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Article history: Microstructure and mechanical properties of sand mold cast Mg4.58Zn2.6Gd0.18Zr magnesium alloy
Received 14 February 2015 after different heat treatments were investigated. As-cast alloy was composed of a(Mg) matrix, interden-
Received in revised form 13 April 2015 dritic a(Mg) + W(Mg3Zn3Gd2) eutectic, icosahedral quasicrystalline I(Mg3Zn6Gd) phase and Mg3Gd parti-
Accepted 9 May 2015
cles within a(Mg) matrix. After solution treatment at 505 C for 16 h, most of a(Mg) + W(Mg3Zn3Gd2)
Available online 12 May 2015
eutectic dissolved into a(Mg) matrix, but a new phase, Zn2Zr3, precipitated within a(Mg) matrix. The
appropriate aging treatment was done at 220 C for 16 h, after which some dispersive ne eutectics
Keywords:
re-precipitated along the grain boundary. Furthermore, rod-like b01 and plate-like b02 formed within
Magnesium alloy
Sand-casting
a(Mg) matrix. The ultimate tensile strength, yield strength and elongation of the experimental alloy in
Microstructure the T6 state at room temperature were 280 MPa, 175 MPa and 7.5%, respectively. According to strength-
Heat treatment ening contribution calculation, it is revealed that both the second phase strengthening and the solid solu-
Mechanical properties tion strengthening played important roles in improving the mechanical properties after T6 treatment.
2015 Elsevier B.V. All rights reserved.
1. Introduction size of Mg4.5Zn (wt%) alloy was rened with increasing Gd con-
tent up to 1.5 wt% and the highest UTS and YS with the values of
MgZn-based alloys are one of the most promising magnesium 231 MPa and 113 MPa had been achieved in Mg4.5Zn1.5Gd
alloys for their low cost and high strength, which are widely used (wt%) alloy after T6 treatment [8]. Kim et al. [9] investigated the
in various airframe components [1]. However MgZn-based alloy effect of Gd (03 wt%) on the microstructure and mechanical prop-
cannot be used above 175 C because of their poor mechanical erties of Mg3Zn (wt%) alloy. The maximum tensile strength at
properties at elevated temperature. More recently, the rare earth both room and 175 C were obtained for (12 wt%)Gd. Mg8Gd
(RE) metals are proved to be the most effective elements to xZn0.4Zr (x = 0, 1 and 3 wt%) alloy reinforced with LPSO and W
improve the tensile strength of Mg alloys at elevated temperatures phases have been developed by Liu et al. [10]. It was found that
[2,3]. Gd is often used in MgZn alloy since it can form some high W phase plays an important role in improving the mechanical
thermal stability phases, such as, Mg3Gd, W(Mg3Zn3Gd2) with properties via pinning the grain boundaries. Srinivasan et al. [11]
cubic structure, I(Mg3Zn6Gd) with icosahedral quasicrystal struc- compared the microstructure and mechanical properties of Mg
ture, and phase with a long periodic stacking ordered (LPSO) struc- xGdyZn (x = 2, 10 wt%, y = 2, 6 wt%) alloys and found that higher
ture, which greatly depends on Zn/Gd ratio. I(Mg3Zn6Gd) phase has Gd-containing alloys showed higher yield strength due to the
been identied by TEM in both Mg95.9Zn3.5Gd0.6 (at%) alloy [4] and higher volume fraction of LPSO phase within a(Mg) matrix. It can
Mg98.25Zn1.5Gd0.25 (at%) alloy [5] with high Zn/Gd values. With the be expected that a high Gd content enhances UTS and YS.
decrease in Zn/Gd ratio, Mg3Gd particles and W(Mg3Zn3Gd2) phase However, it should be noted here that a high Gd content reduces
appear in Mg97.4Zn1.8Gd0.8 (at%) alloy [6]. Further increasing Gd ductility and increases the density and production cost. The opti-
content, LPSO structure phase will form in as-cast Mg96Zn1Gd3 mization of Gd addition into MgZn-based alloy is, therefore, of
(at%) alloy [7]. great necessity to keep a good balance between mechanical prop-
More recently, some results about microstructure and mechan- erties and costs. As reported in the previous works [810], the
ical properties of MgZnGd alloys have been reported. The grain addition of 23 wt% Gd was believed to be an optimizer.
However, there is still a lacking of the detailed investigation on
Corresponding author. Tel.: +86 13679228998; fax: +86 029 88495414. the microstructure evolution and mechanical properties of Mg
E-mail address: ygy@nwpu.edu.cn (G.Y. Yang). ZnGd alloy containing 23 wt% Gd.
http://dx.doi.org/10.1016/j.jallcom.2015.05.062
0925-8388/ 2015 Elsevier B.V. All rights reserved.
