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Materials Science and Engineering A 444 (2007) 99103

Semisolid microstructure of Mg2Si/Al composite by cooling slope


cast and its evolution during partial remelting process
Q.D. Qin, Y.G. Zhao , P.J. Cong, W. Zhou, B. Xu
Key Laboratory of Automobile Materials of Ministry of Education and Department of Materials Science & Engineering,
Jilin University, No. 142 Renmin Street, Changchun 130025, PR China
Received 17 April 2006; accepted 15 August 2006

Abstract
An in situ Mg2 Si/AlSiCu composite with semisolid structure was fabricated by cooling slope cast and partial remelting process. The as-cast
microstructure, and effect of isothermal holding time on the morphology, size and shape factor of the grains were investigated. The results show
that the morphology of primary Mg2 Si and -Al grains in the composite are globular and/or elliptic after partial remelting process. The size and
shape factor of -Al grains increase with the isothermal holding time.
2006 Elsevier B.V. All rights reserved.
Keywords: Semisolid; Aluminum; Composites; Microstructure; Magnesium silicide

1. Introduction
It has been well known that semisolid processing (SSP) has a
lot of significant advantages over conventional casting, such as
minimizing the macrosegregation and solidification shrinkage
and reducing the forming temperature. The key that permits the
semisolid alloys to shape is the absence of dendritic morphology
of the solid phase [1]. The typical non-dendritic microstructure needed is constituted of solid phase globules suspended in
the liquid phase. The thixotropic effect of the semisolid alloys
allows them to be handled as a massive solid and to attain fluidlike properties when sheared during shaping [2]. Many different
routes have been used to produce non-dendritic microstructure,
such as magnetohydrodynamic (MHD) stirring, spray forming,
strain induced melt activated (SIMA)/recrystallisation and partial melting (RAP), liquidus/near-liquidus casting etc. [38].
Recently, Czerwinski [911] investigated the fabrication of
semisolid Mg alloys components by injection molding process.
Kleiner et al. [12] studied the formation of semisolid MgAlZn
alloy by extruded method. Wu et al. [13] constructed a model on
growth morphology of semisolid metals, using solidification and
flow speed of the liquid as variations affecting the morphology
of crystals. Among all the techniques of SSP, the cooling slope

Corresponding author. Tel.: +86 431 509 4481; fax: +86 431 509 5592.
E-mail address: zhaoyg@jlu.edu.cn (Y.G. Zhao).

0921-5093/$ see front matter 2006 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2006.08.074

process is a simple route. The primary phase in the semisolid


alloy by the cooling slope cast has been reported to become
spherical after remelted in the semisolid state [14]. Haga and
Suzuki [14,15] investigated the producing process of ingots for
thixoforming of Al6Si alloys by cooling slope casting.
Hypereutectic AlSi alloys with high Mg content is in fact an
in situ aluminum matrix composites containing a large amount
of hard particles of Mg2 Si, and the Mg2 Si/Al composite has a
potential as automobile brake disc material because the intermetallic compound of Mg2 Si exhibits has high melting temperature, low density, high hardness, low thermal expansion
coefficient and reasonably high elastic modulus [8]. However,
the coarse reinforcement of the primary Mg2 Si particles in the
normal composite leads to poor properties. Therefore, the composite with coarse primary Mg2 Si particles need to be modified
to obtain adequate mechanical strength and ductility. It has been
reported that rare earth elements such as Ce [16], Sr [17] and
its salts [18,19] have the power to modify the morphology of
primary Mg2 Si. A semisolid microstructure in the composite is
expected to improve the mechanical properties. The semisolid
of Mg2 Si/Al composite has been produced via SIMA in previous study [8]. However, this technology is relative complex
because of requiring cold extrusion and deformation. Less work
has been carried out on semisolid Mg2 Si/Al composite by the
cooling slope cast and partial remelting process. In the present
study, a semisolid of in situ Mg2 Si/AlSiCu composite was
prepared by the cooling slope cast and partial remelting process,

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Q.D. Qin et al. / Materials Science and Engineering A 444 (2007) 99103

Table 1
Chemical compositions of the Mg2 Si/Al composite (wt.%)
Materials

Al

Mg

Si

Cu

Cr

Zn

Ni

Fe

AlSiMgCu

Bal.

