US20200056270A1 - Highly molded magnesium alloy sheet and method for manufacturing same - Google Patents

Highly molded magnesium alloy sheet and method for manufacturing same Download PDF

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Publication number
US20200056270A1
US20200056270A1 US16/343,918 US201716343918A US2020056270A1 US 20200056270 A1 US20200056270 A1 US 20200056270A1 US 201716343918 A US201716343918 A US 201716343918A US 2020056270 A1 US2020056270 A1 US 2020056270A1
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Prior art keywords
magnesium alloy
alloy sheet
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excluding
cast material
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English (en)
Inventor
Sang Hyun Kim
Oh-Duck Kwon
Jae Joong Kim
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Posco Holdings Inc
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Posco Co Ltd
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Assigned to POSCO reassignment POSCO ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: KIM, JAE JOONG, KIM, SANG HYUN, KWON, OH-DUCK
Publication of US20200056270A1 publication Critical patent/US20200056270A1/en
Abandoned 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
    • C22C23/04—Alloys based on magnesium with zinc or cadmium as the next major constituent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
    • B21B1/46—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling metal immediately subsequent to continuous casting
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
    • B21B1/46—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling metal immediately subsequent to continuous casting
    • B21B1/463—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling metal immediately subsequent to continuous casting in a continuous process, i.e. the cast not being cut before rolling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B3/00—Rolling materials of special alloys so far as the composition of the alloy requires or permits special rolling methods or sequences ; Rolling of aluminium, copper, zinc or other non-ferrous metals
    • B21B3/003—Rolling non-ferrous metals immediately subsequent to continuous casting, i.e. in-line rolling
    • 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-formed magnesium alloy sheet and a method of manufacturing the same.
  • the density of magnesium is 1.74 g/cm 3 , which is the lightest metal among the structural metals including aluminum and steel. In addition, it is a metal that is attracting attention in mobile and IT fields because of its excellent vibration absorbing ability and electromagnetic wave shielding ability. In addition, in the automobile field, studies are being actively carried out in advanced countries including Europe to reduce the weight of the vehicle body due to the regulation of fuel economy and performance, and magnesium is being reported as a substitute metal. However, since magnesium is expensive compared to competitive materials such as aluminum and stainless steel, its application to magnesium is limited to only some parts that are required to be lightweight.
  • magnesium is difficult to form at room temperature due to hexagonal close packing (HCP). Since the warm forming process is essential for the application of the product, the investment cost of the mold/heating device for the warm forming becomes large. In addition, it is deteriorated the productivity due to sticking, scratching between the mold and the material, and delay time for heating. Therefore, not only the price of the magnesium material, but also the processing cost of the magnesium alloy is more expensive than the competitive material.
  • HCP hexagonal close packing
  • An embodiment of the present invention is to provide a high-formed magnesium alloy sheet and a method of manufacturing the same by controlling the composition range of the Zn, Ca, and Mn components of the magnesium alloy sheet and the relationship of the components.
  • the present invention provides a magnesium alloy sheet excellent in moldability by controlling the Mg—Ca based secondary phase through the composition of the alloy and the manufacturing conditions.
  • a magnesium alloy sheet of one embodiment of the invention may include 3.0 wt % or less (excluding 0 wt %) of Zn, 1.5 wt % or less (excluding 0 wt %) of Ca, 1.0 wt % or less (excluding 0 wt %) of Mn, balance of Mg and inevitable impurities, for a total of 100 wt %, wherein, the magnesium alloy sheet further comprises 0.3 wt % or less of Al, based on 100 wt % of the entire magnesium alloy sheet.
  • the magnesium alloy sheet may satisfy the following formulas (1) and (2):
  • a maximum texture intensity based on the ⁇ 0001 ⁇ plane of the magnesium alloy sheet may be 1 to 4.
  • the magnesium alloy sheet can have 7 to 10 mm of Limit Dome Height (LDH).
  • LDH Limit Dome Height
  • the magnesium alloy sheet may include crystal grain having an average particle size of 1 to 20 ⁇ m.
  • the magnesium alloy sheet may include a Mg—Ca based secondary phase, and the average particle size of the secondary phase is 30 ⁇ m or less.
