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Kun Yang, Hucheng Pan, Sen Du, Man Li, Jingren Li, Hongbo Xie, Qiuyan Huang, Huajun Mo, and Gaowu Qin, Low-cost and high-strength Mg−Al−Ca−Zn−Mn wrought alloy with balanced ductility, Int. J. Miner. Metall. Mater., 29(2022), No. 7, pp.1396-1405. https://dx.doi.org/10.1007/s12613-021-2395-y
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Magnesium alloy, as the lightest metallic structural material [1–2], has great potential to be used in vehicles, airplanes, and aerospace [3–6]. In the past decades, an obvious improvement in the mechanical properties has been made in rare-earth (RE)-containing Mg-based alloys [7]. Both ultra-high yield strength (YS) above 400 MPa and a high ductility larger than 5% can be obtained in Mg–Gd [8], Mg–Y [9], and Mg–Gd–Y based alloy systems [10–11]. For example, Homma et al. [12] reported that a high YS of ~473 MPa, ultimate strength (UTS) of 542 MPa, and elongation (EL) of ~8% can be achieved in the extruded and the subsequently aged Mg–10Gd–6Y–1.6Zn–0.6Zr (wt%) alloy. However, the cost of Mg–RE-based alloys would be largely increased due to the high amounts of expensive RE elements. Moreover, the processing difficulty for these heavily-alloyed Mg–RE-based alloys would also be increased, further hindering their practical applications. In this sense, the development of novel RE-free and high-strength Mg wrought alloys would be much attractive in the viewpoints of low-cost and resource-saving [13–15].
Fortunately, Ca, as one of the non-RE elements, was proved to be effective in enhancing the mechanical property of Mg-based alloys due to its similar chemical properties and atomic size with those of the RE elements [16]. For example, Ikeo et al. [17] produced an Mg–0.3Ca (wt%) alloy by conventional extrusion. Recrystallized grains as fine as only ~0.5 μm were achieved, and a high YS of ~400 MPa has been obtained. Our previous works also proved that an ultra-high YS of ~443 MPa can be further obtained in the as-extruded Mg–2Ca–2Sn (wt%) alloy, which can be ascribed to the surprising grain refinement of the α-Mg matrix down to only ~0.32 μm [18]. Despite that, previously reported Mg–Ca-based alloys are usually brittle, usually <2% in elongation, when the strength is raised to be larger than 350 MPa [19]. In this context, multi-elements of Al, Zn, and/or Mn have been added into the Mg–Ca-based sample to realize higher strength–ductility synergy [20]. For example, Jiang et al. [21] studied the role of Al addition in modifying the microstructure of Mg–Ca based alloys and found that the strength and ductility of Mg–2.32Al–1.7Ca alloy can be greatly improved after extrusion, with a YS, UTS, and EL of 275 MPa, 324 MPa, and 10.2%, respectively. Nakata et al. [22] have developed a wrought magnesium alloy, Mg–1.3Al–0.3Ca–0.4Mn (wt%) alloy, which can exhibit a good combination of strength and elongation, with a YS of ~287 MPa and EL of ~20%. Zeng et al. [23] further reported that the as-extruded Mg–3Al–1Zn–0.3Mn–0.5Ca sample can exhibit a high YS of ~420 MPa and an EL of 5.1%, simultaneously. The results above confirmed the beneficial effects of Al, Zn, and Mn atoms in improving the mechanical properties of Mg–Ca-based alloys.
In this work, the compositions and processing parameters of Mg–Ca-based alloys were further optimized. An excellent combination of strength and elongation was achieved in the as-extruded Mg–1.3Al–1.2Ca–0.5Zn–0.6Mn (wt%) alloy. The mechanism for high strength-ductility synergy was also discussed.
Mg billets were produced by electronic induction melting method with raw materials of pure Mg (99.99wt%), pure Ca (99.99wt%), pure Zn (99.99wt%), pure Al (99.99wt%), and Mg–6wt%Mn master alloys under the protection of Ar atmosphere. Two compositions of Mg–1.3Al–1.2Ca–0.5Zn–0.6Mn and Mg–1Al–1Ca–0.7Zn–0.6Mn (wt%) were prepared, which were named AXZM1100 and AXZM1110, respectively. The actual compositions were measured by the inductively coupled plasma-atomic emission spectroscopy, as listed in Table 1. The as-cast ingots were then homogenized at 500°C for 12 h and quenched into water (~25°C). Before extrusion, billets with 45 mm in diameter and 120 mm in length were pre-heated at 200 or 250°C for 20 min and were then indirectly extruded into a 10-mm bar with a ram speed of ~0.3 mm/s and an extrusion ratio of ~20:1.
