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Journal of Magnesium and Alloys ■■ (2017) ■■–■■
www.elsevier.com/journals/journal-of-magnesium-and-alloys/2213-9567
Review
Experimental investigation on the phase equilibria of the Mg-Sn-Ag
system in the Mg-rich corner
Tingting Tong, Fan Zhang, Shuhong Liu *, Yong Du, Kun Li
State Key Laboratory of Powder Metallurgy, Central South University, Changsha, Hunan 410083, China
Received 12 November 2016; revised 17 February 2017; accepted 17 February 2017
Available online
Abstract
Phase equilibria of the Mg-Sn-Ag system in Mg-rich corner at 320 and 400 °C were experimentally investigated with nine ternary alloys
subjected to electron probe microanalysis and X-ray diffraction techniques. No ternary compounds were observed at both isothermal sections. Two
three-phase triangles, i.e. hcp (Mg) + Mg2Sn + Mg3Ag and Mg2Sn + Mg3Ag + MgAg (bcc_B2), were both observed at 320 and 400 °C. A new
three-phase region of Ag3Sn + Mg2Sn + MgAg (bcc_B2) was additionally observed at 320 °C, which implied that the binary phase Ag3Sn has a
considerable solubility of Mg in the ternary system at the temperature. And the maximal solubility of Mg in Ag3Sn was measured to be 27.2 at.%.
This result is not consistent with the thermodynamic calculated isothermal section at 350 °C from Wang et al. [11] and put forward a new
requirement or refinement for the optimization of the Mg-Sn-Ag ternary system. At 400 °C, the maximal solubility of Sn in the Mg3Ag phase was
determined to be about 3.0 at.% Sn, and the solubility of Ag in Mg2Sn was negligible. The temperature of ternary eutectic reaction at Mg-rich
corner (L↔hcp (Mg) + Mg54Ag17 + Mg2Sn) was measured by differential scanning calorimetry. The partial isothermal sections in Mg-rich corner
of the ternary system at 320 and 400 °C were then constructed based on the above experimental data.
© 2017 Production and hosting by Elsevier B.V. on behalf of Chongqing University. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/).
Keywords: Mg-Sn-Ag system; X-ray diffraction techniques; Electron probe microanalysis; Differential scanning calorimetry; Isotheromal sections
1. Introduction
With their low density, excellent specific strength, good
machinability, high thermal conductivity and recycle ability,
Mg-based alloys have attracted more and more world-wide
attention in recent decades [1] and a number of Mg alloys have
been developed, such as Mg-Al based alloys, Mg-Zn based
alloys and Mg-RE based alloys. However, the strength and
creep resistance of Mg-based alloys are often significantly
reduced with the increase of temperature, which can bring out
the fact that the corrosion resistance, creep resistance and wear
resistance of the alloys have difficulty meeting the requirements. Therefore, increasing the high temperature performance
of the alloys is an important subject for magnesium alloy
research in recent years.
Mg-Sn-based alloys were proved to have good mechanical
properties at high temperatures due to the existence of Mg2Sn,
* Corresponding author. State Key Laboratory of Powder Metallurgy, Central
South University, Changsha, Hunan 410083, China. Fax: +86 731 88710855.
E-mail address: shhliu@csu.edu.cn (S. Liu).
which has a high melting point [2]. They were thus considered
as potential heat-resistant magnesium alloys. Unfortunately, the
quenched Mg-Sn-based alloys take a long time to reach peak
hardness, which is not practical for industrial production [3]. In
addition, with the increase of Sn content, the Mg2Sn phase
coarsens and the alloys form a semi-continuous network structure at the grain boundary. All above phenomena deteriorate the
performance of the alloys [4]. It was reported that the addition
of Ag can significantly refine the grain to improve the creep
resistance and enhance the mechanical properties by aging
strengthening [5–8]. For the advanced development of the
Mg-Sn-Ag based alloys, knowledge on the phase equilibria of
the Mg-Sn-Ag system becomes very important.
Up to now, very limited experimental information is available about the ternary Mg-Sn-Ag system in the literature.
