Materials and Design 32 (2011) 2701–2709

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Materials and Design

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The effect of solution temperature on the microstructure and tensile properties

of Al–15%Mg2Si composite
A. Malekan a, M. Emamy a,⇑, J. Rassizadehghani a, A.R. Emami b
a
School of Metallurgy and Materials Engineering, University of Tehran, P.O. Box 14395-731, Tehran, Iran
b
Department of Mechanical and Aerospace Engineering, Science and Research Branch, Islamic Azad University, Tehran, Iran

a r t i c l e i n f o a b s t r a c t

Article history: The effect of different solution temperatures has been investigated on the microstructure and tensile
Received 21 October 2010 properties of in situ Al–Mg2Si composite specimens were subjected to solutionizing at different temper-
Accepted 8 January 2011 atures of 300 °C, 350 °C, 400 °C, 450 °C, 500 °C, 550 °C and 580 °C for holding time of 4 h followed by
Available online 19 January 2011
quenching. The microstructural studies of the polished and etched samples by scanning electron micros-
copy (SEM) in the solution condition indicated that the increase in the temperature changes the morphol-
Keywords: ogy of both the primary and secondary Mg2Si phases. Solutionizing led to the dissolution of the Mg2Si
A. Composites
particles and changed their morphology. Tensile test results indicated that ultimate tensile strength
C. Heat treatments
C. Casting
(UTS) gradually decreased upon solutionizing from 300 to 550 °C while further increase in the tempera-
ture followed by a sharp decrease in UTS up to 580 °C solutionizing temperature. It was found that the
elongation has become three times greater in comparison to the as-cast state. Elongation results showed
an increase up to 500 °C and then reduced temperatures of 550 and 580 °C. Fractographic analysis
revealed a cellular nature for the fracture surface. On the cellular fracture surface, the features of both
brittle and ductile fracture were present simultaneously. As a result of solution treatment the potential
sites for stress concentration and crack initiation areas were reduced due to softening of the sharp cor-
ners and break up of eutectic network respectively, while increase in the number of fine dimples ren-
dered the nature of fracture to ductile and also increased elongation.
Ó 2011 Elsevier Ltd All rights reserved.

1. Introduction nary phase area. According to Eq. (1), this pseudo-eutectic

reaction is completed at a temperature of 583.5 °C (Fig. 1b) [4,5]:
Al-based composites, reinforced with Mg2Si particles have been
L ! ðMg2 SiÞP þ L1 ! ðMg2 SiÞP þ ðAl þ Mg2 SiÞE ð1Þ
lately introduced as a new group of particulate metal matrix com-
posites (PMMCs) that offer some attractive advantages such as low where E is a Eutectic, P is a Primary, and L1 is a Liquid in two phase
density, good wear resistance and good castability [1,2]. These region.
composites are considered as new engineering materials and Unfortunately, Mg2Si particles are prone to coarsen in the cast
may be viable replacement for some dense alloys in automobile composite during solidification. It has been found that the coarsen-
and airplane components. One of the most appropriate techniques ing of particles, resulting from the eutectic reaction, greatly deteri-
to fabricate these composites is in situ process, since advantages orates the mechanical properties, which is an important obstacle
like an even distribution of the reinforcing phase; good particle for the wide application of this type of composites [3,6–8]. There-
wetting and low costs of production are usually achieved [3]. fore, several works have been focused on the modification of the
It can be concluded from the equilibrium phase diagrams of the composite structure and particularly the Mg2Si particles with the
ternary Al–Mg–Si and binary Al–Mg2Si [4,5] systems (Fig. 1) that Si addition of various alloying elements such as P, Sr, Ce, Ti, B and
can hardly dissolve into solid aluminum and tends to form precip- Zr [5,8–11] and with the use of semi-solid processing techniques
itates with Al or other elements to strengthen the alloy. The equi- [4,9,12].
librium phase diagram (Fig. 1b) shows that Mg2Si particles are the The heat treatment of Al–Mg2Si composite can also be effective
primary phase (Mg2Si)P during solidification. Then a-Al and sec- in improving its mechanical properties by homogenizing the
ondary Mg2Si co-solidify from the liquid alloy in the narrow ter- microstructure and better distribution of the alloying elements,
dissolving soluble phases containing Si and Mg formed during
solidification and spheroidizing the eutectic particles [13]. In Al–
⇑ Corresponding author. Tel.: +98 21 8208 4083; fax: +98 21 6111 4083. Si–Mg alloys, dissolution of Mg2Si phase can occur due to the high
E-mail address: [email protected] (M. Emamy). diffusion rate of Mg in Al and also high solution treatment temper-

