume fraction of the intermetallic compound, the average particle diameter of the Mg-Al intermetallic compound relates to a high-strength magnesium alloy excellent in flame retardancy of 20 ⁇ 500nm.
  • another aspect of the present invention is by weight, Al: 2.0-13.0%, Mn: 0.1-0.5%, B: 0.0015-0.025%, Y: 0.1-1.0%, molten metal containing the remaining Mg and unavoidable impurities Preparing a;
  • It relates to a method of producing a high-strength magnesium alloy having excellent flame retardancy comprising; aging treatment of the cooled magnesium alloy for 2 to 48 hours at 150 ⁇ 250 °C.
  • Figure 2 is a microstructure photograph after completion of the solution treatment of Comparative Material 1.
  • Figure 3 is a microstructure photograph after the solution treatment of Inventive Material 7.
  • Figure 4 is a graph showing the results of measuring the hardness value according to the aging time for Comparative Material 1 (a) and Inventive Material 7 (b) at 200 °C.
  • Comparative Material 5 is a photograph observing the microstructure of the magnesium alloy after the aging treatment of Comparative Material 1 (a), Invention Material 7 (b), and Comparative Material 5 (c).
  • FIG. 6 is a graph showing the change in hardness value and the size of Mg-Al intermetallic compound in the grains with respect to the aging time of the invention material 7.
  • the present inventors have studied in depth to solve the problems of the ignition characteristics and low strength of magnesium alloys, it is possible to finely distribute a large amount of intermetallic compound by complex addition of B and Y and aging treatment, accordingly It was confirmed that the flame retardancy and high strength can be secured and came to complete the present invention.
  • High-strength magnesium alloy having excellent flame retardancy according to an aspect of the present invention is by weight%, Al: 2.0 ⁇ 13.0%, Mn: 0.1 ⁇ 0.5%, B: 0.0015 ⁇ 0.025%, Y: 0.1 ⁇ 1.0%, the remaining Mg and inevitable Impurities, containing at least 6.5% Mg-Al intermetallic compound by volume fraction, the average particle diameter of the Mg-Al intermetallic compound is 20 ⁇ 500nm.
  • the unit of each element content hereafter means weight% unless there is particular notice.
  • Al is an element that increases tensile strength or yield strength and improves castability by improving flowability of the molten alloy.
  • the Al content is less than 2.0%, the above effects are insufficient. On the other hand, when the Al content is more than 13.0% can increase the brittleness can reduce the workability and ductility. Therefore, the Al content is preferably 2.0 to 13.0%.
  • the lower limit of Al content may be 2.5%, and the lower limit may be 6.5% to secure a tensile strength of 160 MPa or more.
  • a more preferable upper limit of the Al content may be 12.0%, and a more preferable upper limit may be 11.0%.
  • Mn is an element that contributes to an increase in tensile strength by making grains fine by forming an intermetallic compound with Al.
  • intermetallic compounds it lowers the corrosion rate of magnesium by lowering the Fe, a representative impurity element unnecessary for magnesium alloy.
  • the Mn content is less than 0.1%, the above effects are insufficient. On the other hand, when the Mn content is more than 0.5%, brittleness may be caused by excessive formation of acicular intermetallic compounds. Therefore, the Mn content is preferably 0.1 to 0.5%.
  • the lower limit of the Mn content may be 0.11%, and the upper limit may be 0.45%.
  • B boron
  • the present invention it is added to ensure flame retardancy and high strength, and in particular, by adding B and Y to a magnesium alloy and performing aging treatment, it contributes to the formation of a large amount of Mg-Al intermetallic compound to improve tensile strength.
  • flame retardancy and strength can be further improved than when B is added alone.
  • it can contribute to preventing the oxidation of the molten metal can reduce the use of expensive SF 6 gas or SO 2 gas that can cause environmental pollution can be reduced production costs and environmental protection.
  • B content When the B content is less than 0.0015%, the above effects are insufficient. On the other hand, when the B content is greater than 0.025%, there is a problem in that the Al-B compound is formed at the grain boundary to reduce ductility. Therefore, it is preferable that B content is 0.0015 to 0.025%.
  • the lower limit of the B content may be more preferably 0.002%, and more preferably 0.02%.
  • Y is an element that combines with Al to form a precipitate and contributes to the improvement of strength, and has a high oxygen affinity to strengthen the protective film on the surface of the molten metal to inhibit oxidation of the molten metal and to improve flame retardancy even after solidification.
  • the Y content is less than 0.1%, the above effects are insufficient.
  • the Y content is more than 1.0%, there is a fear that ductility is reduced due to coarse Al-Y compound formation. Therefore, the Y content is preferably 0.1 to 1.0%.
  • the lower limit of the Y content may be 0.11%, and the upper limit may be 0.95%.
  • 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. For example, there may be Fe, Cu, Ni, Ca, Na, Ba, F, S, N and the like.
  • Zn 0.3 to 3.0% by weight% may be further included.
  • Zn is a solid solution strengthening element, and promotes the formation of Mg 17 Al 12 phase, or is an element to improve the tensile strength by forming a separate intermetallic compound containing Zn, such as Mg 2 Zn.