  • the magnesium alloy sheet can include 1 to 20 secondary phases per 100 ⁇ m 2 of the magnesium alloy sheet area.
  • a method of manufacturing a magnesium alloy sheet of one embodiment of the invention may include: preparing a cast material by casting a molten alloy comprising 3.0 wt % or less (excluding 0 wt %) of Zn, 1.5 wt % or less (excluding 0 wt %) of Ca, 1.0 wt % or less (excluding 0 wt %) of Mn, balance of Mg and inevitable impurities, for a total of 100 wt %; subjecting the cast material to homogenizing heat treatment: preparing a rolled material by subjecting the homogenizing heat treated cast material to hot rolling; and final annealing the rolled material.
  • the molten alloy can further include 0.3 wt % or less of Al, based on 100 wt % of the entire molten alloy, and the magnesium alloy sheet satisfies the following formulas (1) and (2).
  • a temperature range may be from 200 to 500° C.
  • the step of the final annealing the rolled material may be conducted for less than 5 hours (excluding 0 hours).
  • the composition range of the Zn, Ca, and Mn components of the magnesium alloy sheet and the relationship of the above components can be controlled to provide a magnesium alloy sheet of high molding.
  • FIG. 1 is a photograph of the microstructure of the magnesium alloy sheet of Example 2 and Comparative Example 2 observed with an optical microscope.
  • FIG. 2 shows the results of analysis of the secondary phase components of Example 2 and Comparative Example 2 by SEM-EDS.
  • FIG. 3 shows the results of analysis of the ⁇ 0001 ⁇ planes of Example 2 and Comparative Example 3 by the XRD pole diagram and EBSD.
  • One embodiment of the present invention provides a magnesium alloy sheet including: 3.0 wt % or less (excluding 0 wt %) of Zn, 1.5 wt % or less (excluding 0 wt %) of Ca, 1.0 wt % or less (excluding 0 wt %) of Mn, balance of Mg and inevitable impurities, for a total of 100 wt %.
  • the magnesium alloy sheet can further include 0.3 wt % or less of Al, based on 100 wt % of the entire magnesium alloy sheet.
  • composition range of the aluminum component may be such that it is added at an impurity level as compared with essential additive elements such as zinc, calcium, and manganese in the magnesium alloy sheet according to one embodiment of the present invention.
  • Zn may include 3.0 wt % or less, but 0 wt % is excluded.
  • Zn may be 0.5 to 3.0 wt %.
  • Ca may contain up to 1.5% by weight, but excluding 0% by weight.
  • Ca may be 0.1 to 1.5% by weight.
  • calcium like zinc
  • twin crystal phase may be segregated in grain boundaries and twin crystal phase to contribute to the production and growth of non-bottom recrystallized grains.
  • softening phenomenon of the non-bottom surface is brought about, and the slip of the non-bottom surface is activated to improve the formability of the sheet. Therefore, when it is added in an amount of less than 0.1% by weight, it is difficult to secure moldability.
  • Mn may include not more than 1.0 wt %, but not 0 wt %.
  • manganese acts as a recrystallization nucleation site to generate fine grains, and then to suppress grain growth, thereby providing fine and uniform grains. Therefore, in the method of manufacturing a magnesium alloy sheet, which is another embodiment of the present invention described later, it is possible to provide fine crystal grains in the homogenizing heat treatment step, and finely control the crystal grains of the final magnesium alloy sheet.
  • the crystal grains of the homogenizing heat treated sheet are finely formed, and defects such as abnormal crystal growth in the hot rolling step, orange peel due to shear band and surface cracks can be prevented. Therefore, the rolling property can be improved.
  • impurities such as iron (Fe) and silicon (Si) can be controlled to provide excellent corrosion resistance.
  • a sheet having fine crystal grains can be produced through addition of manganese, so that both the strength and the formability can be excellent.
  • the magnesium alloy sheet satisfies the following formulas (1) and (2).
  • the formula (1) may be 3 or less.
  • the magnesium alloy sheet can satisfy the formula (2) ([Zn]+[Ca]>[Mn]).
  • the sum of the Zn and Ca composition is equal to or smaller than the composition of Mn, the rolling property and the formability may be deteriorated.
  • the magnesium alloy sheet satisfying the above-described components and composition ranges may include a Mg—Ca based secondary phase.
