EP2319949A1 - Kaltgewalztes legierungsprodukt auf mg-basis - Google Patents

Kaltgewalztes legierungsprodukt auf mg-basis Download PDF

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Publication number
EP2319949A1
EP2319949A1 EP09800476A EP09800476A EP2319949A1 EP 2319949 A1 EP2319949 A1 EP 2319949A1 EP 09800476 A EP09800476 A EP 09800476A EP 09800476 A EP09800476 A EP 09800476A EP 2319949 A1 EP2319949 A1 EP 2319949A1
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Prior art keywords
deformation
shows
cold
alloy
nominal
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Granted
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EP09800476A
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English (en)
French (fr)
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EP2319949A4 (de
EP2319949B1 (de
Inventor
Toshiji Mukai
Hidetoshi Somekawa
Tetsuya Shoji
Akira Kato
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National Institute for Materials Science
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National Institute for Materials Science
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    • 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
    • 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
    • C22C23/06—Alloys based on magnesium with a rare earth metal 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

Definitions

  • the present invention relates to an Mg-based alloy to which yttrium or another lanthanoid-series rare earth element has been added and relates to an Mg-based alloy which can be easily plastically worked.
  • the present invention has as its object to provide an Mg-based alloy cold worked member which can remarkably lower the load weight required for cold plastic working and enables practical usage of the same.
  • the present invention provides an Mg-based alloy cold worked member obtained by cold working an Mg-based alloy to form it into a predetermined shape, characterized by having a microstructure which includes crystal grains divided and made finer by cold working.
  • the Mg-based alloy forming the member has one or more types of lanthanoid-series rare earth elements added to it.
  • the average value of the crystal grain size is 30 ⁇ m or less.
  • the anisotropy of deformation normally observed in conventional wrought alloys such as the AZ31 alloy is eliminated and the demerit that, for example, the yield stress when a tensile load acts, that is, the plastic deformation starting stress, having to be 1.2 to 1.4 times the plastic deformation starting stress when a compressive load acts is eliminated.
  • the present alloy has isotropy of deformation. Equal deformation in all directions is exhibited for a constant load. At the same time, the load which is required for deformation work does not depend on the load either and is equal.
  • the Mg-based alloy has an alloy microstructure which is homogeneous as a whole in 1 ⁇ m 3 units and has high Y concentration parts of average diameters of 2 to 50 nm dispersed irregularly in 1 ⁇ m 3 .
  • the Mg-based alloy has high Y concentration parts of high concentrations of 1.5 times or more the Y concentration in 1 ⁇ m 3 units.
  • the internal structure of the material of the present invention is characterized in that regions in which the yttrium atoms are present in a concentration higher by 50% or more of the average concentration in the material, that is, a 1.5 times or higher concentration, form sizes of average diameters of 2 nm to 50 nm and, furthermore, these high concentration regions are distributed in the crystal grains of the material at intervals of 2 nm to 50 nm.
  • the yttrium atoms distributed in a high concentration do not form intermetallic compounds with the matrix of the magnesium atoms, that is, a regular structure, but form a high concentration, but random distribution.
  • the material of the present invention is characterized in that, by being cold worked at a nominal strain of 0.15 or more (as absolute value of equivalent strain, 0.17 or more), its internal crystal microstructure is divided and made finer whereby it is given crystal grain sizes of average values of 30 ⁇ m or less.
  • the Mg-based alloy of the present invention can be used to produce any long bars, sheet materials, or block materials. It becomes possible to secure cold workability of magnesium, which had been considered difficult in the past. It is expected to contribute much to all sorts of applications as a light weight structural material.
  • Yttrium (Y) and pure magnesium (Mg) (purity 99.95%) were completely melted in an argon atmosphere and cast in iron casting molds to prepare nine types of Mg-Y alloys having Y contents of 0.1 at%, 0.3 at%, 0.6 at%, 1.0 at%, 1.2 at%, 1.5 at%, 2.0 at%, 2.2 at%, and 3.0 at%. Table 1 shows these as Examples 1 to 18 and Comparative Example 1.
  • the obtained cast alloys were held at a temperature of 500°C for 24 hours in a furnace (air atmosphere), then water cooled for solution treatment.
  • FIG. 1 is a high resolution transmission type electron microscope photograph of the internal microstructure forming the present alloy.