  • the Zn content is less than 0.3%, the above effects are insufficient.
  • the Zn content is more than 3.0%, a large amount of separate intermetallic compounds containing Zn such as Mg 2 Zn may be formed to increase brittleness, which may result in a decrease in ductility or toughness.
  • Zn content is 0.3 to 3.0%.
  • a more preferable range is 0.5 to 1.5% by weight.
  • the high-strength magnesium alloy excellent in flame retardancy according to an aspect of the present invention not only satisfies the alloy composition described above, but also contains Mg-Al intermetallic compound in a volume fraction of 6.5% or more, and the average particle diameter of the Mg-Al intermetallic compound is 20 ⁇ 500 nm.
  • Mg-Al intermetallic compound may be formed when the main alloying element added to magnesium is Al, and a representative Mg-Al intermetallic compound is Mg 17 Al 12 phase. Mg-Al intermetallic compound plays a role of ensuring high strength.
  • Mg-Al metal is used because most Al is dissolved in the Mg matrix rather than causing the formation of intermetallic compounds in the grains.
  • the formation of the liver compound is not a general phenomenon, and it is difficult to form a large amount of Mg-Al intermetallic compound.
  • a large amount of Mg-Al intermetallic compound can be secured by complex addition of B and Y and aging treatment.
  • the volume fraction of the Mg-Al intermetallic compound is less than 6.5%, it is difficult to secure high strength. Therefore, the volume fraction of the Mg-Al intermetallic compound is preferably at least 6.5%, more preferably at least 7.0%, even more preferably at least 7.5%.
  • the upper limit of the volume fraction of the Mg-Al intermetallic compound does not need to be particularly limited. However, when the Mg-Al intermetallic compound is more than 30%, the Mg-Al intermetallic compound may have a coarse particle size and may increase brittleness.
  • the volume fraction of may be 30% or less, more preferably 25% or less.
  • the average particle diameter of the Mg-Al intermetallic compound is less than 20 nm, the fraction of the Mg-Al intermetallic compound is low, making it difficult to secure high strength, and when it exceeds 500 nm, brittleness is increased.
  • the Al-Mn intermetallic compound, Al-Y intermetallic compound further comprises one or more, the total may be 5% or less in volume fraction. If it is more than 5%, the Mn and Y content may be excessive and brittleness may increase.
  • the magnet alloy of the present invention may have a ignition temperature of 700 °C or more.
  • the magnetic alloy of the present invention may have a hardness of 70Hv or more.
  • the magnet alloy of the present invention may have a tensile strength of 130 MPa or more and an elongation of 3% or more. In addition, it is possible to secure the tensile strength of 160MPa or more by controlling the Al content and the like.
  • Another aspect of the present invention is a method for producing a high-strength magnesium alloy having excellent flame retardancy, comprising: preparing a melt that satisfies the alloy composition described above; Casting the molten metal to obtain a magnesium alloy cast material; Obtaining a magnesium alloy by solution treatment of the magnesium alloy casting material in a temperature range of 370 to 490 ° C. for 2 to 20 hours; Cooling the magnesium alloy to 100 ° C. or less; And aging the cooled magnesium alloy for 2 to 48 hours at 150 to 250 ° C.
  • a molten metal that satisfies the alloy composition described above is prepared. It does not need to specifically limit, According to the general preparation of the molten metal for magnesium alloys.
  • the above-described alloying elements are prepared in accordance with the proposed composition range, and then charged into a melting crucible and then dissolved. Since the melting point of the magnesium alloy is relatively low, any method such as gas, electric furnace, induction melting furnace, etc. may be applied.
  • each alloying element may be prepared in a pure form, but may be charged to the crucible in the form of a mother alloy in which Mn, B, and Y are mixed with Mg or Al. Since B, Y, and Mn have a high melting point, it is advantageous to dissolve it in the crucible in the form of a mother alloy mixed with Mg or Al.
  • the molten metal is cast to obtain a magnesium alloy cast material.
  • the casting step need not be particularly limited as in the molten metal preparation step.
  • the method of using a movable mold and the method of using a fixed mold can be used.
  • Representative methods of using a movable mold include twin roll casting and belt casting using a movable mold such as twin roll or twin belt.
  • a typical method using a stationary mold may be continuous casting or semi-continuous casting such as billet casting, and may also include mold casting such as high pressure casting, low pressure casting, and gravity casting.
  • the above various methods can be used as the casting process, it is advantageous to apply a casting method that can increase the cooling rate because boron or yttrium having a low solubility in magnesium is added together with aluminum.
  • the mold must be cooled with cooling water, and when cooling water is applied, the mold surface must be kept above room temperature so that condensate can be removed from the mold surface before casting, and then the mold surface should be kept below room temperature after condensate is removed.
  • the magnesium alloy casting material is subjected to a solution treatment for 2 to 20 hours at a temperature range of 370 to 490 ° C. to obtain a magnesium alloy.