13.276

11.281

3.523

<0.005

<0.023

<0.001

0.325

size and area of the primary solid phase were analyzed statistically by a quantitative analysis system (Omnimet Imaging
Systems-Buehler, USA).
3. Results and discussion

Fig. 1. Technical schematic diagram of the cooling slope cast and partial remelting, adopted from [15].

and the effect of isothermal holding-time on the microstructure


of the composite was investigated.
2. Experimental procedure
Commercial Al13 wt.% Si master alloy (ingot), pure Cu
(ingot, >99.7% purity) and magnesium (ingot, >98.0% purity)
were used to prepare the experimental alloy. About 520 g of
AlSi master alloy melt was molten in a graphite crucible in an
electric resistance furnace. About 100 g of magnesium and 26 g
of Cu, preheated at 300 C, were added into the AlSi melt at
680700 C. After holding 15 min, the melt were poured into a
steel mold via a aluminum cooling slope (preheated at 300 C) to
produce the in situ Mg2 Si/Al composite ingots, and the chemical compositions are listed in Table 1. The schematic of the
casting process is shown in Fig. 1 (adopted from [15]). Subsequently, the ingot was cut into a series of cubic samples of
12 mm 12 mm 12 mm. The partial remelting process was
performed in a vertical tube furnace, and the samples were heated
up to 560 C and held at the temperature for 30, 60, 180 and
600 min, respectively, and then were quenched in cold water.
Metallographic specimens were polished through standard
procedure and the microstructure in them examined using an
optical microscopy. A 0.5% hydrofluoric acid (HF) aqueous
solution was used as the etchant of polishing samples. The grain

According to the composition of the alloy and the previous


studies [8,16], the as-cast microstructure of the composite consists of Mg2 Si, -Al and eutectic Si phases. Fig. 2a and b shows
the typical as-cast microstructure of in situ Mg2 Si/Al composite by the normal cast and cooling slope cast, respectively. The
microstructure of the composite reveals that the morphology of
primary Mg2 Si as-cast in the composite by the normal cast was
dendritic (as indicated with a arrow in Fig. 2a), with a size of
200 m, and the -Al was dendritic as well. However, after the
composite solid with the cooling slope, the morphology of -Al
phase in the composite by the cooling slop cast changes from
dendritic to spheral with a diameter of 10 m, and the primary
Mg2 Si crystals become fine obviously, as seen in Fig. 2b. One
reason for it is due to the increase in the nucleation substrates
in the melt after casting with the cooling slope; another reason
is related to the flow of the melt on the slope. The flowing melt
will cause partial fragments of the dendrites of the dendrites by
convection.
Fig. 3ad shows the evolution of the semisolid microstructures of the composite by the cooling slope cast with the
holding time of isothermal heat treatment of 30, 60, 180 and
600 min, respectively. Fig. 3a shows that the as-cast coarse
Mg2 Si dendrites are fragmented, changing to an irregular
shape, with slightly rounded tips, and the morphology of -Al
have becomes globular with a mean size of 51 m. As the
holding time increases to 60 min, the morphology of the Mg2 Si
particles in the composite becomes mainly elliptic shape and the
morphology of -Al becomes more globular with a mean size
of 85 m seen in Fig. 3b. Furthermore, it also shows that some
smaller -Al grains is not dissolved completely surviving in the
liquid, as indicated by white arrows in Fig. 3b. Fig. 3c shows the

Fig. 2. As-cast microstructures of Mg2 Si/Al composites by (a) the normal cast (adopted from [8]) and (b) the cooling slope cast.