  • the fine dots forming FIG. 1 show the positions of present of the component atoms. This photograph is taken from a direction parallel to a certain crystal plane of the present alloy (Example 4), so that majority of the points, that is, atoms, are arranged on a certain line in the structure.
  • the present alloy is characterized in that the yttrium atoms do not form regular structures with the magnesium matrix atoms, that is, so-called “intermetallic compounds", but form high concentration regions of yttrium.
  • the sizes of the lattice distorted regions can be measured from an electron micrograph such as shown in the illustration. Based on the results of measurement, it was confirmed that the lattice distorted regions had an average diameter size of 2 to 50 nm and dispersion interval of 2 to 50 nm. However, in some regions, formation of unavoidable intermetallic compounds was observed, so the formation of high concentration regions where over half of the yttrium atoms are distributed at random is made the characterizing feature of the present alloy.
  • concentration of yttrium can be made a range of 0.1 at% to 3.0 at%.
  • the method of production of the material comprises production of an alloy having a predetermined yttrium concentration by casting etc., extrusion etc. to impart hot an equivalent plastic strain of 1 or more to the material, then holding it isothermally at 300 to 550°C in range.
  • FIG. 2 is a high resolution transmission type electron microscope photograph of the internal microstructure forming the present alloy (Example 4). This photograph uses the Z contrast method to show the yttrium atoms, which are heavier atoms than magnesium matrix atoms, as dots of different contrasts. For example, the white broken line circles or white broken line ellipses in the figure show regions where large numbers of yttrium atoms are concentrated.
  • the top figure of FIG. 3 is a photograph which shows the locations of presence of yttrium atoms observed by a 3D atom probe by dots for the present alloy (Example 4).
  • the bottom figure is a schematic view based on the distribution of the top figure and shows the regions where yttrium atoms are segregated at a high concentration by gray color contour figures.
  • the average concentration of the yttrium in the illustrated alloy is 0.6 at%.
  • the size and dispersion interval of regions of 1.0 at% or more concentration regions, that is, regions where the concentrations are 1.67 times or more of the average concentration, are shown.
  • the sizes of the concentration regions are 5 to 15 nm.
  • the intervals between regions are also 5 to 15 nm. Results similar to the strain regions of FIG. 1 and the high concentration regions of FIG. 2 are shown.
  • FIG. 4 is a graph showing the compressive nominal stress-nominal strain relationship of the present alloy for the Mg-0.6at%Y alloy of Example 4. As the directions of the compression tests, three are selected: one parallel to the extrusion direction of the extruded material (180°), one perpendicular to it (90°), and one between the two (45°).
  • the yield stress that is, the plastic deformation start stress
  • the yield stress is about 60 MPa.
  • the non-directional dependent compressive deformation performance such as shown above is a property not exhibited by the conventional wrought materials of AZ31 alloy etc.
  • FIG. 5 is a graph for the case where obtaining a test piece from a member, in the compression test shown in FIG. 4 , given a nominal strain of 0.4 in a direction parallel to extrusion, that is, compressive deformation until 60% of the initial height, and performing a static compression test in the same way as the case of FIG. 4 .
  • the present alloy has plastic workability at room temperature, that is, cold workability, and, furthermore, the mechanical properties after plastic working are excellent as well.
  • the die set such as shown in FIG. 6 was used to evaluate the plastic workability.
  • a test piece before deformation was made a columnar shape of a diameter of 8 mm and a height of 6 mm. This was set at a bottom die of tool steel having a columnar cross-section hole of the same diameter.
  • the top die which has a columnar cross-section hole of a diameter of 3 mm at the center axis and an R part of a radius of 1.5 mm at the shoulders, was brought into contact with the top surface of the test piece.
  • the top die was made to move from the top to the bottom of the figure so as to make the test piece constrained by the bottom die plastically flow along the center hole provided in the top die to thereby confirm the shapeability. Note that the surfaces of the test piece and die were coated with a lubricant of silicone grease.
  • a boss of the same diameter as the top die such as shown in FIG. 6 is formed into a protruding shape, so from the observation of the cross-section after working, it is possible to directly confirm the shapeability and any cracking along with working.
  • FIG. 7 is a graph using a jig shown in FIG. 6 for evaluating the cold workability.
  • the load required for shaping the present alloy to obtain the same shaping height is about 20 to 40% lower compared with the case of the conventional material of AZ31.
