US20140373982A1 - Magnesium Alloy Sheet with Low Gd Content, High Ductility and the Hot Rolling Technology Thereof - Google Patents

Magnesium Alloy Sheet with Low Gd Content, High Ductility and the Hot Rolling Technology Thereof Download PDF

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Publication number
US20140373982A1
US20140373982A1 US14/375,717 US201314375717A US2014373982A1 US 20140373982 A1 US20140373982 A1 US 20140373982A1 US 201314375717 A US201314375717 A US 201314375717A US 2014373982 A1 US2014373982 A1 US 2014373982A1
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rolling
magnesium alloy
sheet
temperature
alloy
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Rongshi Chen
Hong Yan
Enhou Han
Wei Ke
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INSTITUTE OF METAL RESEARCH CHINESE ACADEMY OF SCIENCES
Institute of Metal Research of CAS
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INSTITUTE OF METAL RESEARCH CHINESE ACADEMY OF SCIENCES
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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
    • C22C—ALLOYS
    • C22C23/00—Alloys based on magnesium
    • 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 the field of metal material technology, and more especially, to a magnesium alloy sheet with low Gd content, high ductility and the hot rolling technology thereof.
  • magnesium alloy becomes more and more popular in the market.
  • die-cast magnesium alloy has been largely applied to various industrial areas, like automobile and 3C electronic product shell.
  • Subsequent surface treatment technologies of die-cast magnesium alloy are tedious, complex and easy to pollute environment, thus the industrial circle hopes to adopt stamping, press forging and other secondary processing methods which have higher productivity to form magnesium alloy sheets directly into automobiles and 3C electronic product shells.
  • magnesium alloy sheets One of the most economical and efficient methods of preparing magnesium alloy sheets is hot rolling, by which it is realizable, not only to produce wide sheets, but also to adjust grain size, structure and texture distribution through repeated rolling and heat treatment, thus achieving various specifications of sheets with excellent mechanical properties.
  • the existing commercial magnesium alloy sheets such as AZ31
  • those magnesium alloy sheets with weaker basal texture have higher strain hardening rate (index) under medium and low temperatures, thus ensuring the stability of plastic flow to achieve higher plasticity. Therefore, it is acceptable to enhance the forming performance of magnesium alloy by optimizing sheet texture, wherein the weaker the basal texture component of the texture is, the lower the sheet forming temperature will be and the better the forming performance will become too.
  • Texture weakening of magnesium alloy pertains to second phase, solid solution atoms and lattice constant change, etc., among which the solid solution atom is the key factor influencing the texture. Adding a small quantity of rare earth elements to magnesium alloy will randomize the orientation of dynamic recrystallized grains during deformation, thus forming non-basal texture. The texture adjustment by alloying trace quantities of rare earth has positive significance in developing magnesium alloy sheets with high plasticity.
  • phase equilibrium thermodynamics principle and phase diagram of magnesium alloy assume that structure containing fine second phase particles to be obtained by adding rare earth elements, such as Y, Nd and Gd, and magnesium alloy sheets with weak basal texture to be formed by annealing after rolling, so as to reduce sheets' anisotropy, high stress hardening index, tension-compression asymmetry, ensure plastic flow stability during secondary processing and enhance sheets' plasticity and secondary forming performance.
  • rare earth elements such as Y, Nd and Gd
  • magnesium alloy sheets with low anisotropy, weak texture, high stress hardening index and high plasticity by designing and optimizing Mg—RE alloy components, adopting traditional technologies like hot rolling and heat treatment to refine grains, obtain even structure and adjust texture according to the rules of the influence of rare earth elements over magnesium alloy structure, texture and performance becomes one of the research and development emphases in magnesium alloy material field.
  • roller heating technology is important for industrial continuous rolling of magnesium alloy sheets in the future, by which it is possible to ensure billet temperature during rolling, realize multi-pass continuous rolling, reduce annealing times and improve production efficiency.
  • Research shows that roller has the least influence upon the final structure, texture and mechanical properties of the sheets of the present invention when under a heating temperature of 25-400° C., which can ensure the characteristics of the sheets of the present invention.