Raynor et al. [9] firstly measured isothermal sections of the
ternary system in Ag-rich corner at the 450 and 550 °C by
the microscopic and X-ray diffraction (XRD) methods. Using
thermal analysis, optical microscopy and XRD techniques,
Karonik et al. [10] supplemented the phase region of
Mg-rich corner at 450 °C and determined the vertical sections
http://dx.doi.org/10.1016/j.jma.2017.02.003
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(http://creativecommons.org/licenses/by-nc-nd/4.0/).
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Table 1
Crystal structure data on the solid phases in the ternary Mg-Ag-Sn system.
Phase
Pearson
symbol/prototype
Lattice
parameters (Å)
Reference
Ag3Mg
MgAg(bcc_B2)
AgMg4
cP4-AuCu3
cP2-CsCl
hP*
[16]
[12]
[14]
AgMg3
Ag17Mg54
cF*-AsNa3
O/142
Mg2Sn
hcp
cF12-CaF2
hP2- Mg
Ag3Sn
oP8-Cu3Ti
a = 4.111
a = 3.331
a = 2.509
c = 14.470
a = 17.622
a = 14.240
b = 14.209
c = 14.663
a = 6.765
a = 2.966
c = 4.782
a = 5.968
b = 4.780
c = 5.184
[14]
[14]
[13]
[15]
[15]
at constant 10 wt. % Ag and 10 wt. % Sn. In recent years, Wang
et al. [11] determined the phase relations at the Mg-rich corner
at 350 and 415 °C by XRD and electron probe microanalysis
(EPMA). The solubilities of Ag in Mg2Sn at 350 and 415 °C are
both less than 0.1 at.%, the maximal solubility of Sn in Mg3Ag
is as large as 3 ± 0.5 °C at.%. No solubilities of Mg in the
Ag-Sn compounds were observed in the ternary system. The
ternary vertical sections with compositions of 10 at.% Sn and
30 at.% Ag were also determined by differential scanning calorimetry (DSC) measurements. Based on the available experimental data, Wang et al. [11] optimized the Mg-Sn-Ag system
and calculated the isothermal sections of 415 and 350 °C and
the liquidus projection. However, there are very scarce experimental points below 400 °C, it limits the optimization and may
lead to some wrong understandings about the phase relations.
The Mg-Ag and Mg-Sn phase diagrams were critically
evaluated by Nayeb–Hashemi and Clark [12,13]. According to
the assessed Mg-Ag phase diagram, there are three intermediate compounds in the Mg-Ag system, viz. MgAg (bcc_B2),
Ag3Mg, Mg3Ag. Later on, the phase equilibria of the Mg-Ag
system were re-investigated by Lim et al. [14] using DSC, XRD
and scanning electron microscope (SEM) techniques, and the
existences of AgMg4 and Ag17Mg54 were confirmed. In the
Mg-Sn system, there is only one compound viz. Mg2Sn. For
the Ag-Sn system, there are two intermediate compounds, viz.
hcp(Ag4Sn) and Ag3Sn reported by Mas [15]. Table 1 summarizes all the intermediate phases in the three binary systems of
the Mg-Sn-Ag system.
The aims of the present work are to determine the phase
equilibria of Mg-Sn-Ag in Mg-rich corner and to provide more
accurate experimental data for the future thermodynamic modeling of the ternary system.
2. Materials and methods
Nine alloys were prepared with high-purity Mg (99.99wt.%
purity), Ag (99.99wt.% purity) and Sn (99.99 wt.% purity). The
accurately weighed Mg and Ag pieces and the Sn blocks were
mixed in a graphite crucible, and then melted by a frequency
induction furnace under a high-purity argon atmosphere. The
melted alloys were cut into two blocks and sealed into quartz
capsules for an equilibrium treatment. The blocks were
wrapped by tantalum sheets to avoid the interaction of the
samples with quartz capsules at annealed temperatures. The
quartz capsules were put in the L4514-type diffusion furnaces
at 320 ± 2 °C for 60 days and 400 ± 2 °C for 45 days, respectively. After annealing, all the alloys were quenched in cold
water without breaking the quartz tubes.