0261-3069/$ - see front matter Ó 2011 Elsevier Ltd All rights reserved.
doi:10.1016/j.matdes.2011.01.020
2702 A. Malekan et al. / Materials and Design 32 (2011) 2701–2709

Fig. 1. Equilibrium phase diagrams of the (a) ternary Al–Mg–Si and (b) pseudo-binary Al–Mg2Si.

Table 1 This investigation has been carried out to improve tensile prop-
Chemical composition of Al–15%Mg2Si primary ingots (wt.%). erties of the Al–15%Mg2Si composite by solution heat treatment
which is a widespread and also economical process. It should be
Si Mg Fe Cu Mn Cr Ni Zn Ti Al
noted that the treatment temperature and duration depends on
5.87 9.93 0.14 0.03 0.09 0.11 0.02 0.08 0.01 Base
the composition, morphology, size and distribution of different
phases formed after solidification [13].
atures which can be used [4,5]. Several researchers have studied
the behavior of Mg and Al based alloys during solution heat treat- 2. Experimental procedure
ment [14–18], but less work has been carried out on Al–Mg–Si al-
loys with higher Mg and Si contents [3,11]. Therefore, it is of great Starting materials with commercial purity including Al (99.8%),
theoretical and practical significance to investigate the diffusion in Mg (99.9%) and Si (99.5%) were used to prepare the primary ingots
the alloys and the morphology changes of the precipitates during of Al–15%Mg2Si composite. All materials were heated in an electri-
heat treatment. cal resistance furnace using a 10 kg SiC crucible. Table 1 shows the

Fig. 2. Schematic drawing of (a) cast iron mould and (b) tensile sample dimensions.
 A. Malekan et al. / Materials and Design 32 (2011) 2701–2709 2703

Fig. 3. (a) A typical microstructure of as cast Al–15%Mg2Si composite, (b) morphology of primary and (c) pseudo-eutectic Mg2Si.

chemical composition of hypereutectic Al–15%Mg2Si in situ metal was covered during melting period. Degassing was conducted by
matrix composite (MMC). The primary ingots were cut in small using dry tablets containing C2Cl6 powder (0.3 wt.% of the molten
pieces, with the approximate dimensions of 40 mm  30 mm  MMC) by wrapping in an aluminum foil before submerging into
20 mm, appropriate for a 2 kg SiC crucible. Then the cut ingots the melt using a graphite plunger. The melt was degassed for about
were remelted in another electrical resistance furnace. When the 5 min. After stirring and cleaning off the dross, molten MMC was
temperature reached 750 °C, molten MMC was maintained for poured into a cast iron mould. The mould was prepared according
about 15 min. A flux powder was used to ensure the melt surface to B108-03a ASTM standard (Fig. 2a) [19]. The main advantage of

Fig. 4. (a) SEM micrograph of the as cast Al–15%Mg2Si composite, EDX point analysis of (b) primary Mg2Si and (c) a-Al phases.
2704 A. Malekan et al. / Materials and Design 32 (2011) 2701–2709

Fig. 5. SEM micrographs of the samples after the solution treatment at different predetermined temperatures of (a) 300, (b) 400, (c) 500, (d) 550 and (e) 580 °C.