| Sample | Mg | Al | Ca | Zn | Mn |
| AXZM1100 | Bal. | 1.26 | 1.21 | 0.43 | 0.55 |
| AXZM1110 | Bal. | 0.99 | 0.97 | 0.66 | 0.50 |
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Mechanical properties of the as-extruded bars were measured along the extrusion direction (ED) at a strain rate of 10−3 s−1 at room temperature with a length of 25 mm and a diameter of 5 mm. The microstructures of these samples were observed by an optical microscope (OM, Olympus GX, Japan), scanning electron microscopy (SEM, JEOL JEM-7001F, Japan), and transmission electron microscopy (TEM, JEOL 2100F, Japan). Thin foils for TEM observations were prepared by mechanical polishing and ion beam thinning (GATAN, PIPS691, America). The TEM observation was conducted with an accelerating voltage of 200 kV. Moreover, a high-angle annular dark-field (HAADF) observation was also conducted.
Fig. 1 and Table 2 show the mechanical properties of as-extruded Mg samples. The AXZM1100 sample, which was extruded at a temperature of ~250°C (named AXZM1100-250), exhibits a high YS of ~411 MPa, UTS of ~418 MPa, and a balanced ductility of ~8.9%. When the extrusion temperature is reduced to ~200°C for the AXZM1100 billet (named AXZM1100-200), the strength can be obviously increased with a YS of ~437 MPa and a UTS of ~443 MPa. However, the EL is largely reduced to only ~1.5%. With the increasing of the Zn content and the decreasing of the Al, Ca contents in AXZM1110, the strength of the AXZM1110 sample extruded at ~250°C (named AXZM1110-250) does not change much, as compared with that of the AXZM1100-250 sample. Meanwhile, the EL was slightly decreased to ~6.4%.
| Sample | YS / MPa | UTS / MPa | EL / % |
| AXZM1100-250 | 411 | 418 | 8.9 |
| AXZM1100-200 | 437 | 443 | 1.5 |
| AXZM1110-250 | 408 | 413 | 6.4 |
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Figs. 2 and 3 display the OM and SEM images of as-extruded Mg samples. Typical bimodal microstructures involving both the fine dynamically recrystallized (DRXed) grains and elongated un-DRXed grains can be detected in Fig. 2. For the AXZM1100-250 sample (Fig. 2(a) and (b)), the DRXed degree is high (~71%), while the DRXed region in the AXZM1100-200 sample is largely decreased to only ~41% due to the relatively lower extrusion temperature (Fig. 2(c) and (d)). The thickness of elongated un-DRXed grains also increases from 2–10 μm in the AXZM1100-250 sample to 5–20 μm in the AXZM1100-200 sample. Increasing Zn and decreasing the Al, Ca content, the DRXed fraction in the AXZM1110-250 sample is evolved to ~63% after the extrusion at 250°C (Fig. 2(e) and (f)), and the thickness of elongated un-DRXed grains is also in the range of 2–10 μm. Compared with the AXZM1100-250 sample, the DRXed fraction of the AXZM1110-250 is reduced, which should be the main reason for the decreased elongation.
To identify the phase types in the present Mg samples, the energy diffraction spectrum (EDS) analysis was conducted, as shown in Fig. 3(b), (d), and (f). Results show that the micron-sized second phases are mainly composed of Mg, Al, and Ca (>99at% in total), as well as the trace amounts of Zn and Mn. Our previous work [24] reported that the (Mg,Al)2Ca phase is relatively stable, at least in the present condition of low extrusion temperature. In this context, the micron-sized phase is thus determined to be the (Mg,Al)2Ca ternary phase [25–27], which should come from the as-homogenized sample and is retained in the as-extruded Mg sample.