S.J. Liu et al. / Journal of Alloys and Compounds 644 (2015) 846853 847
In this paper, a new experimental alloy with moderate Gd con- equiaxed a(Mg) grains with an average size of about 60 lm. The
tent, Mg5.0Zn2.5Gd0.4Zr (wt%), was designed and prepared discontinuous netted eutectic distributed along the grain boundary
using the traditional sand-casting process. The microstructure and some big-bone-like ones aggregated at tripe junctions.
and mechanical properties of the experimental alloy were investi- Particles marked as A was observed inside a(Mg) matrix from
gated and compared with the commercial ZK51A alloy [1]. The pos- SEM image of Fig. 1(b). Its composition was determined to be
sible strengthening mechanisms were also discussed. Mg25.17Zn65.30Zr (at%) by EDS analysis, as shown in Fig. 1(c),
which is thought to be a(Zr) phase and acts as the nucleation site
2. Experiment procedure for a(Mg) during solidication, leading to the grain renement
[12]. EDS result of point B shown in Fig. 1(d) indicated that the
The experimental alloy with nominal composition of Mg5.0Zn2.5Gd0.4Zr composition of the eutectic phase was Mg15.64Zn8.84Gd (at%),
(wt%) was prepared from pure Mg, pure Zn, Mg28Gd and Mg33Zr (wt%) master
which was further identied as W(Mg3Zn3Gd2) with partially
alloys and melt in an electrical-resistance furnace under the protection of an
anti-oxidizing ux (RJ4, containing 5456% KCl, 1416% BaCl2, 1.52.5% MgO, 27
ordered AlMnCu2-type FCC structure [13], according to the
29% CaCl2). After rening with C2Cl6 and holding at 780 C for 20 min, the melt selected area electron diffraction (SAED) pattern shown in Fig. 2.
was cast in a sand mold of the standard tensile test bars at 740 C. The actual chem- It is also found a quadrangular phase and an ellipsoid phase
ical composition of the as-cast bar was determined to be Mg4.58Zn2.6Gd0.18Zr existing inside a(Mg) matrix, as shown in Fig. 3(a) and (c), respec-
(wt%) by using an inductively coupled plasma-optical emission spectrometry
tively. It is determined that the quadrangular phase was Mg3Gd
(ICP-OES). The melting point was taken on a Universal V4.1DTA differential scan-
ning calorimetry (DSC) with heating rate of 10 C/min. with BiF3 structure [11] and the ellipsoid phase was I(Mg3Zn6Gd)
The test bars were solution treated at 505 C for 16 h (T4), quenched in hot [13] according to SAED patterns shown in Fig. 3(b) and (d), respec-
water of 6080 C, and subsequently aged at different temperatures between 200 tively. The diffraction pattern of the ellipsoid phase showed a
and 250 C for various dwelling times (10 min130 h) (T6). Vickers hardness tests
5-fold symmetry, which is the typical characteristic for the
were conducted using a 0.5 kg load and 15 s of dwell time. At least 10 points were
measured for each specimen and the average value was calculated. The samples for
icosahedral quasicrystalline structure. It has been reported that
tensile tests had a gauge length of 60 mm and a diameter of 12 mm. The tensile I(Mg3Zn6Gd) phase can be formed within Zn/Gd ratio range of
properties were determined in a Zwick 150 type universal tensile testing machine 1.540.0 and W(Mg3Zn3Gd2) formed within Zn/Gd ratio range
with a crosshead speed of 2 mm/min (corresponding to an initial engineering strain of 0.256.0 [14]. Thus, when the ratio of Zn/Gd falls in the range
rate of 4.6 104 s1). At least three specimens were used for each test condition to
of 1.56.0, I(Mg3Zn6Gd) and W(Mg3Zn3Gd2) phases can coexist in
ensure the reproducibility of the data. The microstructure was observed with
Olympus PM-G3 optical microscope (OM), JEOL JSM-5800 scanning electron micro- MgZnGd alloys. The ratio of Zn/Gd in the experimental alloy is
scope (SEM) and Technai 30F transmission electron microscope (TEM). TEM sam- just about 4.24. The low volume fraction of I(Mg3Zn6Gd) phase
ples were prepared using electron polishing. Phase analysis was conducted in was also approved according to XRD pattern results shown in
Oxford Inca X-Ray energy dispersive spectroscope (EDS) and EPMA-1720 Electron
Fig. 4.
probe micro-analyzer (EPMA). The X-ray diffraction (XRD) was performed on
XPert PRo MPD instrument in the diffraction angle (2h) range between 20 and
90, using Cu Ka (k = 0.154 nm) as the radiation source. 3.2. Microstructure after solution treatment
3. Experimental results and discussion Fig. 5 shows the DSC curve of as-cast alloy. The rst peak at
about 520.81 C corresponded to the melting of the eutectic phase,
3.1. As-cast microstructure and the peak at 630.48 C was related to the melting of a(Mg)
grains.