  • Mg-Al intermetallic compounds are also formed in magnesium alloy castings, but due to their coarse form (Coarse Mg-Al) or mixed with Mg matrix (Lamellar Mg-Al) To solute the compound.
  • the solution temperature is less than 370 °C or the holding time is less than 2 hours, the total amount of Mg-Al intermetallic compound is difficult to be employed. If the solution temperature is higher than 490 °C or holding time is more than 20 hours, the production cost increases Productivity may drop, and oxidation may occur before B and Y are added. Therefore, more preferably, it can be carried out for 2 to 20 hours in the temperature range of 400 ⁇ 460 °C.
  • the magnesium alloy is cooled to 100 ° C. or less. This is to minimize the natural aging phenomenon that may appear before aging treatment.
  • the cooling rate may be 1 ⁇ 100 °C / sec. This is to minimize the natural aging phenomenon that can occur during cooling and to prevent the precipitated Al element from randomly precipitation. For example, it is preferable to cool rapidly by methods such as forced air blowing, water cooling, oil cooling, and the like.
  • the cooled magnesium alloy is aged at 150 to 250 ° C. for 2 to 48 hours.
  • the strength of the material cannot be efficiently increased.
  • by aging treatment to precipitate a large amount of Mg-Al intermetallic compound to increase the strength to ensure excellent flame retardancy.
  • B and Y are added in the range set forth in the present invention, a large amount of Mg-Al intermetallic compound can be precipitated through the above-described aging treatment.
  • the precipitation by the aging treatment is a solid phase reaction proceeding in a solid phase, it is possible to form an Mg-Al intermetallic compound having a particle shape, an average particle diameter, a volume fraction, etc., which is advantageous for improving strength and flame retardancy.
  • the aging treatment temperature is less than 150 ° C. or the holding time is less than 2 hours, it is difficult to sufficiently secure the Mg-Al intermetallic compound.
  • the aging treatment temperature is greater than 250 ° C. or the retention time is more than 48 hours, Mg-Al intermetallic compounds may be employed, and the production cost may increase and productivity may decrease. Therefore, it is preferable to aging for 2 to 48 hours at 150 ⁇ 250 °C. More preferably, the temperature and the holding time may be increased within the temperature and the holding time according to the amount of Al added.
  • the molten metal having the component composition shown in Table 1 was cast to cast a magnesium alloy casting material having a thickness of 10 mm.
  • the magnesium alloy casting material was solution treated at 420 ° C. for 4 hours, cooled to 20 ° C., and aged at 200 ° C. for 12 hours to prepare a magnesium alloy.
  • the Mg-Al intermetallic compound and mechanical properties of the magnesium alloy were measured and listed in Table 1 below.
  • the size of the Mg-Al intermetallic compound measured the average size measured by the equivalent circular diameter.
  • Mg-Al means Mg-Al intermetallic compound.
  • the ignition temperature measurement was confirmed as the temperature at which ignition occurred while raising the temperature inside the furnace body while leaving a sample of 10 g in the form of a chip in the furnace in an atmospheric atmosphere.
  • Inventive materials satisfying the alloy composition and manufacturing conditions presented in the present invention include Mg-Al intermetallic compound by more than 6.5% by volume fraction, and the average particle diameter of the Mg-Al intermetallic compound satisfies 20 ⁇ 500nm You can check it.
  • the ignition temperature is more than 700 °C excellent flame retardancy, it can be seen that the mechanical properties are also superior to the comparative materials.
  • the comparative materials satisfy the manufacturing conditions presented in the present invention, but did not satisfy the alloy composition, it could be confirmed that the Mg-Al intermetallic compound was not sufficiently secured.
  • the flame retardancy is inferior, and the mechanical properties can be confirmed that the heat is inferior to the invention materials.
  • Comparative Material 1 is a photograph of the microstructure of the magnesium alloy cast material of Comparative Material 1 (a) and Inventive Material 7 (b).
  • the casting structure of Comparative Material 1 was composed of Mg matrix and coarse Mg-Al intermetallic compound (Coarse Mg-Al), Mg matrix and Mg-Al intermetallic compound mixed structure (Lamellar Mg-Al), and Al-Mn intermetallic.
  • Al-Y intermetallic compound (Al-Y) was observed in the cast structure of Inventive Material 7, which is composed of a compound (Al-Mn), and yttrium and boron were added, and a boron-containing intermetallic compound was separately observed. It wasn't.
  • Inventive material 7 can confirm that a large amount of Mg-Al intermetallic compound having a size of several tens of nm is precipitated, and thus the hardness value of the inventive material is greatly increased.
  • FIG. 6 shows the change in hardness value (rhombus) and the size of Mg-Al intermetallic compound (square) in grains with respect to the aging time of Inventive Material 7, and FIG. 7 shows the Mg-Al intermetallic according to the aging time. The volume fraction of the compound is shown. As shown in FIGS. 6 and 7, when the inventive material 7 was aged for 3 hours or more, the average size and volume fraction of the Mg-Al intermetallic compound were grown to 20 nm or more and 10 vol% or more, respectively.

