WO2012070870A2 - Feuille d'alliage de magnésium ayant une aptitude supérieure au façonnage à la température ambiante et son procédé de fabrication - Google Patents

Feuille d'alliage de magnésium ayant une aptitude supérieure au façonnage à la température ambiante et son procédé de fabrication Download PDF

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WO2012070870A2
WO2012070870A2 PCT/KR2011/008991 KR2011008991W WO2012070870A2 WO 2012070870 A2 WO2012070870 A2 WO 2012070870A2 KR 2011008991 W KR2011008991 W KR 2011008991W WO 2012070870 A2 WO2012070870 A2 WO 2012070870A2
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Prior art keywords
magnesium alloy
alloy sheet
weight
magnesium
rolling
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Korean (ko)
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WO2012070870A3 (fr
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김낙준
배준호
김동욱
김도향
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POSTECH Academy Industry Foundation
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POSTECH Academy Industry Foundation
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Publication of WO2012070870A3 publication Critical patent/WO2012070870A3/fr
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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
    • C22C23/04—Alloys based on magnesium with zinc or cadmium as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/06—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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
    • B22D11/06—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars
    • B22D11/0622—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars formed by two casting wheels

Definitions

  • the present invention relates to a magnesium alloy sheet having excellent room temperature formability and a method of manufacturing the same. More specifically, the present invention exhibits excellent press formability through secondary phase control, sheet casting, and subsequent processing heat treatment through an alloy component added to magnesium.
  • the present invention relates to a method for producing a magnesium plate that can secure high strength through additional heat treatment after molding and to a magnesium plate produced by the method.
  • Magnesium alloy is an alloy for structural materials exhibiting the lowest specific gravity, excellent specific strength, and rigidity among practical structural materials. Recently, demand is increasing for cases of mobile devices and materials for automobiles that require weight reduction.
  • this method is a grain size It is characterized in that the large grain size of the cast material by hot extrusion to make a material capable of pressing or forging.
  • magnesium is a highly active metal, surface blackening and combustion are likely to occur due to processing heat generated during hot extrusion. Accordingly, in the hot extrusion process of magnesium, extrusion must be performed at a speed that can be cooled to a degree that surface blackening or combustion does not occur, thereby limiting the extrusion speed.
  • the hot extrusion process which is essential for the conventional magnesium sheet process, has been a major factor in lowering productivity and increasing manufacturing cost. Moreover, since there is a limit to making the crystal grains fine only by the hot extrusion process, there is also a problem that it is difficult to beautifully process into a complicated shape.
  • Y yttrium
  • Zn zinc
  • a magnesium alloy sheet with improved press formability was proposed through the refinement of the structure and the control of the dispersed phase behavior by a subsequent work heat treatment process.
  • the magnesium alloy has a problem of not only using expensive yttrium, but also having low press formability compared to commercial aluminum, which has a certain limit in the application field.
  • the present invention has been researched and developed to solve the problems of the conventional magnesium alloy sheet and its manufacturing method, and can be manufactured at low cost using a low-cost alloy element, and also has a press formability equivalent to commercial aluminum Therefore, to solve the problem to provide a magnesium alloy plate and a method of manufacturing the same that can be suitably used for the production of a variety of complex parts.
  • the present invention provides a magnesium alloy sheet material containing Zn and Ca as an alloying element, the limit dome height (LDH) is 7mm or more, preferably 8mm or more.
  • LDH 'Limit Dome Height
  • the content of the Zn is 1 to 10% by weight, preferably 1 to 7% by weight
  • the content of Ca is 0.1 to 5% by weight, preferably 0.5 to 3% by weight It is characterized by that.
  • the magnesium alloy sheet material according to the present invention is characterized in that the grain size average grain size is 10 ⁇ m or less.
  • the magnesium alloy sheet according to the present invention is characterized in that the yield strength (YS) is 200MPa or more, the tensile strength (UTS) is 270MPa or more, and the elongation (EL) is 12% or more.