Q.D. Qin et al. / Materials Science and Engineering A 444 (2007) 99103

101

Fig. 3. Semisolid microstructures of the Mg2 Si/Al composite by the cooling slope cast with different isothermal holding time of (a) 30 min, (b) 60 min, (c) 180 min
and (d) 600 min.

microstructure of the composite with a isothermal treatment for


180 min. The morphologies of the Mg2 Si and -Al particles do
not change obviously, however, the mean size of -Al particles
increases to 111 m. It is of interest to note that some smaller
grains emerge on the surface of the large globular grains of
-Al, as indicated by black arrows in Fig. 3c. The amount of the
survived small solid particles increases, in comparison with that
of 60 min holding time. It seems that the liquid fraction increases
as well. Unfortunately, the liquid fraction could not be measured
in the present study, because of the survived of the small solid
particles. Poirier et al. [20] reported that the volume fraction of
liquid of AlCu alloy slightly decreased at the coarsening period
during semisolid isothermal treatment. The phenomenon needs
further study. Fig. 4a shows that the morphology of the smaller
grains is columnar and some survived solid phases are irregular
shape as denoted by the white arrow in Fig. 4a. As the isothermal

treatment time increases up to 600 min, the morphologies of


the primary Mg2 Si particles and -Al grains are still globular,
as shown in Fig. 3d. The size of the -Al grains increase
obviously with a mean size of 149 m. In addition, the amount
of the survived solid particles evidently decreases, and the
smaller grains on the surface of large -Al grains disappear.
The smaller grains emergence may be the consequence of
solidification of the liquid during handling of the samples before
quenching in water, and that emergence and disappearance
may be due to the difference of the handle time for quenching.
From Fig. 4b, it is clearly indicated that the morphologies of
the survived solid particles do not change obviously.
To get better understanding of the evolution of the solid particles is of important, because it determines the final grain size
of the composite, and thus the mechanical properties [21]. The
formation of a semisolid structure by isothermal holding from a

Fig. 4. Metallographs of the composites with the isothermal time of (a) 180 min and (b) 600 min, showing the -Al smaller grains.

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Q.D. Qin et al. / Materials Science and Engineering A 444 (2007) 99103

Fig. 5. The relationship of the mean size of -Al grains and the holding time.

Fig. 6. Relationship of the shaper factor of the -Al grains ant the holding time.

conventionally cast dendritic structure has been studied earlier


[8]. The transition of the solid phase from dendritic into spheral
is thought to be due to the liquid penetration, namely, the ascast grain boundary is penetrated by liquid during the semisolid
isothermal holding, causing the fragmentation of the dendrite
arms and then, the fragmented arms change into spheroidal or
ellipsoidal grains.
The relationship between the grain size of the -Al particles
and holding time is shown in Fig. 5. The size of the -Al particles increases with the holding time. One coarsening mechanism
is the coalescence of the grains, namely, two grains encounter
joining together and forming new bigger grain [22]. Another
coarsening mechanism is the Ostwald ripening [22,23], in which
the larger grains grow and the smaller grains remelt.
Using the image analysis system, the number of the objects
in a selected area, and the perimeter and area of selected objects
can be measured [2]. Normally, the shape of an object is characterized by the shape factor F0 defined as [2]:

ing time, the higher curvature part of the solid particle will be
dissolved, and leading to the increase of the F0 . Finally, the process reaches to a dynamic equilibrium and the shape factor of
the grains will not change.

4A0
F0 =
P02

4. Conclusion
The semisolid structure of in situ Mg2 Si/Al composite is
successfully produced by the cooling slope cast and partial
remelting process. The results show that: (a) the morphology
of primary Mg2 Si phase is globular and/or elliptic not changing
obviously with increase in the isothermal holding time; (b) with
increase in the isothermal holding time from 30 to 600 min, the
mean size of -Al grains increases from 50 to 150 m, and its
morphology becomes more globular; (c) the shape factor of the
-Al solid particles rapidly from 0.51 to 0.69 with the holding
time from 30 to 60 min.
Acknowledgements