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Abstract

L'un des aspects de la présente invention concerne un alliage de magnésium de résistance élevée présentant une excellente ininflammabilité, l'alliage de magnésium comprenant de 2,0 à 13,0 % en masse d'Al, de 0,1 à 0,5 % en masse de Mn, de 0,0015 à 0,025 % en masse de B, et de 0,1 à 1,0 % en masse d'Y, le reste comprenant Mg et d'autres impuretés inévitables, et comprenant 6,5 % ou plus d'un composé intermétallique Mg-Al en termes de fraction volumique, le composé intermétallique Mg-Al ayant une granulométrie moyenne de 20 à 500 nm.
PCT/KR2017/015291 2016-12-21 2017-12-21 Alliage de magnésium de résistance élevée présentant une excellente ininflammabilité, et son procédé de production Ceased WO2018117713A1 (fr)

Priority Applications (4)

Application Number Priority Date Filing Date Title
CN201780079314.7A CN110114485A (zh) 2016-12-21 2017-12-21 耐燃性优异的高强度镁合金及其制造方法
JP2019533182A JP2020509196A (ja) 2016-12-21 2017-12-21 難燃性に優れた高強度マグネシウム合金及びその製造方法
US16/471,939 US20200087757A1 (en) 2016-12-21 2017-12-21 High strength magnesium alloy with excellent flame retardancy, and method for producing same
EP17883943.7A EP3561097A4 (fr) 2016-12-21 2017-12-21 Alliage de magnésium de résistance élevée présentant une excellente ininflammabilité, et son procédé de production

Applications Claiming Priority (2)

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KR10-2016-0176119 2016-12-21
KR1020160176119A KR101858856B1 (ko) 2016-12-21 2016-12-21 난연성이 우수한 고강도 마그네슘 합금 및 그 제조방법

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US (1) US20200087757A1 (fr)
EP (1) EP3561097A4 (fr)
JP (1) JP2020509196A (fr)
KR (1) KR101858856B1 (fr)
CN (1) CN110114485A (fr)
WO (1) WO2018117713A1 (fr)

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WO2025177884A1 (fr) * 2024-02-21 2025-08-28 日本精機株式会社 Alliage de magnésium et élément en alliage de magnésium
KR20250175418A (ko) 2024-06-10 2025-12-17 파인트리포스마그네슘 주식회사 난연성이 우수하고 고강도의 마그네슘 합금 및 이의 제조방법

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EP3561097A1 (fr) 2019-10-30
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KR101858856B1 (ko) 2018-05-17
CN110114485A (zh) 2019-08-09

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