this mould is the application of an appropriate uphill filling system Tensile test bars were machined, according to ASTM B557M-
and feeding design, which results in a rather sound casting. 02a sub-size specimens (Fig. 2b) [20]. Tensile tests were carried
Heat treatment experiments were performed in a high accurate out on a computer controlled MTS tension machine, equipped with
temperature controlled electrical resistance furnace (±2 °C). The a strain gauge extensometer, at a constant cross-head speed of
specimens were solutionized at 300, 350, 400, 450, 500, 550 and 1 mm/min. The fracture surfaces of tensile test specimens were
580 °C for 4 h followed by quenching in cold water. also examined with SEM.
Microstructural studies were made on the polished sample sur-
faces which were selected from the gauge length portion of the test 3. Results and discussion
bars (with 6 mm diameter), as seen in Fig. 2b. The cut sections
were polished and then etched by HF (1%) to reveal the structure. 3.1. Microstructural characterization
The microstructural characteristics of the specimens were exam-
ined by scanning electron microscopy performed in a VegaÓTescan Fig. 3 shows a typical microstructure of an as cast Al–15%Mg2Si
SEM. composite. As seen, the microstructure consists of coarse particles
 A. Malekan et al. / Materials and Design 32 (2011) 2701–2709 2705

Fig. 6. SEM micrographs of specimens, showing morphological changes in secondary Mg2Si particles at (a) 300, (b) 400 and (c) 550 °C.

Fig. 8. Engineering stress vs. elongation at different solution temperature.

Fig. 7. Ultimate tensile strength and elongation percent as a function of solution
temperature.

tectic Mg2Si inside the solidification cell has fibrous morphology as

shown in Fig. 3c [3].
(dark color) of primary Mg2Si and a-Al grains (bright) in a matrix of Fig. 5a–e shows the microstructures of the MMC specimens
Al–Mg2Si eutectic cells [11]. Fig. 4a–c also shows the SEM micro- after solution heat treatment at different solution temperatures.
graphs of the as cast Al–15%Mg2Si composite (Fig. 4a), energy dis- From Fig. 5, it is noticeable that as temperature increases during
persive X-ray (EDX) point analysis of primary Mg2Si (Fig. 4b) and solution treatment, the size of primary Mg2Si does not change con-
a-Al (Fig. 4c), respectively. The presence of a-Al around Mg2Si pri- siderably but its morphology changes to round shape from sharp
mary particles is due to the non-equilibrium solidification of the edges of such coarse particles. As a consequence of the treatment,
subjected alloys which restricts the diffusion rate of Mg and Si into primary Mg2Si particles encountered the solution which proceeds
the surrounding liquid of the Mg2Si particles [21]. The pseudo-eu- by the diffusion of Mg and Si elements into the matrix. It is be-
2706 A. Malekan et al. / Materials and Design 32 (2011) 2701–2709

Fig. 9. SEM back-scattered images of (a) a typical fracture surface of Al–15%Mg2Si composite, (b) decohesioned particles, (c) fractured particles indicating a brittle mode of
failure and (d) dimples with honeycomb appearance.

appearance of the primary Mg2Si phase by increasing solution tem-

perature, heat treatment significantly alters the eutectic Mg2Si
phase to fine dot-like and eutectic network is partially broken, as
shown in Fig. 6 (white circles). Qin et al. have reported similar re-
sults on Al–25Mg2Si–3Si–3Cu–0.5P material after solution and
ageing heat treatment [6]. This reduction is clearly seen in Fig. 6c
(solution treated at 500 °C for 4 h) which shows a more homoge-
neous distribution of secondary Mg2Si intermetallic precipitates.
During solution treatment, it is expected that the low melting
point phases (such as eutectic Mg2Si phase) dissolve into alumi-
num matrix more easily and transforms to fine intermetallics [6].
Further increase in temperature (580 °C) has led to the formation
of porosity in the matrix as a consequence of partial remelting,
as shown in Fig. 5e. Although the working temperature is lower
than that of the eutectic [3], but non-equilibrium conditions of
the experiment may lead to partial remelting. Presence of these
partially remelted regions leads to the formation of the subjected
shrinkage pores which occur during the solidification process. This
in turn can have a detrimental effect on mechanical properties of
the composite as they may act as crack initiation potentials and
cause catastrophic fracture and lower UTS and elongation values.