The annealed alloys were examined by XRD (D8-advance,
Bruker, Germany) at 40 kV and 40 mA to identify the phases
included in the alloys. The metallographic samples of the
annealed alloys were firstly examined using optical microscopy
and then analyzed by EPMA (JXA-8530, JEOL, Japan) employing pure Mg (99.99 wt.%), Sn (99.9 wt.%) and Ag (99.9 wt.%) as
standard to determine the composition of each phase in the
ternary system. The EPMA measurements were carried out at
15 kV and 2 × 10−8 A. To avoid a reaction with water, the metallographic samples were ground and polished under alcohol.
Alloy # 9 (Mg85.0Ag5.0Sn10.0) annealed at 320 °C for 60 days
was examined by DSC (DSC404C, Netzsch, Germany). The
sample was sealed in a small Ta crucible due to the high
evaporability of Mg. The measurement was conducted from
room temperature to 800 °C with heating and cooling rates of
5 °C/min under an argon gas atmosphere. In the examined
temperature range, the accuracy of the temperature measurement was estimated to be ±2 K by measuring the melting temperatures of some pure metals (In, Sn, Zn, Al, Ag, Au, Bi, Ni).
The accurate temperature of the invariant reaction was determined from the onset of the thermal effects during the heating
step.
3. Results and discussions
The nominal compositions and the experimental information
on the phase equilibria of the alloys annealed at 320 °C for 60
days and 400 °C for 45 days are summarized in Tables 2 and 3,
respectively. Phases identification and the compositions of all
the alloys were analyzed by XRD and EPMA. All the results of
both measurements agreed well with each other.
3.1. Isothermal section at 400 °C
The experimental investigation of the isothermal section at
400 °C mainly focused on the composition region from 50 at.%
Mg to 100 at.% Mg. It is because of that that the other compositions are in single phase regions or contain liquid phase which
could react with quartz capsules.
XRD patterns and backscattered electron (BSE) images
of the alloys annealed at 400 °C for 45 days are presented
in Figs. 1 and 2, respectively. Figs. 1a and 2a are the XRD
pattern and the BSE micrograph of the annealed alloy # 1
(Mg50.0Ag45.0Sn5.0), respectively. As shown in Fig. 2a, the gray
phase is Mg2Sn and the light-gray phase is MgAg (bcc_B2).
It reveals that the alloy is located in a two-phase region of
Mg2Sn and MgAg (bcc_B2). Alloys # 2 (Mg50.0Ag30.0Sn20.0) and
# 3 (Mg50.0Ag40.0Sn10.0) have the similar microstructure with
the different volume ratio of Mg2Sn and MgAg (bcc_B2). The
BSE microstructure and XRD pattern of the annealed alloy # 4
Please cite this article in press as: Tingting Tong, Fan Zhang, Shuhong Liu, Yong Du, Kun Li, Experimental investigation on the phase equilibria of the Mg-Sn-Ag system in the Mg-rich
corner, Journal of Magnesium and Alloys (2017), doi: 10.1016/j.jma.2017.02.003
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Table 2
Summary of the experimental information on the phase equilibria in the alloys annealed at 400 °C for 45 days (at.%).
Nominal Composition
Composition by EPMA
No.
Mg
Ag
1
50.0
45.0
Sn
5.0
2
50.0
30.0
20.0
3
50.0
40.0
10.0
4
65.0
15.0
20.0
5
75.0
5.0
20.0
Phases
Mg
Ag
Sn
Remark
Mg2Sn
MgAg (bcc_B2)
Mg2Sn
MgAg (bcc_B2)
Mg2Sn
MgAg (bcc_B2)
Mg3Ag
Mg2Sn
MgAg (bcc_B2)
hcp(Mg)
Mg2Sn
Mg3Ag
66.9
46.0
67.1
38.2
66.6
49.0
73.5
66.8
56.2
97.4
67.8
77.0
1.0
49.5
0.5
52.5
2.2
49.1
23.5
0.2
43.5
1.6
0.1
20.6
32.1
4.5
32.5
9.3
31.2
2.0
3.0
32.9
0.3
1.0
32.1
2.3
Tie-line
(Mg65.0Ag15.0Sn20.0) indicate that Mg2Sn, Mg3Ag and MgAg
(bcc_B2) are in three-phase equilibrium, as shown in Figs. 1b
and 2b. In the Fig. 2b, the black phase is Mg3Ag, the gray phase
is Mg2Sn, and the lighter gray phase is MgAg (bcc_B2). In the
three-phase region, both the solubilities of Ag in Mg2Sn and
Sn in MgAg (bcc_B2) are negligible, but the solubility of Sn
in Mg3Ag is up to be about 3 at.%. Experimental results of the
annealed alloy # 5 (Mg75.0Ag5.0 Sn20.0) in Figs. 1c and 2c show
that the alloy is composed of the dark hcp (Mg) phase, the light
Mg2Sn phase and the gray Mg3Ag phase. This alloy is located in
a three-phase field of hcp (Mg) + Mg2Sn + Mg3Ag. The solubilities of Ag and Sn in hcp (Mg) are about 1.6 at. % and 1.0 at.