Fig. 4 displays the typical TEM images for the as-extruded AXZM1100-250 sample. Fine DRXed grains with an average size of ~0.7 μm have been observed (Fig. 4(a)–(c)). Numerous sphere-like nanoparticles with a diameter size of 20–80 nm, which are marked by a red dotted line, can also be found in the grain interiors. Profuse dislocations are activated during the extrusion process and are remained in the grain interiors, as shown in Fig. 4(d)–(f). Some dislocations are gradually evolved into low angular grain boundaries (LAGBs) [4,19], and subgrains with a lamellar thickness of 200–500 nm can be detected. Importantly, in the most un-DRXed regions and some of the DRXed grains, another two kinds of nano-precipitations can be found, i.e., needle-like nano-phases and bulk-like phases. These needle-like nano-phases have been frequently reported in Mg–Al–Ca-based alloys, which can be determined to be the Al2Ca [28–29]. Furthermore, the high angle annular dark field-scanning transmission electron microscopy (HAADF-STEM) and corresponding mapping images are also detected, and high-density nano-phases are found to disperse in the Mg matrix (Fig. 5). The sphere-like nanoparticles mainly contain Al and Ca atoms, which can also be determined to be the Al2Ca phase. In addition, the bulk nanoparticles mainly contain Al and Mn atoms, which can be identified to be Al–Mn phases. These Al–Mn phases are found to co-exist with Al2Ca, as shown in Fig. 5(a). The interaction between the nano-precipitations and dislocation lines can be observed in Fig. 4(d)–(f), which can contribute to the dislocation multiplication during extrusion and lead to the obvious DRXed grain nucleation. Meanwhile, a large number of dispersive nano-phases have been shown in Fig. 4(g)–(i). Some of these nano-phases can effectively hinder the growth of DRXed grains via impeding GB migrations in Fig. 4(i).
Fig. 6 displays the typical TEM images for the as-extruded AXZM1100-200 sample. Fine DRXed grains with an average size of ~0.4 μm have been detected (Fig. 6(a)–(c)), and the numerous sphere-like nanoparticles with a diameter size of 20–50 nm, which are marked by the red dotted line, can be found in the grain interiors. Besides that, profuse dislocations are also activated during the extrusion process and are remained in the grain interiors (Fig. 6(d)–(f)). According to the “g·b = 0 dislocation invisible” criterion [30], these residual dislocations can be determined to be the <c + a> type. Some dislocations have been evolved to be LAGBs (Fig. 6(e) and (f)). Compared with the AXZM1100-250 sample, the density of LAGBs is significantly increased, which divides the un-DRXed region into lamellae structures with a thickness of 100–300 nm. Numerous nano-precipitations can be found to disperse among the Mg matrix of AXZM1100-200, as shown in Fig. 6(g)–(i), which mainly include the sphere-like phase as marked by red dotted circles and the bulk phases as marked by yellow dotted circles.
To further clarify the second phases in the AXZM1100-200 sample, the HAADF-STEM and corresponding mapping images are detected in Fig. 7. Similar to the AXZM1100-250 sample extruded at a higher temperature, the sphere-like nanoparticles in the present AXZM1100-200 sample mainly contain Al and Ca atoms, which can be determined to be the Al2Ca phase, while the bulk-like nano-phase particles mainly contain Al and Mn atoms, which can be identified to be the Al–Mn phase [28,31].
Fig. 8 displays the typical TEM images for the as-extruded AXZM1110-250 sample. Fine DRXed grains with an average size of ~0.6 μm have been found (Fig. 8(a)–(c)). Numerous sphere-like nanoparticles with an average size of 30–80 nm and the bulk nano-phase with an average size of 50–100 nm can be observed in the grain interiors. Residual dislocations, as marked by purple arrows, are found to exist among the Mg matrix (Fig. 8(d)–(f)). Besides, a large number of nano-phases are dispersed in the as-extruded AXZM1110-250 sample, which also include sphere-like nano-phases and bulk nano-phases. HAADF-STEM images in Fig. 9 confirm that the sphere nano-phase is Al2Ca and the bulk nano-phase is Al–Mn. Compared to as-extruded AXZM1100 samples, the number density and average sizes in the AXZM1110 are largely increased, which is mainly due to the higher amount of Zn addition.
In the present Mg–Al–Ca–Zn–Mn sample, the dynamic recrystallization occurred during the extrusion process, and fine DRXed grains with an average size of ~0.7 μm have been formed in the as-extruded AXZM1100-250 sample. Three kinds of nanoparticles, including sphere-like Al2Ca phases, needle-like Al2Ca phases, and bulk Al–Mn phases, are precipitated in the present Mg samples. High-density nano-precipitations are homogeneously dispersed among the Mg matrix, which can effectively hinder the movement of dislocations and contribute to increasing the nucleation rate for the DRXed grains. Moreover, nano-precipitates distributing in grain interiors and/or along the GBs can pin the growth of GBs via the Zener pinning mechanism [19–20,32–33]. Simultaneously, the co-segregation of Ca, Al, and Zn elements has been reported in the present Mg–Al–Ca–Zn–Mn alloy system [14], which can also decrease the GB energy and enhance the thermal stability of ultra-fine DRXed grains [34]. As a result, ultra-fined grains with a size of less than 1 μm can be formed in the present Mg sample.