(1)

where A0 and P0 represent the area and perimeter of the object,


respectively [2]. The change of the shape factor during the
isothermal treatment is shown in Fig. 6. It is indicated that the
shape factor increases rapidly from 0.51 to 0.69 with the holding
time from 30 to 180 min and however, a much larger holding
time cannot result in a considerable change of F0 , suggesting
that the F0 seems to reach to a maximum value. It is reported
that the solid phase particles tend to become spherical, but, for
a longer holding time, the change of the shape of the particles
slows down and even reverses in the case of the high values of
solid volume fraction [21]. Keeping in mind that the high solid
volume fraction means also a high contiguity, this reversion from
the spherical shape can be attributed to the hard impingement
of the solid particles, leading to the local shape distortions [21].
In the present study, however, the solid volume fraction in the
microstructures is lower relatively (0.6) according to the result
of the quantitative analysis, and consequently, the chance of the
hard impingement is lower as well. With increase in the hold-

This work is supported by The Project 985-Automotive Engineering of Jilin University and The Innovation and Invention
Foundation of Jilin University (2003CX029).
References
[1]
[2]
[3]
[4]

[5]
[6]
[7]
[8]
[9]
[10]

E. Tzimas, A. Zavaliangos, Mater. Sci. Eng. A 289 (2000) 217.


W.R. Loue, M. Suery, Mater. Sci. Eng. A 203 (1995) 1.
H.V. Atkinson, Prog. Mater. Sci. 50 (2005) 341.
M.P. Kenney, J.A. Courtois, R.D. Evans, G.M. Farrior, C.P. Kyonka, A.A.
Koch, K.P. Young, Metals Handbook, vol. 15, 19th ed., ASM International,
Metals Park, OH, USA, 1988, p. 327.
P.J. Ward, H.V. Atkinson, P.R.G. Anderson, L.G. Elias, B. Garcia, L.
Kahlen, J.M. Rodriguez-Ibade, Acta Mater. 44 (1996) 1717.
K.P. Young, C.P. Kyonka, J.A. Courtois, Fine grained metal composition,
US Patent no. 4,414,374 (30 March 1982).
European Patent 0745694A1, Method and apparatus of shaping semisolid
metals, UBE Industries Ltd. (1996).
Q.D. Qin, Y.G. Zhao, K. Xiu, W. Zhou, Y.H. Liang, Mater. Sci. Eng. A 407
(2005) 196.
F. Czerwinski, Acta Mater. 53 (2005) 1973.
F. Czerwinski, Mater. Sci. Eng. A 392 (2005) 51.

Q.D. Qin et al. / Materials Science and Engineering A 444 (2007) 99103
[11]
[12]
[13]
[14]
[15]
[16]

F. Czerwinski, Int. Powder Met. 41 (2005) 64.


S. Kleiner, O. Beffort, P.J. Uggowitzer, Scr. Mater. 51 (2004) 405.
S.S. Wu, X.P. Wu, Z.H. Xiao, Acta Mater. 52 (2004) 3519.
T. Haga, S. Suzuki, J. Mater. Process. Technol. 118 (2001) 169.
T. Haga, J. Mater. Process. Technol. 130131 (2002) 558.
Y.G. Zhao, Q.D. Qin, W. Zhou, Y.H. Liang, J. Alloys Compd. 389 (2005)
L1.
[17] Y.G. Zhao, Q.D. Qin, Y.H. Liang, W. Zhou, Q.C. Jiang, J. Mater. Sci. Lett.
40 (2005) 1831.

103

[18] Y.G. Zhao, Q.D. Qin, Y.Q. Zhao, Y.H. Liang, Q.C. Jiang, Mater. Lett. 58
(2004) 2192.
[19] J. Zhang, Z. Fan, Y. Wang, B. Zhou, J. Mater. Sci. Lett. 18 (1999)
783.
[20] D.R. Poirier, S. Ganesan, M. Andres, P. Ocansey, Mater. Sci. Eng. A 148
(1991) 289.
[21] M. Ferrante, E. Freitas, Mater. Sci. Eng. A 271 (1999) 172.
[22] J.L. Wang, Y.H. Su, C-Y.A. Tsao, Scr. Mater. 37 (1997) 2003.
[23] M.C. Flemings, Metall. Trans. A 22A (1997) 957.

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