%, respectively. The solubility of Sn in Mg3Ag is about 2.3 at.
%. However, the solubility of Ag in Mg2Sn is negligible.
Taking into account the present experimental results, the
isothermal section at 400 °C in Mg-rich corner is presented in
Tie-line
Tie-line
Tie-triangle
Tie-triangle
Fig. 3, in which the nominal compositions of the alloys are
also indicated. Two three-phase regions at the Mg-rich corner
are determined at 400 °C, i.e. hcp (Mg) + Mg2Sn + Mg3Ag and
Mg2Sn + Mg3Ag + MgAg (bcc_B2), which is consistent with
the experimental and calculated results at 415 °C in literature
[11].
3.2. Isothermal section at 320 °C
Figs. 4 and 5 are the XRD patterns and BSE images of a few
representative alloys annealed at 320 °C for 60 days, respectively. Figs. 4a and 5a are the XRD pattern and BSE image
of annealed alloy # 2 (Mg50.0Ag30.0 Sn20.0), which indicate that
the alloy is located in a two-phase region of Mg2Sn + MgAg
(bcc_B2). Besides, the alloy # 1 (Mg50.0Ag45.0Sn5.0) has the
similar microstructure with the different volume ratio of Mg2Sn
and MgAg (bcc_B2). Because of the small amount of the
Table 3
Summary of the experimental information on the phase equilibria in the alloys annealed at 320 °C for 60 days (at.%).
Nominal Composition
Composition by EPMA
No.
Mg
Ag
Sn
1
50.0
45.0
5.0
2
50.0
30.0
20.0
4
65.0
15.0
20.0
5
75.0
5.0
20.0
6
35.0
45.0
20.0
7
65.0
25.0
10.0
8
77.5
17.5
5.0
9
85.0
5.0
10.0
Phases
Mg
Ag
Sn
Mg2Sn
MgAg (bcc_B2)
Mg2Sn
MgAg (bcc_B2)
Mg3Ag
Mg2Sn
MgAg (bcc_B2)
hcp(Mg)
Mg2Sn
Mg3Ag
Ag3Sn
Mg2Sn
MgAg (bcc_B2)
Mg3Ag
Mg2Sn
MgAg (bcc_B2)
hcp(Mg)
Mg2Sn
Mg3Ag
hcp(Mg)
Mg2Sn
Mg3Ag
——
49.5
67.2
38.0
74.1
68.4
54.0
97.6
67.3
77.9
27.2
67.4
35.0
73.8
67.3
56.8
97.1
68.2
77.2
97.7
68.6
78.6
——
48.7
0.5
52.9
23.0
0.2
45.7
1.3
0.1
19.8
54.8
0.4
52.4
23.4
1.4
45.2
2.5
0.2
20.7
0.8
1.4
19.3
——
1.8
32.3
9.2
2.9
31.5
0.3
1.1
32.6
2.3
18.1
32.2
12.7
2.8
31.3
0.2
0.4
31.6
2.2
1.5
30.1
2.2
Remark
Tie-line
Tie-triangle
Tie–triangle
Tie-triangle
Tie-triangle
Tie–triangle
Tie–triangle
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Fig. 1. XRD patterns of the representative alloys annealed at 400 °C for 45
days: (a) alloy 1 (Mg50.0Ag45.0Sn5.0), (b) alloy 4 (Mg65.0Ag15.0Sn20.0), (c) alloy 5
(Mg75.0Ag5.0Sn20.0).