  • the magnesium alloy sheet according to the present invention is characterized in that the texture intensity of the (0002) plane is 2.5 or less.
  • the present invention to solve the above problems, (a) Zn: 1 to 10% by weight, Ca: 0.1 to 5% by weight to prepare a molten alloy of the alloy consisting of magnesium and magnesium inevitable; (b) maintaining the molten metal in a temperature range from a temperature at which the liquid fraction is 70% to a temperature before the molten metal is ignited; (c) injecting the molten metal maintained in the temperature range between two rotating cooling rolls to form a thin sheet of magnesium alloy sheet; (d) solution treatment of the cast magnesium alloy plate at 300 to 490 ° C. for 1 to 24 hours; (e) preheating the solution-treated magnesium alloy sheet to 300 to 400 ° C. and then rolling it to a required thickness of 1 to 45% per pass with a heated rolling roll; And (f) performing a solution treatment at 300 to 490 ° C. for 0.5 to 4 hours after the rolling.
  • the gap between the two cooling rolls in the step (c) is 1 to 5mm and the rotational speed of the cooling roll during the injection of the molten metal is 0.2 to 20m / min, It characterized in that the cooling rate of 10 2 ⁇ 10 3 K / s.
  • the content of Zn is 1 to 10% by weight, preferably 1 to 7% by weight
  • the content of Ca is 0.1 to 5% by weight, preferably 0.5 ⁇ 3% by weight is characterized in that.
  • the method for producing a magnesium alloy sheet according to the present invention may further include the step of performing an aging treatment for 1 to 72 hours at 150 to 200 °C the solution-treated magnesium alloy sheet after the rolling.
  • the method for producing a magnesium alloy sheet according to the present invention is characterized in that the addition of Ca is carried out by a method of adding a Mg-Ca mother alloy. This is because, when pure Ca is used, the melting point of Ca is not so high that it is not easily added as desired in casting, and the Mg-Ca master alloy is preferably a Mg-2 to 3.5 wt% Ca master alloy.
  • Zn is 6.2% by weight at 340 ° C in the maximum solid solution at Mg, and when 1.0% by weight or more is added, Zn forms an acicular precipitate through heat treatment. The hardening phenomenon is hardly expected, and when Zn is added in excess of 10% by weight, equilibrium precipitation may be encouraged at grain boundaries, resulting in deterioration of mechanical properties. Therefore, the content of Zn is preferably 1 to 10% by weight.
  • the addition of an appropriate amount of Zn leads to softening of the base and activates the base slip, but the addition of more Zn causes not only the bottom base but also a decrease in mechanical properties. In order to maximize the slip and precipitation strengthening effect of the upper limit of Zn is more preferably limited to 7% by weight.
  • Ca is an effective element for improving the high temperature strength of magnesium alloy. If the Ca content is less than 0.1% by weight, the effect of increasing the high temperature strength is insufficient, and if the Ca content is more than 5% by weight, the spreading decreases and the fluidity of the molten metal is reduced, resulting in poor castability and hot cracking. When solidified, the adhesion to the mold increases, resulting in a decrease in productivity. Therefore, the content of Ca is preferably in the range of 0.1 to 5% by weight, more preferably 0.5 to 3% by weight because the effect can be maximized.
  • the unavoidable impurity refers to a component that is incorporated in an unintentional state in a raw material or a manufacturing process, and the incorporated component is preferably contained at 0.5 wt% or less so as not to affect the physical properties of the magnesium alloy according to the present invention. More preferably 0.01% by weight or less.
  • elements such as Fe, Ni, Cr, Cu, Co, etc. may adversely affect the corrosion resistance, so management is required to be 0.005% by weight or less.
  • the grain size average grain size of the microstructured grains is preferably 10 ⁇ m or less.