  • FIG. 8 is a photograph of the cross-section of a sample after shaping. It shows the results of an extrusion speed of 0.0003 mm/sec and a 4.5 ton load.
  • the top figure shows the case of the AZ31 alloy shown in Comparative Example 1.
  • the shaping height including the R part was 1.8 mm.
  • the bottom figure shows an example of the Mg-0.6at%Y alloy of the present alloy (Example 4).
  • the shaping height was 3.7 mm.
  • a shaping height of at least 2 times that of an AZ31 alloy was obtained. The shapeability of the present alloy was therefore confirmed.
  • FIG. 9 is a photograph of the cross-section of a sample after shaping. Here, it shows the results of an extrusion speed of 0.03 mm/sec and a 4.5 ton load.
  • the top figure shows the case of the AZ31 alloy shown in Comparative Example 1.
  • the shaping height, including the R part, was 1.4 mm.
  • the bottom figure shows the Mg-0.6at%Y alloy of the present alloy (Example 4).
  • the shaping height was 2.9 mm. A shaping height of at least 2 times that of an AZ31 alloy was obtained. The shapeability of the present alloy was therefore confirmed.
  • FIG. 10 shows the changes in distribution of orientation of crystal grains before and after compressive deformation of a material of Mg-0.6at%Y extruded at 425°C and held at 400°C for 24 hours and the average crystal grain size.
  • it shows the internal microstructure formed before shaping and after 4% (nominal strain 0.04), 15% (nominal strain 0.15), and 25% (nominal strain 0.25) deformation.
  • the average crystal grain size becomes 30 ⁇ m or less, that is, becomes finer.
  • FIG. 11 shows the internal microstructure formed after deformation of a material similar to FIG. 10 by 45% (nominal strain 0.45).
  • the boundary lines shown by the black lines in the figure show parts where the crystal orientation difference is 5 degrees or more as the crystal grain boundaries. Compared with the microstructure before deformation shown in FIG. 10 , it is learned that the crystal grain size is made a finder 1/5 size.
  • FIG. 12 is an enlarged view of the internal microstructure formed after deformation of a material similar to FIG. 10 by 15% (nominal strain 0.15).
  • the changes in crystal orientation on the lines shown by L and T in the figure are shown by the solid lines in the right figures.
  • the locations where the density changes, for example, the parts shown by the white arrows in the figure, clearly show an increase of the orientation angle by 5 degrees from the bottom right graph. That is, the cold worked member of the present invention, by being cold worked, changes in orientation inside certain crystal grains. Along with the increase of the strain imparted, the difference in crystal orientation becomes greater. Finally, crystal grain boundaries are formed, whereby the crystal grains are divided and the average crystal grain size inside the material becomes finer, it is shown.
  • FIG. 13 shows the change in microstructure formed inside a material after cold working of a comparative material, obtained by extruding the conventional material of an AZ31 alloy at 250°C, then holding it at 400°C for 24 hours, by the method shown in FIG. 6 by a top die at a speed of 0.0003 mm/sec. At the center part D of the worked material, no division of the crystal grains is seen. Deformation twins are formed as a banded structure in an oblique direction.
  • FIG. 14 shows the change in microstructure formed inside a material after cold working of a material, obtained by extruding Mg-0.6at%Y at 320°C, then holding it at 400°C for 24 hours, by the method shown in FIG. 6 by a top die at a speed of 0.0003 mm/sec.
  • a top die At the center part D of the worked material, there is no formation of a banded structure in any specific direction such as deformation twins. New grain boundaries are formed in random directions, it is learned.
  • FIG. 15 shows the change in microstructure formed inside a material after cold working of a material, obtained by extruding Mg-0.1at%Y at 290°C, then holding it at 400°C for 24 hours, by the method shown in FIG. 6 by a top die at a speed of 0.0003 mm/sec.
  • a top die At the center part D of the worked material, there is no formation of a banded structure in any specific direction such as deformation twins. New grain boundaries are formed in random directions, it is learned.
  • FIG. 16 shows, as an example of cold working, the internal microstructure of a boss-shaped protrusion formed after cold working a material, obtained by extruding Mg-0.1at%Y at 290°C and holding it at 400°C for 24 hours, and a material, obtained by extruding Mg-0.3at%Y at 300°C and holding it at 400°C for 24 hours, by the method shown in FIG. 6 by a top die at a speed of 0.0003 mm/sec and 3.0 mm/sec.
  • FIG. 17 shows, as an example of cold working, the internal microstructure of a boss-shaped protrusion formed after cold working a material, obtained by extruding Mg-0.1at%Y at 290°C and holding it at 400°C for 24 hours, and a material, obtained by extruding Mg-0.3at%Y at 300°C and holding it at 400°C for 24 hours, by the method shown in FIG. 6 by a top die at a speed of 3.0 mm/sec.