OM and SEM micrographs of the as-cast experimental alloy are Solution treatment temperature should be normally lower by
shown in Fig. 1(a) and (b). It is seen that the as-cast alloy had 1020 C than the eutectic temperature [15]. According to DSC
Fig. 1. OM and SEM images of the as-cast experimental alloy. (a) OM image, (b) SEM image, (c) EDS result at the point A, and (d) EDS result at the point B.
848 S.J. Liu et al. / Journal of Alloys and Compounds 644 (2015) 846853
Fig. 2. TEM analysis of eutectic phase along grain boundary. (a) TEM bright eld image, and (b) SAED pattern.
Fig. 3. TEM analysis of the second phase within a(Mg) matrix. (a) and (c) TEM images of quadrangular and ellipsoid phases, (b) and (d) corresponding SAED patterns.
analysis of the experimental alloy, solution treatment temperature, Some long-rod-like particles were observed in a(Mg) grains
therefore, was selected to be 505 C, and the solution time was after solution treatment, as shown in Fig. 8(a) and (b), which had
selected to be 16 h, considering the slow diffusion rate of rare earth an average size about 150 nm in length and 15 nm in width.
element in a(Mg) matrix. After the solution treatment, as shown in According to EDS analysis, as shown in Fig. 8(c), the precipitate
Fig. 6, big-bone-like interdendritic a(Mg) + W(Mg3Zn3Gd2) disap- was enriched in Zn and Zr, which can be further identied as
peared and most of the continuous network eutectics decomposed Zn2Zr3 phase according to SAED pattern shown in Fig. 8(d). As
to ne particle-shaped ones. According to XRD pattern shown in reported previously [16], Zn2Zr3 precipitate was governed predom-
Fig. 7, the quenched experimental alloy mainly consisted of inantly by the core of Zr content during solidication, which asso-
W(Mg3Zn3Gd2), I(Mg3Zn6Gd) and Mg3Gd phases. ciated with the grain rening process. Due to the low contents of Zr
S.J. Liu et al. / Journal of Alloys and Compounds 644 (2015) 846853 849
Fig. 7. XRD pattern of the experimental alloy after solution treated at 505 C for
Fig. 4. XRD pattern of the as-cast experimental alloy.
16 h.
Fig. 8. TEM analysis of the long-rod-like precipitates in the solution treated experimental alloy. (a) low and (b) higher magnied TEM micrographs, (c) corresponding EDS
spectra and (d) SAED pattern.
Fig. 10. OM image of the quenched experimental alloy after aged at 220 C for 16 h.
Fig. 9. Hardness as a function of time for solution-treated experimental alloy aged
at various temperatures.
89 MPa, respectively, which is at less 27% higher than those of
are presented in Fig. 13, respectively. Compared with the as-cast ZK51A alloy [1]. The improvement of mechanical properties at
specimen, solution treatment resulted in a great enhancement in elevated temperatures can be directly related to the concurrent
elongation accompanied by a relatively small increase in UTS and formation of the thermally stable W(Mg3Zn3Gd2) phase, quasicrys-
YS. Further aging treatment led to a signicant improvement in talline I(Mg3Zn6Gd) phase and Mg3Gd particles with a high
UTS and YS but with a small decrease in elongation. The UTS and thermal stability, which can effectively restricted the grain defor-
YS of T6 state experimental alloy were up to 280 MPa and mation and dislocation gliding at high temperatures [711].
175 MPa, respectively, which was higher than those of ZK51A alloy
under T6 state [1]. 3.5. Strengthening mechanisms
The high temperature mechanical properties of the T6 state
experimental alloy is shown in Fig. 14. It can be seen that UTS The strengthening mechanisms for the magnesium alloy in dif-
and YS at 200 C of the experimental alloy are up to 145 MPa and ferent conditions are typically divided into fourfold (i) pure Mg
S.J. Liu et al. / Journal of Alloys and Compounds 644 (2015) 846853 851
Fig. 12. TEM analysis of the precipitates in a(Mg) grain. (a) TEM image of the long-rod-like Zn2Zr3 precipitates, (b) TEM images of the rod-like and plate-like precipitates, (c)
0a direction, (d) HRTEM image, and (e) the corresponding FFT image of the plate-like precipitate.
SAED pattern in 0 1 1
852 S.J. Liu et al. / Journal of Alloys and Compounds 644 (2015) 846853
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