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Effects of cooling rate and pressure on microstructure and mechanical propertiesof sub-rapidly solidified Mg–Zn–Sn–Al–Ca alloy
Chen Jihua
, Wei Juying, Yan Hongge, Su Bin, Pan Xueqiang
School of Materials Science and Engineering, Hunan University, Changsha 410082, PR China
a r t i c l e i n f o
 Article history:
Received 26 July 2012Accepted 2 September 2012Available online 18 September 2012
Keywords:
Magnesium alloySolidificationMicrostructureMechanical properties
a b s t r a c t
Effects of cooling rate and pressure on microstructure and mechanical properties of sub-rapidly solidifiedMg–6Zn–3Sn–2Al–0.2Ca alloy were investigated by OM, XRD, SEM and tensile testing. The alloy preparedby steel mould casting with no applied pressure is mainly composed of four phases i.e.
a
-Mg, Mg
2
Sn,MgZn and Mg
32
(Al,Zn)
49
, while those prepared by water-cooling steel mould casting under pressureand water-cooling copper mould casting under pressure consist of 
a
-Mg, Mg
2
Sn, Mg
51
Zn
20
and Mg
32
(-Al,Zn)
49
. The higher cooling rate promotes the formation of the grain boundary compounds, while theapplied pressure has an inhibiting effect on it. The alloy prepared by water-cooling copper mould castingunder pressure is characteristics of the finest grain size, the smallest dendrite arm spacing and the muchfiner, well-distributed second phases among the five as-studied alloys, exhibiting the optimal mechanicalproperties, with the ultimate tensile strength, the yield strength and elongation to rupture of 224 MPa,157 MPa and 16.1% respectively. In comparison with the alloy prepared by steel mould casting with noapplied pressure, the ductile fracture characteristics of void coalescence is dominant for the alloy pre-pared by water-cooling copper mould casting under pressure.
Ó
2012 Elsevier Ltd. All rights reserved.
1. Introduction
Conventional magnesium alloys exhibit the relatively lowstrength, poor creep resistance and inferior plasticity due to theintrinsic hcp structure and cannot be used for the manufacture of key structural components[1].Therefore, it is of great significance to develop novel magnesium alloys with high strength and goodtoughness. In the recent years, more and more attention has beenpaid to the Mg–Zn–Snsystem. Moststudies are focused on improv-ing microstructure and mechanical properties of the Mg–Zn–Snsystem by alloying such as RE[2]and Al[3–5]and micro-alloying such as Ca[6,7]and Y [8]. Sasaki et al. have conducted the study on the heat-treatable Mg–Sn–Zn wrought alloy[9]. Up to now, veryfew investigations have been conducted on the effects of solidifica-tion conditions especially sub-rapid solidification on this system.Sub-rapid solidification is the solidification process of moltenmetal with a relatively high cooling rate, ranging from 10
0
K/s to10
3
K/s[10], which has the advantages of both conventional solid-ification and rapid solidification. In comparison with rapid solidifi-cation, it is more near the actual production and is easier to realizethe industrial production. Therefore, it is an effective means to im-prove strength of magnesium alloys[11]. In fact, water-coolingmetallic mould casting under pressure can elevate the cooling rateof molten metal and is likely to achieve sub-rapid solidification,which is similar to die casting or twin-roll casting.One previous study showed that the as-cast Mg–6Zn–3Sn–2Al–0.2Ca alloy exhibited the best combination of mechanical proper-ties and was the most corrosion-resistant among the as-studiednine alloys[12]. Another study exhibited that the ultimate tensilestrength and elongation to rupture of the Mg–6Zn–3Sn–2Al–0.2Cawrought alloy extruded at 300
°
C with the extrusion ratio of 25were up to 387 MPa and 9% respectively[13]. Obviously, the Mg–6Zn–3Sn–2Al–0.2Ca alloy has a great potential for alloy develop-ment. Therefore, this alloy composition is selected for the presentstudy. In this paper, the effects of cooling rate and pressure onmicrostructure and mechanical properties of sub-rapidly solidifiedMg–6Zn–3Sn–2Al–0.2Ca alloy are reported. The main goals of thestudy are to explore the mechanical performance potential of thisalloy and to provide a way of preparing the high-quality ingot suit-able for the subsequent plastic forming.
2. Experimental details
The Mg–6Zn–3Sn–2Al–0.2Ca alloy (in mass%) was prepared inan electric resistance furnace with a mild steel crucible protectedby the RJ-2 flux (37.1% KCl–43.2% MgCl
2
–6.8% BaCl
2
–4.8%CaF
2
–6.6% [NaCl + CaCl
2
]–1.3% water-insoluble–0.4% moisture).Commercially pure Mg, Al, Zn, Sn, Mn (99.9%) blocks and Ca(99.99%) powders were added to prepare the alloy. Mn was added
0261-3069/$ - see front matter
Ó
2012 Elsevier Ltd. All rights reserved.http://dx.doi.org/10.1016/j.matdes.2012.09.003
Corresponding author. Tel.: +86 731 88664005.