Fig. 2. BSE images of representative alloys annealed at 400 °C for 45 days:
(a) alloy 1 (Mg50.0Ag45.0Sn5.0), (b) alloy 4 (Mg65.0Ag15.0Sn20.0), (c) alloy 5
(Mg75.0Ag5.0Sn20.0).
Please cite this article in press as: Tingting Tong, Fan Zhang, Shuhong Liu, Yong Du, Kun Li, Experimental investigation on the phase equilibria of the Mg-Sn-Ag system in the Mg-rich
corner, Journal of Magnesium and Alloys (2017), doi: 10.1016/j.jma.2017.02.003
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Fig. 3. Experimental isothermal section at 400 °C of the Mg-Sn-Ag system in
Mg-rich corner with the nominal compositions.
5
Mg2Sn in the alloy # 1 (Mg50.0Ag45.0Sn5.0) at 320 °C, the measurement of EPMA was not determined. The compositions of
phases MgAg (bcc_B2) and Mg2Sn determined by EPMA are
presented in Fig. 6, which exhibit that the solubility of Sn in
MgAg (bcc_B2) changes along with the compositions of alloys
and the solubility of Ag in Mg2Sn can be negligible.
The annealed alloy # 6 (Mg35.0Ag45.0Sn20.0) is located in a
three-phase equilibrium region of Ag3Sn + Mg2Sn + MgAg
(bcc_B2), as shown in Fig. 4b. The microstructure of the alloy
is shown in Fig. 5b, in which the black and gray phases are
Mg2Sn and MgAg (bcc_B2), respectively, the lighter gray phase
is Ag3Sn. The phase boundary of the three-phase region
(Ag3Sn + Mg2Sn + MgAg (bcc_B2)) is accurately established
based on the EPMA measurement. And the solubility of Mg in
Ag3Sn was measured to be 27.2 at. %.
Fig. 4. XRD patterns of the alloys annealed at 320 °C for 60 days: (a) alloy 2 (Mg50.0Ag30.0Sn20.0), (b) alloy 6 (Mg35.0Ag45.0Sn20.0), (c) alloy 7 (Mg65.0Ag25.0Sn10.0),
(d) alloy 8 (Mg77.5Ag17.5Sn5.0).
Please cite this article in press as: Tingting Tong, Fan Zhang, Shuhong Liu, Yong Du, Kun Li, Experimental investigation on the phase equilibria of the Mg-Sn-Ag system in the Mg-rich
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Fig. 5. BSE images of representative alloys annealed at 320 °C for 60 days: (a) alloy 2 (Mg50.0Ag30.0Sn20.0), (b)alloy 6 (Mg35.0Ag45.0Sn20.0), (c) alloy 7
(Mg65.0Ag25.0Sn10.0), (d) alloy 8 (Mg77.5Ag17.5Sn5.0).
It should be noted that the experimental results observed
in the annealed alloy # 6 (Mg35.0Ag45.0Sn20.0) are not consistent
with the work of Wang et al. [11], in which the thermodynamically
extrapolated three-phase region is Mg2Sn + hcp (Ag4Sn) + MgAg
Fig. 6. (Online color) Experimental isothermal section at 320 °C of the
Mg-Sn-Ag system in Mg-rich corner with the nominal compositions.
(bcc_B2), and there is not a phase region including Ag3Sn
and MgAg (bcc_B2) simultaneously. Besides, thermodynamic
extrapolation is based on limited experimental information, we
think our present experimental results are confidential.
The differences indicate that the experimental information
about the Mg-Sn-Ag ternary system is not comprehensive to
optimize. The annealed alloy # 7 (Mg65.0Ag25.0Sn10.0) is characterized to be in the three-phase region of Mg2Sn + Mg3Ag + MgAg
(bcc_B2), as shown in Figs. 4c and 5c. As presented in Fig. 5c,
three phases can be seen, i.e. the dark Mg3Ag phase, the gray
Mg2Sn phase and the light-gray MgAg (bcc_B2) phase. The
XRD pattern and BSE image of the annealed alloy # 8
(Mg77.5Ag17.5Sn5.0) are presented in Figs. 4d and 5d, respectively.