When the extrusion temperature for the AXZM1100 billet is reduced to ~200°C, the second phases become smaller and denser, and the residual dislocation density also becomes higher in the AXZM1100-200 sample (Figs. 6 and 7). Moreover, the nucleation and growth of DRXed grains are significantly affected by the extrusion temperature. In general, driving forces for DRXed grain nucleation and growth also become lower due to the relatively lower extrusion temperature [35]. Accordingly, the DRX degree is largely decreased compared to the AXZM1100-250 sample. The average DRXed grain size is also decreased to only ~0.4 μm in AXZM1100-200.
Adjusting the sample composition in the AXZM1110, the amount of Zn atoms is increased (~0.6wt%), and the Al, Ca contents are decreased. However, the amount of Mn is identical to that in AXZM1100 (~0.5wt%). Consequently, the number density of Al2Ca phases in AXZM1110-250 is largely decreased due to the lower content of Al and Ca (~0.9wt%), since the formation of the nano-Al2Ca phase is closely related to the total amount of Al and Ca atoms dissolved in the Mg matrix and their relative ratio. Moreover, the number density of Al–Mn phases is largely increased in the AXZM1110-250 sample. The particle size of Al–Mn phases also becomes larger due to the absences of the adjacent Al2Ca phase. These larger Al–Mn phases would thus deteriorate the ductility of AXZM1110-250.
The high YS of above 400 MPa in the present Mg samples can be ascribed to multiple factors, including ultra-fined grains, nano-precipitations, and residual dislocations. First, the fine DRXed grains with an average size of 0.4–0.7 μm can contribute to the high YS by following the Hall–Petch relationship:
Besides, the high-density nano-phases distributing among the Mg matrix can hinder the movement of dislocations and improve the YS via following the Orowan strengthening mechanism [12],
| ΔτOrowan=(Gb2π√1−v)(1λ)ln(DPr0), |
where G is the shear modulus (~17 GPa), b is the modulus of the Burgers Vector in dislocation (~0.32 nm); v is the Poisson ratio (~0.3), r0 is the core radius of the dislocation (about the value of b), DP is the average diameter of the second phase, λ is the average spacing of the second phase, and
Importantly, the strength and ductility combinations in Mg alloys are also correlated with texture. For un-DRXed regions, which usually exhibit a typical strong texture of <
Compared to the AXZM1100-250, the AXZM1110-250 sample exhibits a slight decrease in elongation of ~6.4%. First, the lower DRXed volume fraction (~63%) should be the reason for this observation [42–43], as illustrated above. Second, the average size of Al–Mn nanoparticles in the AXZM1110-250 sample is also larger than those in AXZM1100-250. Moreover, the stress concentration can occur at the interphase between the in-coherent Al–Mn particle and Mg matrix, which can thus lead to more severe microcracks and, consequently, a lower ductility.
In this work, a novel low-cost Mg–Al–Ca–Zn–Mn-based sample was investigated and the strength and ductility have been improved simultaneously. The main conclusions can be drawn as follows.
(1) An ultra-high YS of ~411 MPa and a high EL of ~8.9% have been achieved in the AXZM1100-250 sample. EL would be largely decreased to only ~1.5% in the AXZM1100-200 sample.
(2) The high strength of the AXZM1100-250 sample is mainly due to the fine grain strengthening caused by ultra-fine DRXed grains, high-density dislocations in the un-DRXed region, and nano-precipitates distributed among the α-Mg matrix.
(3) The good ductility in the AXZM1100-250 sample can be ascribed to the high volume fraction of DRXed grains with a more randomized texture. In contrast, the lower DRXed degree and the larger-sized Al–Mn phases lead to the relatively lower ductility of ~6.4% in the AXZM1110-250 sample.
The work is financially supported by National Key Research and Development Program of China (No. 2021YFB3701000), the National Natural Science Foundation of China (Nos. U2167213 and 51971053), the Young Elite Scientists Sponsorship Program by China Association for Science and Technology (Nos. 2019-2021QNRC001, 2019-2021QNRC002, and 2019-2021QNRC003), and the Fundamental Research Funds for the Central Universities (No. N2202020). Special thanks are due to Dr. Na Xiao in Analytical and Testing Center of Northeastern University for the assistance with EBSD analysis.
The authors have no competing interests to declare that are relevant to the content of this article.
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| Sample | Mg | Al | Ca | Zn | Mn |
| AXZM1100 | Bal. | 1.26 | 1.21 | 0.43 | 0.55 |
| AXZM1110 | Bal. | 0.99 | 0.97 | 0.66 | 0.50 |
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| Sample | YS / MPa | UTS / MPa | EL / % |
| AXZM1100-250 | 411 | 418 | 8.9 |
| AXZM1100-200 | 437 | 443 | 1.5 |
| AXZM1110-250 | 408 | 413 | 6.4 |
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