E-mail address:
Contents lists available atSciVerse ScienceDirect
Materials and Design
 
to diminish the negative effect of the impurity Fe on corrosionresistance of the as-prepared alloy. The melt was purged for10 min and held for 15 min at 760
°
C so that homogenization of alloying elements and settlement of inclusions could be realized.Then, molten alloy was cast into the steel mould with no appliedpressure, the water-cooling steel mould with no applied pressure,the water-cooling copper mould with no applied pressure, thewater-cooling steel mould casting under pressure and the water-coolingcoppermouldcastingunder pressurerespectivelyat acast-ing temperature of 720
°
C. Three types of moulds were adopted toachieve different cooling rates. Hereafter, the as-cast samples werereferred to as A, B, C, D and E respectively. The applied pressure of about 45 MPa on the melt was achieved by the YJ32-315A four-col-umn hydraulic press. The 0.45%C carbon steel and the brass wereadopted as the mould material respectively and the cavity dimen-sion of the mould was 100 mm
Â
150 mm
Â
20 mm. The speci-mens for microstructure examination and mechanical testing aresectioned near the bottom of the casting and their sectioned posi-tions are identical.The as-cast microstructures were observed using an MM-6metallographic microscope (OM) and a FEI QUANTA 200 scanningelectron microscopy (SEM) after etching with a solution of 1.5 goxalic acid, 5 ml acetic acid, 10 ml water and 25 ml ethanol. Themicro-compositional analysis of some certain phases was con-ducted on a FEI QUANTA 200 scanning electron microscopyequipped with the Oxford X-ray energy dispersive spectroscopy(EDS).Thevolumefractionofthegrainboundaryphaseswascalcu-lated using the Image-PropPlus 6.0 software. The overall phaseconstitutions of these alloys were analyzed by a D5000 X-ray dif-fraction instrument with Cu K
a
and a scanning rate of 0.01 deg/s.The as-cast plates were machined into the flat tensile specimenswith a gauge section of 15 mm
Â
4 mm
Â
2 mm. They were pro-portional test bars according to the ISO 377-1997[14]. The tensiletests were performed on a WDW-200 tensile testing machine withan initial strain rate of 1.1
Â
10
À
3
s
À
1
. The ultimate tensile strength(UTS), the yield tensile strength (YTS) and elongation to rupture(Er) were averaged over four or five specimens. Micro-hardnesstesting was conducted on a MHV-2000 micro-hardness instrumentwith the load of 0.98 N and a holding time of 15 s. Fracto-graphicobservations were conducted on the FEI QUANTA 200 scanningelectron microscopy to clarify the fracture process.
3. Results and discussion
 3.1. As-cast microstructures
The OM images of the as-cast alloys sectioned from the sameposition are shown inFig. 1. The five alloys are characteristics of divorced eutectics, with the Mg solid solution as the matrix anda portion of grain boundary compounds. The average grain size
d
and the primary dendrite arm spacing
k
1
of the as-cast alloys arelisted inTable 1. Obviously, both of them are in the descending or-der of A, B, C, D and E. The casting A has an average grain size of 70
l
m, while the casting E is characteristic of an average grain sizeof 40
l
m. Moreover, the grain boundary phases have differentmorphologies. They are bone-like, semi-continuously scattered inthe casting A, relatively fine, semi-continuously scattered in thecasting B and the casting C, and granular, isolately scattered inthe casting D and the casting E. It is clear that cooling rate andpressure have obvious influences on the grain size and the mor-phology of the grain boundary phases.The heat-transfer coefficient (HTC) at the metal/mould interfaceis a very important factor in predicting the solidification rate andfinal grain structure. The cooling of the casting depends, in the firststage, on the heat capacity of the mould. The heat conductivityplays a role in later stages unless the air-gap between the castingand mould controls the heat flux[15]. On the basis of the experi-ments utilizing different types of water-cooled chills for Al–Si al-loys, there is a direct relationship between the thermaldiffusivity of the chill material and the HTC values[16]. The heatconductivities of the 0.45C% steel and the Cu–30Zn brass at600
°
C are 35.17 W/(m K) and 117.23 W/(m K) respectively[17].Accordingly, the cooling rate of the casting C (
R
C
) is much higherthan that of the casting B (
R
B
) during the later stage of solidifica-tion. In contrast to the casting B, the casting A is lack of water cool-ing. Hence,
R
A
<
R
B
<
R
C
. According to Furer and Wunderlin[18],Kirkwood[19]and Mortenson[20], the relationship between the dendrite arm spacing
k
and the cooling rate
R
is represented bythe following equation:
k
¼
Á
R
À
1
=
3
ð
l
m
Þ ð
1
Þ
where
is the coefficient. Increasing the cooling rate of the meltcontributes to grain refinement and the smaller primary or second-ary dendrite arm spacing. As shown inTable 1, the
k
1
value is in thedescending order of A, B, C and adverse to the cooling rate
R
.According to Eq.(1),
R
C
is about 4 times of 
R
A
and 2 times of 
R
B
. Itwas reported that the cooling rates of the steel mould and thewater-cooling copper mould were 48.6 K/s and 253.5 K/s respec-tively[21]. Therefore,
R
B
and
R