In Fig. 5d, the black phase is hcp (Mg), the gray phase is Mg3Ag
and the light-gray phase is Mg2Sn. The experimental results
indicate the alloy is located in the three-phase equilibrium field of
Mg2Sn + Mg3Ag +hcp (Mg).
Based on the present experimental results and the binary
phase diagrams reported in literature [12–16], the isothermal
section of Mg-rich corner at 320 °C is constructed and
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reasonable. All the reaction temperatures are consistent with
the experimental results (463, 529 and 569 °C respectively)
from Wang et al. [11].
4. Conclusions
Fig. 7. DSC curves of the representative alloy 9 (Mg85.0Ag5.0Sn10.0).
exhibited in Fig. 6. The measured tie-lines and tie-triangles
along with the locations of the prepared alloys are displayed
in the figure. According to our present work, Ag3Sn is in
equilibrium with Mg2Sn and MgAg (bcc_B2) at 320 °C and the
solubility of Mg in Ag3Sn is 27.2 at. %, which are not consistent
with the work of Wang et al. [11]. All the results indicate that it
is necessary for the optimization of Wang et al. [11] to do some
refinement in order to reproduce the experimental information.
No ternary compounds were observed.
3.3. DSC measurements
The DSC curves of alloy # 9 (Mg85.0Ag5.0Sn10.0) annealed at
320 °C for 60 days are presented in Fig .7. There are two
distinct endothermic peaks in the heating process, referred to
the vertical section at constant 10 at. % Sn from Wang et al.
[11], the first peak represents the ternary eutectic reaction
L↔hcp (Mg) + Mg54Ag17 + Mg2Sn, and the second peak indicates a monovariant transition of binary eutectic reaction
L↔hcp (Mg) + Mg2Sn. Three exothermic peaks are presented
during the cooling curve. The first two peaks are well repeated
the peaks during heating process, and the third peak represents
the transition of L↔Mg2Sn. The reason for the difference
between the cooling curve and heating curve is that the peak of
the reaction L↔Mg2Sn is weak during the heating process.
In conclusion, the ternary eutectic equilibrium temperature
of L↔hcp (Mg) + Mg54Ag17 + Mg2Sn was determined to be
470 °C and the transition reaction temperatures of L↔hcp
(Mg) + Mg2Sn and L↔Mg2Sn were measured to be 534 °C and
566 °C, respectively. Compared to the temperature of eutectic
reaction: L↔hcp (Mg) + Mg2Sn, in the Mg-Sn binary system
(561 °C) from Nayeb–Hashemi and Clark [13], the result is
Based on XRD, EPMA and DSC measurements, phase equilibria of the Mg-Sn-Ag system in the Mg-rich corner were
analyzed, the isothermal sections in Mg-rich corner at 320
and 400 °C were constructed, and no ternary compounds were
obtained. The three-phase regions of Mg2Sn + Mg3Ag + MgAg
(bcc_B2) and Mg2Sn + Mg3Ag + hcp (Mg), and the two-phase
fields of Mg2Sn + MgAg (bcc_B2) and Mg2Sn + Mg3Ag were
observed at both isothermal sections. Three-phase equilibrium
of Ag3Sn + Mg2Sn + MgAg (bcc_B2) was observed at 320 °C
but not 400 °C. At 320 °C, the solubility of Mg in Ag3Sn was
measured to be 27.2 at. %. The results put forward a new
requirement for the optimization of the Mg-Sn-Ag ternary
system. The temperature of the invariant reaction (L↔hcp
(Mg) + Mg54Ag17 + Mg2Sn) in Mg-rich corner was determined
to be 470 °C.
Acknowledgments
The financial support from National Key Research and
Development Plan (No. 2016YFB0701202) and State Key
Laboratory of Powder Metallurgy Central South University,
China (No. 1991DA105636), are greatly acknowledged.
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Please cite this article in press as: Tingting Tong, Fan Zhang, Shuhong Liu, Yong Du, Kun Li, Experimental investigation on the phase equilibria of the Mg-Sn-Ag system in the Mg-rich
corner, Journal of Magnesium and Alloys (2017), doi: 10.1016/j.jma.2017.02.003