  • the microstructure of the part shown by D is shown. It is learned that by a working speed of a speed of 3.0 mm/sec, similar crystal grain refinement occurs.
  • FIG. 18 shows, as an example of cold working, the internal microstructure of a boss-shaped protrusion formed after cold working a material, obtained by extruding Mg-0.1at%Y at 290°C and holding it at 400°C for 24 hours, by the method shown in FIG. 6 by a top die at a speed of 0.0003 mm/sec. From the distribution chart of orientation of the microstructure after deformation, it is learned that the crystal grain structure becomes finer.
  • FIG. 19 shows that the hardness of a protrusion formed after shaping by the cold working method described in FIG. 6 increases in comparison with parts with little amounts of deformation. It is learned that refinement of the crystal grains due to cold working increases the strength.
  • FIG. 20 shows, as a comparative example, a nominal stress-nominal strain curve (top figure) obtained when causing compressive deformation of a material obtained by extruding pure magnesium at 328°C and holding it at 400°C for 24 hours and a nominal stress-nominal strain curve obtained when causing compressive deformation of a compression test piece, obtained by stopping deformation at a nominal strain of 0.14, then machining again, in parallel and perpendicular directions to the extrusion.
  • the yield strength greatly differs and anisotropy of deformation can be confirmed.
  • FIG. 21 shows, as an example, a nominal stress-nominal strain curve (top figure) obtained when causing compressive deformation of a material obtained by extruding Mg-0.3at%Y at 300°C and holding it at 400°C for 24 hours and a nominal stress-nominal strain curve obtained when causing compressive deformation of a compression test piece, obtained by stopping deformation at a nominal strain of 0.4, then machining again, in parallel and perpendicular directions to the extrusion. It can be confirmed that the anisotropy of the yield strength is reduced.
  • FIG. 22 shows, as an example, a nominal stress-nominal strain curve (top figure) obtained when causing compressive deformation of a material obtained by extruding Mg-1.0at%Y at 425°C and holding it at 400°C for 24 hours and a nominal stress-nominal strain curve obtained when causing compressive deformation of a compression test piece, obtained by stopping deformation at a nominal strain of 0.4, then machining again, in parallel and perpendicular directions to the extrusion. It can be confirmed that the anisotropy of the yield strength is reduced.
  • FIG. 23 shows, as an example, a nominal stress-nominal strain curve (top figure) obtained when causing compressive deformation of a material obtained by extruding Mg-0.3at%Yb at 300°C and holding it at 450°C for 24 hours and a nominal stress-nominal strain curve obtained when causing compressive deformation of a compression test piece, obtained by stopping deformation at a nominal strain of 0.4, then machining again, in parallel and perpendicular directions to the extrusion. It can be confirmed that the anisotropy of the yield strength and rate of work hardening is reduced.
  • FIG. 24 shows, as an example, a nominal stress-nominal strain curve (top figure) obtained when causing compressive deformation of a material obtained by extruding Mg-0.3at%Gd at 300°C and holding it at 450°C for 24 hours and a nominal stress-nominal strain curve obtained when causing compressive deformation of a compression test piece, obtained by stopping deformation at a nominal strain of 0.35, then machining again, in parallel and perpendicular directions to the extrusion. It can be confirmed that the anisotropy of the yield strength and rate of work hardening is reduced.
  • FIG. 25 shows, as a comparative example, the crystal grain structure of a material obtained by extruding Mg-0.6at%Y at an extrusion ratio of 25:1 and a temperature of 320°C.
  • the black line in the figure shows the interface of a crystal orientation difference of 5° or more as a crystal grain boundary.
  • FIG. 26 shows the results when taking test pieces in the parallel and perpendicular directions of extrusion from the material obtained by extrusion of Mg-0.6at%Y at an extrusion ratio of 25:1 and temperature of 320°C shown as a comparative example in FIG. 25 and testing them by a compression test at room temperature. It is learned that the nominal strain at the time of break is 0.13 or less and that, while having a composition similar to the alloys of the working examples shown in FIG. 4 and FIG. 5 , the cold workability is lower. Further, the rate of work hardening after yielding greatly differs depending on the direction in which the sample is taken. It is learned that the nominal stress right before breakage at the time of a compression test in a direction parallel to extrusion becomes a value close to two times that in the direction perpendicular to extrusion, so the anisotropy of deformation is strong.
  • an Mg-based alloy cold worked member which can remarkably lower the load weight required for cold plastic working is provided and can be practically used.