  • the average particle size of the secondary phase may be 30 ⁇ m or less. Specifically, it may be 25 ⁇ m or less. Specifically, it may be 20 ⁇ m or less.
  • the average particle size in this specification means the average diameter of the spherical substance present in the unit of measurement. If the material is a non-spherical material, it can be calculated by approximating the non-spherical material to the spherical shape.
  • the range of the secondary phase size is significantly smaller than that of the secondary phase of the general magnesium alloy sheet.
  • the moldability of the alloy material may be lowered.
  • the magnesium alloy sheet can include 1 to 20 secondary phases per 100 ⁇ m 2 of the magnesium alloy sheet area.
  • the strength and moldability of the magnesium alloy sheet can be excellent.
  • the magnesium alloy sheet may include crystal grains having an average particle diameter of 1 to 20 ⁇ m.
  • the crystal grain size of the magnesium alloy sheet is in the above range. More specifically, when the grain size of the magnesium alloy sheet is in the above range, the strength can be excellent.
  • the maximum texture intensity based on the ⁇ 0001 ⁇ plane of the magnesium alloy sheet may be 1 to 4.
  • the texture intensity of the magnesium alloy sheet is in the above range, crystal grains of various orientations can be distributed. Accordingly, since the fraction of the bottom grain ( ⁇ 0001>//C-axis orientation) is small, a magnesium alloy sheet having excellent formability can be provided.
  • the bottom crystal grain means a crystal grain having a bottom orientation.
  • magnesium has an HCP (Hexagonal Closed Pack) crystal structure.
  • HCP Hexagonal Closed Pack
  • the crystal grains is referred to as crystal grains having a bottom crystal orientation (that is, bottom crystal grains). Therefore, in the present specification, the bottom grain can also be expressed as “ ⁇ 0001>//C axis”.
  • the magnesium alloy sheet according to an embodiment of the present invention has a texture intensity of 1 to 4 based on the ⁇ 0001 ⁇ plane, so that the moldability can be excellent.
  • the Erichsen value of the magnesium alloy sheet at room temperature may be 7 to 10 mm.
  • the Erichsen value means an experimental value derived from the Ericsson test at room temperature. More specifically, the Erichsen value refers to the height at which the sheet is deformed until a fracture occurs, when the sheet is deformed into a cup shape.
  • the room temperature moldability can be compared through the Erichsen value.
  • the yield strength of the magnesium alloy sheet may be 170 MPa or more. Specifically, it may be 170 to 220 MPa.
  • the tensile strength of the magnesium alloy sheet may be 240 MPa or more. Specifically, it may be 240 to 300 MPa.
  • the elongation of the magnesium alloy sheet may be 20% or more. Specifically, it may be 20 to 30%.
  • the present invention is not limited thereto.
  • the yield strength, the tensile strength, and the elongation are preferably as good as possible, and the magnesium alloy sheet according to one embodiment of the present invention can realize mechanical properties at least the minimum value.
  • the strength and elongation of the magnesium alloy sheet according to one embodiment of the present invention are excellent in strength and elongation as compared with the conventional case in which an additional element is added to the AZ-based magnesium alloy.
  • a method of manufacturing a magnesium alloy sheet of one embodiment of the invention may include: preparing a cast material by casting a molten alloy comprising 3.0 wt % or less (excluding 0 wt %) of Zn, 1.5 wt % or less (excluding 0 wt %) of Ca, 1.0 wt % or less (excluding 0 wt %) of Mn, balance of Mg and inevitable impurities, for a total of 100 wt % (S10); subjecting the cast material to homogenizing heat treatment (S20); preparing a rolled material by subjecting the homogenizing heat treated cast material to hot rolling (S30); and final annealing the rolled material (S40).
  • a step of preparing a cast material by casting a molten alloy comprising 3.0 wt % or less (excluding 0 wt %) of Zn, 1.5 wt % or less (excluding 0 wt %) of Ca, 1.0 wt % or less (excluding 0 wt %) of Mn, balance of Mg and inevitable impurities, for a total of 100 wt % (S10) can be performed.
  • the magnesium molten alloy can satisfy the following formulas (1) and (2).