  • the increase in texture intensity in magnesium alloys inhibits formability in the case of magnesium having a low slip system, and the texture intensity of the (0002) surface, which is the base surface, is 2.5 or less. If not, since it is difficult to implement press formability comparable to that of aluminum alloy, 2.5 or less is preferable, and more preferably 2.2 or less.
  • the melt temperature of the step (b) is less than the temperature at which the liquid fraction is 70% or less, the viscosity of the melt increases, so that the melt solidifies before contacting the cooling roll of the step (c) and does not exit the roll. Since the process cannot be performed when the temperature to be ignited is exceeded, the molten metal temperature should be maintained in the above range.
  • the cooling rate of the molten metal in the step (c) is less than 10 2 K / s, there is a problem that the cooling rate is slow, there is no significant difference in the microstructure of the general mold casting method and the flow of the molten metal before the casting can be unstable, If it exceeds 10 3 K / s, it is difficult to reach it commercially except for the quench solidification method, which obtains a very thin ribbon, so it is preferable to keep it at 10 2 to 10 3 K / s. Maintaining the gap between the rolls of 10 mm or less is also advantageous for obtaining the cooling rate as described above.
  • the fast cooling rate as in step (c) not only refines the cast structure and reduces segregation, but also finely disperses the intermetallic compounds in the matrix that play a detrimental role in tensile properties when the cooling rate is slow. Rather, it can play a beneficial role.
  • it is possible to manufacture a relatively thin plate compared to other casting methods in the casting step it is possible to reduce the rolling reduction rate and the rolling pass in the rolling process, thereby minimizing the texture generated in the rolling process, which adversely affects press formability.
  • the anisotropy of the plate can be reduced.
  • the solution treatment because the unevenness of the processed material may occur due to segregation of alloy elements that may occur during casting, and the solution treatment temperature and time are the main alloy elements. It is set in consideration of the diffusion of Zn, secondary dendrite arm spacing (SDAS), incipient melting and oxidation degree measured through DTA / DSC, and should be performed under conditions of 1 to 24 hours at 300 to 490 ° C. Sufficient solution treatment results can be obtained.
  • SDAS secondary dendrite arm spacing
  • the preheated temperature range may not be maintained when the solution-treated magnesium alloy sheet is preheated at 300 to 400 ° C. and then rolled to a required thickness of 1 to 45% per pass with a heated rolling roll.
  • it is preferable to maintain the preheating temperature range because it is difficult to obtain a healthy plate, and it is preferable to keep the reduction rate per pass in the range of 1 to 45% because the aggregate structure develops and the moldability decreases as the reduction amount increases. .
  • it may comprise the step of performing the aging treatment for 1 to 96 hours at 150 ⁇ 200 °C heat-treated magnesium alloy plate material after the rolling, which is most This is because the tensile properties can be improved efficiently.
  • the alloy component suitable for the twin roll type sheet casting method, grain refinement and intermetallic compound formation and volume fraction control by thin sheet casting and subsequent heat treatment or processing heat treatment Through the conventional commercial magnesium alloy sheet, the strength and room temperature as well as the elongation and formability is improved to provide a room temperature forming magnesium sheet that can be widely applied to the automotive and electronics industry.
  • the manufacturing method of the magnesium alloy plate material which concerns on this invention, since a manufacturing process number is reduced compared with the conventional manufacturing process of a plate material, a magnesium alloy plate material can be manufactured at low cost compared with the conventional commercial magnesium alloy plate material. In addition, since the final reduction can be greatly reduced, it is possible to minimize the formation of the aggregate structure, from which an improved press formability can be obtained.
  • FIG. 1 is a schematic view of a sheet casting apparatus for producing a magnesium alloy sheet used in an embodiment of the present invention.
  • Figure 2 is a schematic diagram showing the evaluation method of the limit dome height of the magnesium alloy sheet according to the present invention.
  • Figure 3 shows the microstructure of the thin plate cast magnesium plate according to an embodiment of the present invention observed with an optical microscope after 1 hour heat treatment at 440 °C.