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  • Materials Engineering (AREA)
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  • Metallurgy (AREA)
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EP09800476.5A 2008-07-22 2009-07-22 Kaltgewalztes legierungsprodukt auf mg-basis Not-in-force EP2319949B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2008188397 2008-07-22
PCT/JP2009/063452 WO2010010965A1 (ja) 2008-07-22 2009-07-22 Ｍｇ基合金冷間加工部材

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EP2319949A1 true EP2319949A1 (de) 2011-05-11
EP2319949A4 EP2319949A4 (de) 2012-12-12
EP2319949B1 EP2319949B1 (de) 2015-02-18

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US (1) US20110135532A1 (de)
EP (1) EP2319949B1 (de)
JP (1) JP5549981B2 (de)
CN (1) CN102105613A (de)
WO (1) WO2010010965A1 (de)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2835437A1 (de) * 2012-05-31 2015-02-11 National Institute for Materials Science Magnesiumlegierung, magnesiumlegierungselement und verfahren zur herstellung davon sowie verfahren zur verwendung der magnesiumlegierung

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
PL2967012T3 (pl) 2013-03-14 2021-04-19 Erasmus University Medical Center Rotterdam Transgeniczne ssaki inne niż człowiek do wytwarzania przeciwciał

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Publication number Priority date Publication date Assignee Title
JPH0941066A (ja) * 1995-08-01 1997-02-10 Mitsui Mining & Smelting Co Ltd 冷間プレス加工可能なマグネシウム合金
JP2001294966A (ja) * 2000-04-14 2001-10-26 Matsushita Electric Ind Co Ltd マグネシウム合金薄板及びその製造方法並びにそれを用いた成形品
JP2003328065A (ja) * 2002-05-10 2003-11-19 Toyo Kohan Co Ltd 成形性に優れる展伸用マグネシウム薄板およびその製造方法
WO2006003899A1 (ja) * 2004-06-30 2006-01-12 Sumitomo Electric Industries, Ltd. マグネシウム合金材の製造方法
JP2006016658A (ja) * 2004-06-30 2006-01-19 National Institute For Materials Science 高強度・高延性マグネシウム合金及びその製造方法
WO2007058276A1 (ja) * 2005-11-16 2007-05-24 National Institute For Materials Science マグネシウム系生分解性金属材料
JP2008214668A (ja) * 2007-02-28 2008-09-18 National Institute Of Advanced Industrial & Technology マグネシウム合金プレス成形体及びその作製方法

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Publication number Priority date Publication date Assignee Title
JPH0941066A (ja) * 1995-08-01 1997-02-10 Mitsui Mining & Smelting Co Ltd 冷間プレス加工可能なマグネシウム合金
JP2001294966A (ja) * 2000-04-14 2001-10-26 Matsushita Electric Ind Co Ltd マグネシウム合金薄板及びその製造方法並びにそれを用いた成形品
JP2003328065A (ja) * 2002-05-10 2003-11-19 Toyo Kohan Co Ltd 成形性に優れる展伸用マグネシウム薄板およびその製造方法
WO2006003899A1 (ja) * 2004-06-30 2006-01-12 Sumitomo Electric Industries, Ltd. マグネシウム合金材の製造方法
JP2006016658A (ja) * 2004-06-30 2006-01-19 National Institute For Materials Science 高強度・高延性マグネシウム合金及びその製造方法
WO2007058276A1 (ja) * 2005-11-16 2007-05-24 National Institute For Materials Science マグネシウム系生分解性金属材料
JP2008214668A (ja) * 2007-02-28 2008-09-18 National Institute Of Advanced Industrial & Technology マグネシウム合金プレス成形体及びその作製方法

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2835437A1 (de) * 2012-05-31 2015-02-11 National Institute for Materials Science Magnesiumlegierung, magnesiumlegierungselement und verfahren zur herstellung davon sowie verfahren zur verwendung der magnesiumlegierung
EP2835437A4 (de) * 2012-05-31 2015-07-15 Nat Inst For Materials Science Magnesiumlegierung, magnesiumlegierungselement und verfahren zur herstellung davon sowie verfahren zur verwendung der magnesiumlegierung

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JP5549981B2 (ja) 2014-07-16
CN102105613A (zh) 2011-06-22
WO2010010965A1 (ja) 2010-01-28
US20110135532A1 (en) 2011-06-09
EP2319949A4 (de) 2012-12-12
EP2319949B1 (de) 2015-02-18
JPWO2010010965A1 (ja) 2012-01-05

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