3.2. Tensile properties and fractography

Fig. 10. Fracture of mixed morphology, cleavage transcrystalline and cellular. The ultimate tensile strength (UTS) and elongation (%) values
obtained from tensile tests of specimens treated at different solu-
tion temperatures are shown in Figs. 7 and 8. As can be seen,
lieved that the solution is preferential at some parts of the particles UTS has been smoothly decreased upon temperature increase up
rather than the others which in turn leads to the changes in the to 550 °C, while further increase in the temperature led to a shar-
morphology of the primary particles of Mg2Si. This is traced by per reduction of the UTS. As mentioned before, the formation of
white circles which captures the primary particles (Fig. 5). shrinkage porosity is the main reason for the observed reduction
Fig. 6a–c also illustrate these phases at higher magnification. It in both UTS and elongation values. Very interesting results
can be seen that although slight changes is seen in the size and obtained from elongation variations with solutionizing tempera-
 A. Malekan et al. / Materials and Design 32 (2011) 2701–2709 2707

Fig. 11. SEM back-scattered images, showing the fracture surfaces of Al–Mg2Si composites with different solution temperature: (a) 300, (b) 400, (c) 500, (d) 550 and (e)
580 °C.

ture, which are presented in Figs. 7 and 8. It is clear that upon tem- Decreasing the risk of brittle fracture in polyphase regions can
perature increment up to 500 °C, the elongation has been increased be realized only by reducing the intensity of the stress-concentra-
significantly to a value of 7.8, while previous studies have shown a tion effect on the Mg2Si particles and by eliminating microregions
maximum value of 2.5 [3,11]. These interesting results confirm the of potential crack initiation sites. The breaking of the Mg2Si precip-
effectiveness of the used solutionizing treatment on the ductility itates network and their spheroidization are very important. This
improvement of the MMC. It is important to note that the cast allows a decrease in the stress-concentration factor value (Kn) in
MMCs basically suffer from lack of ductility [3,11]. An increase in these regions, depending on brittle phase morphology [22,23]:
the strength of soft matrix of a-aluminum solid solution can be
K n ¼ 2a=b ð2Þ
achieved by hardening through point defects, such as substituted
atoms and vacancies or by precipitation hardening with dispersion where a is one-half the length of a particle and b is one-half the
particles of the second phase. width of a particle.
2708 A. Malekan et al. / Materials and Design 32 (2011) 2701–2709