  • the reason for limiting the component and the composition range of the molten alloy is the same as the reason for limiting the component and the composition range of the magnesium alloy sheet described above, so that the description is omitted.
  • the molten alloy can be cast by gravity casting, continuous casting, strip casting (thin sheet casting), sand casting, vacuum casting, centrifugal casting, die casting, or thixo molding.
  • the present invention is not limited thereto, and any method capable of producing a cast material is possible.
  • step (S20) of subjecting the cast material to homogenizing heat treatment can be performed.
  • overheating can be prevented by homogenizing the cast material in the temperature and time range, and the microstructure and segregation of the cast material can be sufficiently homogenizing heated.
  • step (S30) of preparing a rolled material by subjecting the homogenizing heat treated cast material to hot rolling may be performed.
  • hot rolling can be performed in a temperature range of 150 to 400° C.
  • the cast material may be hot rolled once or twice at a reduction ratio of not more than 40% (excluding 0%) per rolling.
  • the homogenizing heat treated cast material can be hot rolled by using a hot rolling mill.
  • an intermediate annealing may be performed at least once between hot rolling.
  • the intermediate annealing may be performed at a temperature range of 300 to 500° C.
  • the intermediate annealing may be performed for 5 hours or less (excluding 0 hours).
  • the stress of the hardened tissue is not sufficiently solved by the cumulative rolling reduction, and the annealing process may not be performed properly. Further, the abnormal crystal grains can grow due to excessive annealing.
  • the thickness of the rolled material that is hot-rolled at least twice may be 2.0 mm or less.
  • step (S40) of final annealing the rolled material can be carried out.
  • the magnesium alloy sheet produced can secure the desired formability at room temperature.
  • an alloyed molten metal of an inventive material and a comparative material was cast to produce a cast material.
  • the cast material was subjected to homogenizing heat treatment at 330 to 450° C. for 16 hours.
  • the homogenizing heat treated cast material was rolled at 300° C. at a reduction ratio of 10 to 20% to prepare a rolled material. At this time, intermediate annealing was performed at 450° C. for 0.5 to 1 hour.
  • Table 2 shows mechanical properties of the magnesium alloy sheet according to Examples and Comparative Examples and Erichsen's values at room temperature.
  • the Ericsson values measurement method is as follows.
  • a magnesium alloy sheet having a size of 50 to 60 mm in each of the width and the length was used, and a lubricant was used on the surface of the sheet to reduce the friction between the sheet and the spherical punch.
  • the temperature of the die and the spherical punch was set at room temperature.
  • the outer peripheral portion of the sheet was fixed with a force of 10 kN. Thereafter, the sheet was deformed at a rate of 5 mm/min using a spherical punch having a diameter of 20 mm. Thereafter, the punch was inserted until the sheet was broken, and then the deformation height of the sheet was measured at the time of breaking.
  • the deformation height of the plate measured in this way is called the Erichsen value or the limit dome height (LDH).
  • Examples 1 to 3 have a much higher Erichsen value than the Comparative Examples.
  • the present example has a yield strength of 170 MPa or more, a tensile strength of 240 MPa or more, an elongation of 20% or more, and a room temperature Erichsen value of 7 mm or more.
  • the comparative examples which satisfy the range of the composition of Zn, Ca, and Mn according to one embodiment of the present invention, but do not satisfy both the formula [Zn]+[Ca]>[Mn] and the formula [Zn]/[Ca] ⁇ 4.0, can be confirmed that there is an effect of heating strength and formability.
  • FIG. 1 is a photograph of the microstructure of the magnesium alloy shee of Example 2 and Comparative Example 2 observed with an optical microscope.
  • Example 2 As a result, comparing the microstructures of Example 2 and Comparative Example 2 in which the final annealing conditions were the same and the components of the alloy were different, the secondary phase in the form of agglomerated black in Comparative Example 2 is more than Example 2. It can be seen with the naked eye.
  • the coarse secondary phase adversely affects the moldability.
  • FIG. 2 shows the results of analysis of the secondary phase components of Example 2 and Comparative Example 2 by SEM-EDS.
  • a peak may appear at a value corresponding to the energy of the material.
  • component analysis can be derived from the wavelengths shown.
  • a secondary phase (dark gray spherical shape) is finely dispersed in an EDS (Energy Dispersive Spectroscopy) photograph of a scanning electron microscope (SEM) of Example 2.