  • Figure 4 shows the microstructure observed by the optical microscope after 30 minutes solution treatment at 440 °C after rolling a thin sheet cast magnesium alloy sheet according to an embodiment of the present invention.
  • Figure 5 shows the microstructure observed by transmission electron microscope after 30 minutes solution treatment at 440 °C after rolling 0.95Zn, 0.9Ca alloy.
  • Figure 6 shows the microstructure observed by transmission electron microscope after 30 minutes solution treatment at 350 °C after rolling a 5.99Zn, 0.98Ca alloy.
  • Figure 7 shows the deformation of the specimen before and after the solution treatment after 30 minutes solution treatment at 440 °C after rolling 0.95Zn, 0.9Ca alloy using EBSD.
  • FIG. 8 shows the deformation of the specimens before and after the 30 minute solution treatment at 350 ° C. after rolling the 5.99 Zn and 0.98Ca alloys using EBSD.
  • 9A and 9B show the results of analysis of a basal pole figure of a magnesium alloy sheet manufactured according to an embodiment of the present invention, respectively.
  • Figure 10 shows the (0002) aggregate strength and LDH of the magnesium alloy sheet according to the embodiment and the comparative example of the present invention.
  • a magnesium alloy molten metal was prepared by dissolving a pure Mg (99.9%), a pure Zn (99.9%), and a Mg-3 wt% Ca master alloy under a CO 2 and SF 6 mixed gas atmosphere. At this time, the content ratio of each component in the prepared molten metal was set to the composition of Table 1 below.
  • a twin roll plate casting apparatus includes a melting furnace 10, a nozzle 20, and two cooling rolls 30.
  • the casting method using the twin roll type sheet casting apparatus is specifically, a temperature of about 70% of the molten metal dissolved in the above composition in the induction melting furnace 10 under a CO 2 and SF 6 mixed gas atmosphere (about 650). At a temperature of about 950 ° C. up to the temperature before the molten metal is ignited, and then transferred to the nozzle 20. In this case, if the temperature of the molten metal is too high, a liquid phase may exist inside the plate that has passed through the cooling roll, and thus, in the embodiment of the present invention, the melt is transferred to the nozzle 20 while maintaining the temperature below 750 ° C, specifically 710 ° C. .
  • the molten metal whose temperature is maintained at 710 ° C. is injected through the nozzle 20 between two cooling rolls 30 being cooled by a cooling device (not shown) provided in the twin roll sheet casting device.
  • a cooling device not shown
  • the casting speed of the molten metal was cast to be 200 ⁇ 300K / s under such conditions
  • a magnesium alloy sheet having a length of about 5 m, a width of about 70 mm, and a thickness of about 2 mm was obtained.
  • the plate material thus cast was subjected to the following processing heat treatment as follows. First, the cast plate was subjected to solution treatment at 440 ° C. for 1 hour. The solution treatment is to remove as much as possible the casting structure and segregation generated during casting before rolling, and to avoid defects caused by uneven grains or segregation during rolling.
  • plate material was preheated to 300 degreeC, and hot rolling was performed by the rolling roll heated to 200 degreeC.
  • Figure 3 is a photograph of the magnesium alloy sheet cast as described above after heat treatment at 440 °C for 1 hour to observe the microstructure of the specimen with an optical microscope.
  • Figure 4 is a photograph of the microstructure after the solution treatment for 30 minutes at 440 °C after rolling the magnesium alloy sheet prepared by the present invention with an optical microscope. As shown in FIG. 4, after the solution treatment after rolling, the average grain size of the microstructure is about 11 ⁇ m, and fine precipitated phases are evenly distributed throughout the microstructure.
  • 5 and 6 are photographs of the magnesium alloy plate produced by the present invention, respectively, and then rolled and subjected to a solution-treated microstructure with a transmission electron microscope.
  • the precipitated phase is formed differently according to the amount of Zn.