  • this invention application hopes to prepare a magnesium alloy sheet with non-basal texture and high ductility under room temperature via common rolling and heat treatment technologies by utilizing the unique effect of rare earth elements in magnesium alloy.
  • Al and Zn are main alloying elements in magnesium alloy, but due to Al's strong adhesion to rare earth, Al—RE phase will be easily formed, which reduces the content of solid solution rare earth atoms in the matrix, thus presenting unobvious adjustment effect; so, select Zn as the second alloying element in addition to rare earth.
  • Mn can not only enhance alloy corrosion resistance, but also inhibit the growth of crystallized grains, besides, will not affect texture adjustment effect, for which an appropriate amount of Mn must be added to alloy.
  • Xi'an Jiaotong University reported an in-situ synthesized quasicrystal phase-reinforced high-strength magnesium alloy (publication number: CN1789458A), with the component and weight percentages being: Zn of 3-10%, Y of 0.5-3.5%, Ce of 1% and Nd of 0-1%, wherein after rapid solidification and reciprocating large plastic extrusion, the tensile strength under room temperature is no less than 500 MPa; the elongation is no less than 20%.
  • the contents of Zn in alloys are both no less than 3%, or even reach 10%.
  • the increase of Zn content may form second phase with low melting point in the matrix, which not only leads to hot cracking during casting, but also cause poor rolling performance of magnesium alloy, narrow rolling temperature interval and small single-pass rolling deformation amount (less than 20% generally), thus the product productivity and yield are low.
  • the processing method of three-dimensional compressive stress such as extrusion, which is not suitable for producing wide sheets, so the two patents adopt “extrusion process” and “rapid solidification+extrusion process” respectively.
  • materials of the two inventions have good strength, but with the plasticity being around 20%, they cannot meet the performance requirement for room temperature forming of magnesium alloy sheets.
  • products of the two patents are indeed not appropriate for being sheet products with high ductility.
  • Zn takes up no more than 2.1%, and the alloy has good rolling performance, with which single-pass rolling reduction can reach 50% or even more, so it is acceptable to produce wide magnesium alloy sheets efficiently in a short process via ordinary rolling method.
  • the room-temperature elongation of extruded materials is no more than 20%.
  • the patent takes Ce whose solid solubility is quite small to generate second phase at grain boundary and refine grains, so as to enhance strength. Since Ce does not weaken the texture of magnesium alloy, the enhancement of magnesium alloy plasticity will be unobvious.
  • Gd with the solid solubility being 23.49wt % in magnesium is adopted and the weakening effect of Gd solid solution atoms Gd upon the texture of magnesium alloy is utilized, so as to enhance alloy rolling performance and change the grain orientation of magnesium alloy sheets after rolling to obtain non-basal texture, thus improving room-temperature plasticity and forming performance of rolled sheets.
  • Gd is found to work better than Y, so it is selected from RE as alloying element, and at the same time, it is hoped to minimize Gd content on the basis of ensuring Gd's weakening of rolled sheet texture and enhancement of the room-temperature forming performance, thus reducing the costs of the alloy and sheet products of the original patent.
  • the present invention defines the scope of the lowest effective content of Gd for non-basal texture, which greatly reduces alloy costs and can meet the requirement of civil products-used magnesium alloy for low cost, and meanwhile, re-designs and re-optimizes the chemical components of Mg—Zn—Gd (—Mn) alloy based on Mn's favourable role in enhancing magnesium alloy corrosion resistance and inhibiting grain growth and on the premise of not affecting Gd's ability of texture weakening, which is an effective improvement and optimization of the previous patent of the applicant.
  • the present invention provides a new magnesium alloy sheet with low Gd content, high ductility, good room-temperature ductility and forming performance as well as its hot rolling technology, whose principle is to fully utilize the weakening effect of trace quantities of Gd solid solution atom upon magnesium alloy texture during rolling to determine the lowest effective content of Gd for texture weakening and thus reduce alloy costs.
  • the prepared magnesium alloy sheets have non-basal texture with the room-temperature elongation being 35 ⁇ 50%, wherein the elongation in the rolling direction is no less than 35% and that in the horizontal direction no less than 45%.