Materials with fine microstructures have lower tendency for low- (1) Upon temperature increment the morphology of both pri-
energy brittle cracking. To obtain acceptable morphology and degree mary and secondary Mg2Si particles was changed with the
of dispersion of the components, one can interfere at the crystalliza- later being more significant.
tion stage by modifying the alloy and by controlling the solidification (2) The ultimate tensile strength decreased gradually up to
behavior and after solidification by heat treatment. 550 °C while further increase in the solutionizing tempera-
Typical fracture surfaces of the Al–15%Mg2Si composite in as-cast ture to 580 °C sharply reduced the UTS value.
condition are shown in Fig. 9. The fracture planes of almost all coarse (3) In contrast to UTS, elongation was greatly improved upon the
Mg2Si particles exhibit clear cleavage characteristic creating a rapid temperature increment while similar to the UTS further
fracture deriving from their intrinsic brittleness and precracked increase in the temperature led to the reduction of elongation.
structure (a). Fig. 9 shows particle decohesion (b), particle cracking (4) Observed increase in the elongation was due to the reduction
(c) and some dimples (d) in the fractured surface of the composite in both potential sites for crack initiation and stress concen-
before heat treatment which suggests cellular fracture surface tration which was due to (1) break up of eutectic network
[24]. It is a type of polyphase material, where the microstructure and (2) softening of sharp corners in primary Mg2Si particles.
components have different mechanical properties. On the cellular (5) According to the tensile results, solution treatment in the
fracture surface, the features of both brittle and ductile fracture are range of 500–550 °C can greatly enhance the properties of
present simultaneously. Fracture of cellular morphology forms in the Al–Mg2Si composite. An optimum temperature of 500 °C
most cases in alloys with modified Mg2Si morphology (in liquid or was found for the solutionizing treatment to have the best
solid state). The Mg2Si precipitates become rounded or fibrous; the influence on the characteristics of the subjected composite.
eutectic network is partially broken. The brittle particles are sur-
rounded by relatively soft matrix and sometimes are isolated. Due
to the strong cohesion at the interfaces between a-aluminum and
Acknowledgements
Mg2Si [24], the matrix is deformed under local active stress (Figs. 9
and 10). The cells form around the Mg2Si-cracked particles by plastic
The authors would like to thank University of Tehran for finan-
deformation of the matrix. The traces of these events are visible as
cial support of this work.
snecks or ligaments on the fracture profile or the high tear ridges
on the fracture surface. In the alloys after solution heat treatment,
the typical ductile fracture mechanism can take place in the matrix, References
as shown in Fig. 11. The mechanism of local decohesion, initiated at
[1] Lu L, Thong KK, Gupta M. Mg-based composite reinforced by Mg2Si. J Comput
a-aluminum/brittle particle interface, is very often composed: voids Sci Technol 2003;63:627–32.
and dimples coalesce on the cell ridges, on both sides of the tear line. [2] Mabuchi M, Higashi K. Strengthening mechanisms of Mg–Si alloys. J Acta
The shear surfaces, plane or with open shear dimples, are formed as a Mater 1996;44:4611.
result of the successive slips in the numerous near slip planes in the [3] Emamy M, Nemati N, Heidarzadeh A. The influence of Cu rich intermetallic
phases on the microstructure, hardness and tensile properties of Al–15%Mg2Si
aluminum crystal lattice. Decohesion at the interface between a- composite. J Mater Sci Eng A 2008;490:250–7.
aluminum and Mg2Si is rather rare, while the secondary cracks in [4] Qin QD, Zhao YG, Xiu K, Zhou W, Liang YH. Microstructure evolution of in-situ
the brittle phases are often observed [24]. Babout et al. proposed a Mg2Si/Al–Si–Cu composite in semisolid remelting processing. J Mater Sci Eng A
2005;407:196–200.
model to simulate the fracture behavior in metal matrix composites [5] Zhang J, Fan Z, Wang YQ, Zhou BL. Microstructural evolution of the in-situ Al–1
suggesting that regardless of the volume fraction of the particles, wt.%Mg2Si composite with extra Si contents. J Scripta Mater 2000;42:1101–6.
interface fracture was strength controlled, and that decohesion oc- [6] Qin QD, Li WX, Zhao KW, Qiu SL, Zhao YG. Effect of modification and aging