  • Zn When prepared by fixing Ca at 1% by weight and changing the Zn content to about 1, 4, 6% by weight, as shown in FIG. 5, when Zn is 1% by weight, Mg 2 Ca phase was formed, and Zn When the content of 6% by weight (4% by weight or more) can be seen in Figure 6 that the Mg 6 Zn 3 Ca 2 phase is formed.
  • FIG. 7 and 8 show the backscattering electron diffraction (EBSD) of the solution-treated microstructure after rolling 0.95 Zn, 0.9 Ca and 5.99 Zn, 0.98 Ca in the magnesium alloy sheet produced by the present invention, respectively.
  • EBSD backscattering electron diffraction
  • the method of manufacturing the magnesium alloy sheet according to the embodiment of the present invention can obtain a precipitated phase evenly dispersed in the microstructure by a simple process of the hot extrusion process compared with the conventional method.
  • the heat treatment temperature is set to be lower, which is an optimum temperature at which the precipitated phase is evenly distributed in each grain for each embodiment of the present invention, which is higher than the temperature.
  • the grain boundary is partially dissolved, and a large amount of precipitated phases are distributed in the grain boundary, thereby impairing room temperature tensile properties and formability.
  • FIG. 2 schematically illustrates a method for obtaining a selected limit dome height (LDH) value as an index for evaluating formability (particularly pressability) of a magnesium alloy sheet in an embodiment of the present invention.
  • a disk-shaped test piece having a diameter of 50 mm and a thickness of 0.7 mm was prepared, a test piece was inserted between the upper die and the lower die, and the specimen was fixed with a force of 5 kN, and lubricating oil was used as a known press oil. Then, a strain was applied at a speed of 0.1 mm / sec using a spherical punch having a diameter of 27.5 mm, the punch was inserted until the disc-shaped specimen was broken, and the deformation height at the fracture was measured.
  • the limit dome height test was carried out not only for the examples of the present invention but also for the magnesium alloy plates (AZ31 H24, ZW41) and aluminum plates (Al 5052) that are currently commercially available for comparison.
  • Table 2 shows the tensile and molding properties measured by the above method.
  • the magnesium alloy sheet produced according to the embodiment of the present invention exhibited an LDH of 6.6 to 8.8 mm.
  • the magnesium alloy prepared through the examples of the present invention not only shows three times or more excellent moldability as compared with the commercial AZ31 H24 alloy, but also has excellent moldability in the related art.
  • the ZW41 alloy known to represent it can be seen that the LDH is greatly improved in some examples.
  • the moldability is excellent in some embodiments.
  • FIGS. 9A and 9B show the results of analysis of a basal pole figure of a magnesium alloy sheet manufactured according to an embodiment of the present invention, respectively.
  • the pole plane of the basal plane becomes stronger during the rolling process, and the increase of the texture intensity results in a slip system. Less magnesium impairs formability.
  • the magnesium alloy sheet according to the embodiment of the present invention shows a low intensity (see FIG. 9A) of 3.8 in the case of the base surface even after rolling, and the heat treated alloy specimen exhibiting the highest LDH value.
  • the low intensity (see FIG. 9B) of case 2.0 is shown.
  • Table 3 it shows a low intensity (intensity) compared to the conventional magnesium plate.
  • Figure 10 shows the ratio of the base structure (0002) and the pyramid surface (10-11) texture of the alloy and the comparative example of the alloy, in the case of magnesium alloy sheet according to the present embodiment
  • the structure is relatively strong and has a lower value than that of the AZ31 alloy. This means that a random texture is formed in the magnesium alloy sheet according to the embodiment.
  • the magnesium alloy sheet according to the embodiment of the present invention has a considerably superior tensile strength compared to the same thin cast magnesium alloy sheet, and some examples of the magnesium alloy has a tensile strength of commercial AZ31 H24 A comparatively low degree is shown.