  • a magnesium alloy sheet with low Gd content and high ductility wherein the magnesium alloy belongs to Mg—Zn—Gd series and calculated as per mass percent, with chemical components: 0.9 ⁇ 2.1% as Zn, 0.2 ⁇ 0.8% as rare earth, Gd, 0 ⁇ 0.9% as Mn and the balance amount as Mg.
  • the hot rolling technology of the above-mentioned magnesium alloy sheet with low Gd content and high ductility includes the following steps:
  • Hot rolling of ingots Rolling temperature: 250 ⁇ 525° C. (roller preheating temperature: room temperature to 400° C.); rolling reduction of each pass: 35 ⁇ 50%; return the ingots back to the furnace every time after rolling of 1 ⁇ 5 passes, heat them up to the rolling temperature and keep the temperature for 10 ⁇ 60 minutes before further rolling, with the total rolling reduction being 80 ⁇ 95%;
  • Annealing of rolled sheets the rolled sheets are annealed for 0.5 ⁇ 120 hours under 250 ⁇ 500° C.
  • the content of rare earth, Gd is very low, only 0.2-0.8%, which reduces alloy costs on the basis of ensuring texture weakening and room-temperature plasticity, and excludes costly Zr, thus enabling enterprises to accept the alloy costs.
  • the alloy has good rolling performance and the rolling deformation amount of each pass can reach 50% or above, which reduces the frequency and time of reheating during rolling, shortens the technological process and enhances the productivity, thus achieving high product yield and reducing the total costs of products; it is acceptable to adopt the existing rolling equipment and technology, featuring simple technology and easy control, for industrial continuous production.
  • the sheet technically prepared for the present invention has non-basal texture, low anisotropy and high strain hardening rate with the room-temperature elongation being 35 ⁇ 50%, which can realize room-temperature secondary forming of sheets, reduce costs of secondary plastic forming and enhance productivity, for which the sheet will be extensively applied to fields like electronic product shell and automobile.
  • the alloy of the present invention not only applies to rolled sheets, but also can be popularized and applied to the production of profiles, tubes and pipes, free forgings and die forgings.
  • FIG. 1 (a)-(b) are the microphotographs of the rolled sheet of magnesium alloy; wherein: (a) refers to the Mg-2.0Zn-0.2Gd-0.8Mn alloy of Example 1; (b) refers to the Mg-1.8Zn-0.4Gd alloy of Example 2; (c) refers to the Mg-3.1Zn-0.9Gd alloy of Comparative Example 2; (d) refers to the Mg-1.2Zn-4.9Gd alloy of Comparative Example 3.
  • FIG. 2 (a)-(d) are the structures of the rolled sheet of magnesium alloy; wherein: (a) refers to the Mg-2.0Zn-0.2Gd-0.8Mn alloy of Example 1; (b) refers to the Mg-1.8Zn-0.4Gd alloy of Example 2; (c) refers to the Mg-1.9Zn-0.6Gd alloy of Example 3; (d) refers to the Mg-0.9Zn-0.7Gd-0.6Mn alloy of Example 4; (e) refers to the Mg-1.8Zn-0.1Gd alloy of Comparative Example 1.
  • FIG. 3 (a)-(d) are the structures of the rolled sheet of magnesium alloy annealed under different temperatures; wherein, (a) shows the Mg-2.0Zn-0.2Gd-0.8Mn sheet annealed for 2 hours under 250° C. of Example 1; (b) shows the Mg-1.8Zn-0.4Gd sheet annealed for 3 hours under 325° C. of Example 2; (c) shows the Mg-1.9Zn-0.6Gd sheet annealed for 1 hour under 350° C. of Example 3; (d) shows the Mg-0.9Zn-0.7Gd-0.6Mn sheet annealed for 0.5 hours under 400° C. of Example 4; (e) shows the Mg-1.8Zn-0.1Gd alloy sheet annealed for 1 hour under 400° C. of Comparative Example 1.
  • FIG. 4 shows the basal (0002) structures of the rolled sheet after annealing; wherein, (a) shows the Mg-2.0Zn-0.2Gd-0.8Mn sheet annealed for 2 hours under 250° C. of Example 1 (texture strength levels: 1.07, 1.23, 1.41, 1.62, 1.86, 2.14, 2.46 and 2.82); (b) shows the Mg-1.8Zn-0.4Gd sheet annealed for 3 hours under 325° C. of Example 2 (texture strength levels: 1.08, 1.26, 1.47, 1.71, 1.86, 2.14, 2.46 and 2.82); (c) shows the Mg-1.9Zn-0.6Gd sheet annealed for 1 hour under 350° C.