treatment on mechanical properties of Mg2Si/Al composite. J Mater Sci Eng A
curred when the average tensile stress in the particles surpassed a 2010;527:2253–7.
critical value known as the interface strength. In in situ composites, [7] Qin QD, Zhao YG, Liang YH, Zhou W. In-situ Mg2Si/Al–Si composite modified by
interface is strong enough and load is transferred to Mg2Si primary K2Ti F6. J Alloys Compd 2005;399:106–9.
[8] Zhao YG, Qin QD, Zhao YQ, Liang YH, Jiang QC. Microstructure of the Ce-
particle and fracture occurs as soon as the threshold stresses is modified in-situ Mg2Si/Al–Si–Cu composite. J Mater Lett 2004;58:2192–4.
reached. However, if the matrix is soft and the interface is weak, dec- [9] Zhao YG, Qin QD, Zhou W, Liang YH. Effects of melt superheating treatment on
ohesion prevails [25]. As mentioned above, it can be summarized microstructure of Mg2Si/Al–Si–Cu composite. J Alloys Compd 2005;399:106–9.
[10] Zhang J, Fan Z, Wang Y, Zhou B. Microstructural refinement in Al–Mg2Si in-situ
that softening of sharp corners in primary Mg2Si particles and break
composites. J Mater Sci Lett 1999;18:783–4.
up of eutectic network (secondary Mg2Si) has led to a decrease in [11] Hadian R, Emamy M, Varahram N, Nemati N. The effect of Li on the tensile
both the stress concentration areas and crack initiation sites. properties of cast Al–Mg2Si metal matrix composite. J Mater Sci Eng A
As seen in Fig. 9, in the as-cast condition, very few dimples on 2008;490:250–7.
[12] Ward PJ, Atkinson HV, Anderson PRG, Elias LG, Garcia B, Kahlen L. Semi-solid
the fracture surface were found to be rather coarse and elongated. processing of novel MMCs based on hypereutectic aluminium–silicon alloys. J
As known, dimples with honeycomb appearance are characteristics Acta Metall 1996;44:1717–27.
of a ductile mode of fracture [24]. The ductile fracture is decided by [13] Sjölander E, Seifeddine S. The heat treatment of Al–Si–Cu–Mg casting alloys. J
Mater Proc Technol 2010;210:1249–59.
the size of dimples, meaning more homogeneous and deeper dim- [14] Rometsch PA, Arnberg L, Zhang DL. Modelling dissolution of MgzSi and
ples producing a higher ductility for the alloys. Fig. 11a–e exhibits homogenisation in Al–Si–Mg casting alloys. J Cast Metal Res 1999;12:1–8.
typical fracture surfaces of Al–Mg2Si composite at different solu- [15] Closset B, Drew RAL, Gruzleski JE. Eutectic silicon shape control by in-situ
measurement of resistivity. J AFS Trans 1986;94:9–16.
tion temperatures. As seen, dimples have increased with increase [16] Shivkumar S, Ricci S, Keller C, Apelian D. Effect of solution treatment
in the solution temperature up to 550 °C and also they have be- parameters on tensile properties of cast aluminum alloys. J Heat Treat
come finer in size. Combination of these reasons arising from solu- 1990;8:63–70.
[17] Zhang DL, Zheng LH, StJohn DH. Effect of a short solution treatment time on
tionizing treatment leads to a change in the mode of fracture from microstructure and mechanical properties of modified Al–7 wt.%Si–0.3
brittle to ductile and increased the elongation. wt.%Mg alloy. J Light Metal 2002;2:27–36.
[18] Lu YZ, Wang QD, Zeng XQ, Zhu YP, Ding WJ. Behavior of Mg–6Al–xSi alloys
during solution heat treatment at 420 °C. J Mater Sci Eng A 2001;301:255–8.
[19] ASTM B557M-02a. Standard methods of tension testing wrought and cast
4. Conclusions aluminum and magnesium alloy products. Annual Book of ASTM Standards,
vol. 02.02; 2003.
The effect of different solutionizing temperatures on the micro- [20] ASTM B108-03a. Standard specification for aluminum-alloy permanent mold
castings. Annual Book of ASTM Standards, vol. 02.02; 2003.
structure and tensile properties of Al–15%Mg2Si composite was [21] Kurz W, Fisher DJ. Fundamentals of solidification. J Trans Tech Publications;
studied. The following conclusions can be drawn: 1998. p. 12.
 A. Malekan et al. / Materials and Design 32 (2011) 2701–2709 2709

[22] Hertzberg RW. Deformation and fracture mechanics of engineering materials. [24] Warmuzek M. Aluminium silicon casting alloys: an atlas of microfractographs.
2nd ed. New York: John Wiley & Sons; 1989. ASM International; 2004.
[23] Jiang D, Wang C. Influence of microstructure on deformation behavior [25] Babout L, Brechet Y, Maire E, Fougeres R. On the competition between particle
and fracture mode of Al–Mg–Si alloys. J Mater Sci Eng A 2003;A352: fracture and particle decohesion in metal matrix composites. J Acta Mater
29–33. 2004;52:4517–25.