C
are estimated to be 100 K/s and200 K/s respectively. In addition, the amount of grain boundarycompound in the casting increases in the order of A, B and C. Itcan be possibly attributable to the reduced solid solubility associ-ated with a fairly high cooling rate.The casting D and the casting E are solidified under pressure.Due to the different mould material, the cooling rate of the castingE (
R
E
) is higher than that of the casting D (
R
D
). Thus, the
d
and
k
1
values of the casting E are smaller than those of the casting Drespectively. Moreover, the casting D has finer grains and less grainboundary compound than the casting B, and the casting E has finergrains and less grain boundary compound than the casting C.Seemly, the applied pressure contributes to grain refinement, sup-presses the formation of grain boundary compounds and refinesthe grain boundary eutectics.The grain refining effect derived from pressure can be explainedin two aspects. On the one hand, the applied pressure is beneficialto the smaller air gap between the melt and the mould and thusthe effective contact area is increased[22]. The latter brings aboutthe higher HTC and thus results in the higher cooling rate duringsolidification, which is beneficial to grain refinement. On the otherhand, solidification of liquid metal involves two processes i.e.nucleation and crystal growth. Both are affected by the appliedpressure at the same time. Different from aluminum alloys, mag-nesium alloys exhibit volume shrinkage during solidification[23].As far as the alloys with solidification contraction are concerned,solidification under pressure is associated with the higher meltingpoint when the freezing point is constant and thus the degree of supercooling is increased. According to the solidification theory,the higher degree of supercooling is associated with the highernucleation density and the larger crystalline growth velocity. Morenuclei are formed and nucleus growth is suppressed by growth of adjacent grains. For this reason, grain refinement can be achievedduringsolidification under pressureeven thoughthe largercrystal-line growth velocity is involved. Therefore, the casting E is featuredwith the smallest
d
and
k
1
values.Theappliedpressurehas an inhibitingeffect onthe formationof grain boundary compounds in the Mg–6Zn–3Sn–2Al–0.2Ca alloy,indicating the extended solid solubility of some certain soluteatoms. It was reported that the volume fraction of Mg
17
Al
12
inthe Mg–Al alloy system increased with the increment of appliedpressure[23–25], indicating that the solid solubility of Al in Mg
 J. Chen et al./Materials and Design 45 (2013) 300–307 
301
 
was reduced when solidified under pressure. However, the volumefraction of second phases in the Mg–Zn alloy was opposite, indicat-ing that the solid solubility of Zn in Mg was extended when solid-ified under pressure[23]. Obviously, the change of solid solubilitywith applied pressure is dependent on the kind of solute atoms.This inhibiting effect on the formation of grain boundary com-pounds is possibly related to the elevated solid solubility of Zn,Sn and Ca in Mg when solidified under pressure. The detailed rea-son will be discussed later and is worth further study.The SEM images of the casting A and the casting E are shown inFig. 2. Evidently, the block-like divorced eutectics are distributedalong grain boundaries and have a splitting effect on the matrixin the casting A, while finer, more homogenous intermetallicsalong grain boundaries are detected in the casting E and have a rel-atively weak splitting effect on the matrix. It can be predicted thatthe casting E exhibits higher strength and better plasticity than thecasting A, which is confirmed by the subsequent mechanical test-ing. In addition, the volume fraction of grain boundary compoundsin the casting A is 4.62 vol.%, while that in the casting E is7.83 vol.%. The latter is about 69% higher than the former. The de-tailed reason will be described below.To clarify the compositions of certain phases, the EDS analysis isadopted. The EDS analysis results of the solid solution cores andthe grain boundary compounds are listed inTable 2. As shown inFig. 2c andTable 2, the atomic ratio of Mg–Zn of the coarse grain boundary phase in the casting A is approached to 1 and it is likely
Fig. 1.
The OM images of the castings solidified under different conditions. (a) Steel mould casting with noapplied pressure (Casting A). (b) Water-coolingsteel mould castingwith no applied pressure (Casting B). (c) Water-cooling copper mould casting with no applied pressure (Casting C). (d) Water-cooling steel mould casting under pressure(Casting D). (e) Water-cooling copper mould casting under pressure (Casting E).
 Table 1
The average grain size
d
and the primary dendrite arm spacing
k
1
of the castingssolidified under different condition.
Alloy symbol Solidification condition
d
(
l
m)
k
1
(
l
m)Mould Cooling Pressure(MPa)Casting A Fe0.45%C Air-cooling 0 70 69.55Casting B Fe0.45%C Water-cooling 0 60 53.44Casting C Cu30Zn Water-cooling 0 50 44.55Casting D Fe0.45%C Water-cooling 45 45 38.79Casting E Cu30Zn Water-cooling 45 40 31.55302
J. Chen et al./Materials and Design 45 (2013) 300–307 

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