  • Example 3 texture strength levels: 1.09, 1.28, 1.50, 1.77, 2.08, 2.45, 2.89 and 3.40; (d) shows the Mg-0.9Zn-0.7Gd-0.6Mn sheet annealed for 0.5 hours under 400° C. of Example 4 (texture strength levels: 1.08, 1.27, 1.48, 1.74, 2.03, 2.38, 2.79 and 3.27); (e) shows the Mg-1.8Zn-0.1Gd alloy sheet annealed for 1 hour under 400° C. of Comparative Example 1 (texture strength levels: 1.1, 2.0, 3.3, 5.0, 6.9, 8.5, 10.1 and 12.4).
  • FIG. 5 shows the tensile stress-strain curves of the rolled sheet after annealing; wherein, (a) shows the Mg-2.0Zn-0.2Gd-0.8Mn sheet annealed for 2 hours under 250° C. of Example 1; (b) shows the Mg-1.8Zn-0.4Gd sheet annealed for 3 hours under 325° C. of Example 2; (c) shows the Mg-1.9Zn-0.6Gd sheet annealed for 1 hour under 305° C. of Example 3; (d) shows the Mg-0.9Zn-0.7Gd-0.6Mn sheet annealed for 0.5 hours under 400° C. of Example 4; (e) shows the Mg-1.8Zn-0.1Gd alloy sheet annealed for 1 hour under 400° C. of Comparative Example 1.
  • Table 1 shows the chemical composition of the Mg—Zn—Gd alloys of examples 1-4 of the present invention (the data herein are the results of chemical analysis and based on mass percent), wherein the formulas are only partial components within the protective scope.
  • Table 2 shows the chemical composition of the Mg—Zn—Gd alloys of comparative examples 1-3 (based on mass percent).
  • the rolled sheet achieves more even equiaxed grain structure, see (a) of FIG. 3 .
  • the annealed sheet has non-basal texture and presents a double peak texture deviating by ⁇ 40 ⁇ laterally, as shown in (a) of FIG. 4 , which contributes to enhancing sheet plasticity.
  • the rolled sheet After 3 hours of annealing under 320° C., the rolled sheet exhibits static recrystallization and achieves evener structure, see (b) of FIG. 3 .
  • the annealed sheet has non-basal texture and presents a double peak texture deviating by 40° laterally, as shown in (b) of FIG. 4 , which contributes to enhancing sheet plasticity.
  • the rolled sheet is annealed after 1 hour of heat insulation under 350° C., with obvious static recrystallization generated and even equiaxed grain structure obtained, see (c) of FIG. 3 .
  • the annealed sheet has non-basal texture and presents a double peak texture deviating by ⁇ 40 ⁇ laterally, as shown in (c) of FIG. 4 , which contributes to enhancing sheet plasticity;
  • the rolled sheet is annealed after 0.5 hours of heat insulation under 400° C., with evener equiaxed grain structure obtained, see (d) of FIG. 3 .
  • the annealed sheet has non-basal texture and presents a double peak texture deviating by ⁇ 40 ⁇ laterally, as shown in (d) of FIG. 4 , which contributes to enhancing sheet plasticity.
  • the roller temperature is 25° C.; the rolling reduction of the first pass is 30%, afterwards, the rolling reduction of each pass is 30-45%; return the ingot back to the furnace every time after rolling of 1 pass and keep the temperature for 5 ⁇ 10 minutes before further rolling, until the sheet has a width of 2 mm and a total rolling reduction of 85%, wherein, the edges and surface of the sheet have no cracks; in addition, dynamic recrystallization occurs in the course of rolling and the sheet has bigger grain size than the alloys of other numbers, see (e) of FIG. 2 ;

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PCT/CN2013/080696 WO2014075466A1 (zh) 2012-11-15 2013-08-02 一种低Gd含量、高延展性镁合金板材及其热轧制工艺

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