  • the magnesium alloy sheet according to the embodiment of the present invention may simultaneously control high formability and high mechanical properties so as to have mechanical properties comparable to those of aluminum, which is a lightweight metal, by heat treatment after rolling.
  • twin-roll thin plate casting method which is a method of manufacturing magnesium alloy sheet of the present invention, it is economical and provides a very fast cooling rate compared to the prior art, thereby making it possible to refine the particles. It can be improved.
  • the conventional magnesium alloy plate is relatively less strength than heat-treated aluminum, but the alloy plate according to the embodiment of the present invention can be applied to the automotive and structural materials industry that requires a high strength plate by implementing a relatively high strength.
  • due to the excellent moldability compared to the conventional magnesium can be used in a variety of fields that require a complex form of the plate is not applied to the conventional magnesium alloy plate.

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Abstract

La présente invention a pour but de proposer une feuille d'alliage de magnésium ayant une aptitude élevée au façonnage, dans laquelle du Ca est ajouté à un alliage à base de Mg et de Zn qui est un alliage durci par précipitation, et un procédé de coulée en bande mince à double rouleau et un procédé de traitement thermique ultérieur sont réalisés pour améliorer le comportement de précipitation, permettant ainsi à la feuille d'alliage de magnésium d'avoir une résistance supérieure et une faible anisotropie, et en particulier, une aptitude au façonnage à la presse qui est remarquablement améliorée par comparaison avec des feuilles d'alliage de magnésium classiques. Pour atteindre l'objectif, la feuille d'alliage de magnésium ayant une aptitude au façonnage élevée selon la présente invention comprend de 1 à 10 % en poids de Zn et de 0,1 à 5 % en poids de Ca, le reste étant constitué par les impuretés inévitables et le magnésium, la feuille d'alliage de magnésium ayant une hauteur limitante du dôme (LDH) de 7 mm ou plus.
PCT/KR2011/008991 2010-11-23 2011-11-23 Feuille d'alliage de magnésium ayant une aptitude supérieure au façonnage à la température ambiante et son procédé de fabrication Ceased WO2012070870A2 (fr)

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KR1020100116975A KR101303585B1 (ko) 2010-11-23 2010-11-23 상온성형성이 우수한 마그네슘 합금 판재 및 그 제조방법
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2014180187A1 (fr) * 2013-05-07 2014-11-13 宝山钢铁股份有限公司 Feuille d'alliage de magnésium ayant un coût faible, des grains fins, et une texture faible, et procédé de fabrication de celle-ci
JP2016516126A (ja) * 2013-05-07 2016-06-02 宝山鋼鉄股▲分▼有限公司 安価な細粒弱組織マグネシウム合金シートおよびそれを製造する方法
US10000836B2 (en) 2013-05-07 2018-06-19 Baoshan Iron & Steel Co., Ltd. Low-cost fine-grain weak-texture magnesium alloy sheet and method of manufacturing the same
CN109295365A (zh) * 2018-10-23 2019-02-01 西安卓恰医疗器械有限公司 一种可降解镁合金成型胚料，其制备设备，制备方法及由该成型胚料制备的加压螺钉
CN109295365B (zh) * 2018-10-23 2019-09-06 西安卓恰医疗器械有限公司 一种可降解镁合金成型胚料，其制备设备，制备方法及由该成型胚料制备的加压螺钉
CN113840939A (zh) * 2019-05-20 2021-12-24 大众汽车股份公司 具有高的可弯曲性的钣金产品及其制造
CN115044812A (zh) * 2022-06-17 2022-09-13 北京机科国创轻量化科学研究院有限公司 一种高延伸率微合金化改性az31镁合金薄板材料及其制备方法

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WO2012070870A3 (fr) 2012-08-23
EP2644728A2 (fr) 2013-10-02
KR20120055304A (ko) 2012-05-31
KR101303585B1 (ko) 2013-09-11
EP2644728A4 (fr) 2017-05-17

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