  • EDS Electronic Dispersive Spectroscopy
  • SEM scanning electron microscope
  • Example 2 as a result of the content ratio of Zn and Ca and the content ratio of Zn/Ca satisfying all the ranges defined in the embodiment of the present invention, it was also confirmed that the formation of the secondary phase of the Mg—Ca two-atom system is more easy than the secondary phase of Ca—Mg—Zn three-atom system.
  • the secondary phase of Comparative Example 2 in which the Zn content is excessive is larger than that of the secondary phase of Example 2.
  • Example 2 of the present application the Ma-Ca based secondary phase is finely dispersed and distributed at a level of 20 ⁇ m or less, thereby contributing to improvement of the strength and moldability of the magnesium alloy sheet.
  • FIG. 3 shows the results of analysis of the ⁇ 0001 ⁇ planes of Example 2 and Comparative Example 3 by the XRD pole diagram and EBSD.
  • FIG. 3 shows the texture according to the crystal orientation of the crystal grains by using the XRD pole figure method and EBSD (Electron Backscatter Diffraction) method.
  • the EBSD can inject electrons into the specimen through the e-electron beam and measure the crystal orientation of the grains using inelastic scattering diffraction at the back of the specimen.
  • the pole figure is a stereo projection of the direction of the arbitrarily fixed crystal coordinate system in the specimen coordinate system. More specifically, the poles for the ⁇ 0001 ⁇ planes of the crystal grains of various orientations can be displayed in the reference coordinate system, and the poles can be represented by plotting density contours according to the poles density distribution. At this time, the poles are fixed in a specific lattice direction by the Bragg angle, and a plurality of poles can be displayed for a single crystal.
  • the numerical representation of the density distribution values of the contour lines indicated by the poling method can be referred to as the texture intensity for the ⁇ 0001 ⁇ plane.
  • the grain size of the grain in Example 2 is as fine as 1 to 20 ⁇ m as compared with that of Comparative Example 3.
  • Example 2 the maximum texture intensity of the ⁇ 0001 ⁇ plane of Example 2 was 2.46. It is significantly lower than that of Comparative Example 3 with a maximum texture intensity of 12.11. From this, it can be interpreted that the crystal grains of various orientations are distributed in Example 2 of the present invention, whereas the crystal grains (bottom crystal grains) of the ⁇ 0001>//C axis orientation are distributed much in Comparative Example 3.
  • the embodiment has better moldability because the fraction of the bottom surface crystal grain is smaller than that of the comparative example.

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  • Organic Chemistry (AREA)
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  • Crystallography & Structural Chemistry (AREA)
  • Heat Treatment Of Sheet Steel (AREA)
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  • Shaping Metal By Deep-Drawing, Or The Like (AREA)
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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
CN115074563A (zh) * 2022-06-29 2022-09-20 华南理工大学 一种高强韧低合金含量Mg-Zn-Ca合金及其制备方法

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KR101889019B1 (ko) * 2016-12-23 2018-08-20 주식회사 포스코 마그네슘 합금판, 및 그 제조방법
JP7248252B2 (ja) * 2019-03-29 2023-03-29 国立研究開発法人産業技術総合研究所 強度－延性バランスと常温加工性に優れたマグネシウム合金板
CN110819920B (zh) * 2019-11-22 2020-12-29 中国兵器工业第五九研究所 一种低成本高强韧镁合金时效强韧化方法
WO2021215241A1 (ja) * 2020-04-21 2021-10-28 国立研究開発法人産業技術総合研究所 マグネシウム合金、マグネシウム合金板、マグネシウム合金棒およびこれらの製造方法、マグネシウム合金部材

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JP4306547B2 (ja) * 2004-06-30 2009-08-05 住友電気工業株式会社 マグネシウム合金板及びその製造方法
JP5035893B2 (ja) * 2006-09-01 2012-09-26 独立行政法人産業技術総合研究所 高強度高延性難燃性マグネシウム合金及びその製造方法
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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
CN115074563A (zh) * 2022-06-29 2022-09-20 华南理工大学 一种高强韧低合金含量Mg-Zn-Ca合金及其制备方法

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CN109844152A (zh) 2019-06-04
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