Journal of Alloys and Compounds 683 (2016) 485e494

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Journal of Alloys and Compounds

journal homepage: http://www.elsevier.com/locate/jalcom

Effect of solution time in T6 heat treatment on microstructure and

hardness of a directionally solidified AleSieCu alloy

rcio G. Gomes b, Ota
Thiago A. Costa a, Marcelino Dias a, Lae
vio L. Rocha b,
Amauri Garcia a, *
a
Department of Manufacturing and Materials Engineering, University of Campinas, UNICAMP, 13083-860 Campinas, SP, Brazil
b
, IFPA, 66093-020 Bel

Federal Institute of Education, Science and Technology of Para em, PA, Brazil

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

Article history: An experimental investigation on the role of solution time during the T6 heat treatment on the scale of
Received 1 April 2016 the secondary dendrite arm spacing (l2), morphology and distribution of Si particles and Al2Cu in-
Accepted 10 May 2016 termetallics and the resulting effect on microhardness of Al-5.5 wt%Si-3.0 wt%Cu alloy samples is per-
Available online 13 May 2016
formed. A directionally solidified (DS) casting was previously obtained using a water-cooled apparatus,
which permitted a wide range of cooling rates (T)_ to be associated with samples having quite different
Keywords:
microstructural parametric features. An experimental growth law relating l2 to T_ is proposed. The T6
AleSieCu alloy
heat treatment was then carried out on the DS samples for different solution times: 8 h and 5 h at
Solidification
Heat treatment
490 ± 2
C, followed by quenching in warm water (60 ± 2
C), ageing for 5 h at 155 ± 2
C and air-cooling.
Microstructure The microstructure characterization (optical and scanning electron microscopies) has shown that l2 was
Hardness only affected (when compared with those of the DS casting samples) when the solution time increased
from 5 h to 8 h. In contrast, significant influences on the morphology and distribution of both Si and
Al2Cu particles are shown to occur. The highest hardness is shown to be associated with a sample
subjected to the 5 h treatment, having lowest l2 and appropriate modification of Si and Al2Cu particles.
© 2016 Elsevier B.V. All rights reserved.

1. Introduction manufacture of components such as cylinders, pistons, engine

Aluminum alloys have properties of great industrial interest,
such as: low density, good corrosion resistance, high thermal and
electrical conductivity, good combinations of mechanical proper-
ties, good workability in machining processes and mechanical
forming [1e19]. These alloys can be divided into two groups. One
contains those alloys for which the mechanical properties are
controlled by work hardening and annealing. Commercial purity
aluminum and alloys of the AleMg and AleMn systems are com-
mon examples [7]. The second group comprises alloys such as
AleCueMg, AleMgeSi, AleCueSi and AleZneMgeCu that respond
to age or precipitation hardening [7,20].
Particularly AleCueSi alloys of the ANSI series 319.1 and 333.1
(in which compositions lie mostly within the ranges 5.5e10 Si and
3.0e4.0% Cu) are extremely important considering their applica-
bility in the automotive and aeronautics industries, in the
* Corresponding author.
E-mail address: amaurig@fem.unicamp.br (A. Garcia).
blocks, etc. Their main characteristics are good castability and
strength at relatively high temperatures, low coefficient of thermal
expansion and good wear resistance [3,5e7,21e24]. In general, the
AleSieCu alloys are used for many of the applications listed for the
binary alloys but where higher strength is needed [3,5e7,21,22].
Increasing demands on such properties have pointed to the need
for close microstructural control through tighter specification of
composition, casting practice, and subsequent heat treatment.
In unmodified AleSi alloys, the Si particles have a plate-like
morphology, which can act as crack initiators and have negative
influence on ductility [3]. The ductility can be improved by
changing the morphology of the Si particles towards a more fibrous
form. This can be done using high cooling rates (T) _ during casting,
by addition of a chemical modifier, by exposing the casting to high
temperature for long periods (heat treatments), or by a combina-
tion of these processes [3e7,21,22,25]. For instance, the magnitude
of cooling rate during solidification of Al-(Si, Cu) alloys, determines
the fineness of the microstructure and other microstructural fea-
tures such as fraction, size and distribution of intermetallic phases
and segregation profiles of solute in the interdendritic regions

http://dx.doi.org/10.1016/j.jallcom.2016.05.099
0925-8388/© 2016 Elsevier B.V. All rights reserved.
486 T.A. Costa et al. / Journal of Alloys and Compounds 683 (2016) 485e494

Fig. 1. Macrostructure of the DS casting and experimental solidification cooling-rate along the length of the casting: P is the position from the cooled surface of the casting. R2 is the
coefficient of determination.

[3,5,6]. Large and brittle intermetallic phases can be formed during
slow solidification, with deleterious effects to the mechanical
properties. Increased cooling rates result in finer microstructures
and improved mechanical properties [1,2,8e15].
The literature presents both theoretical and experimental
studies focusing on the microstructural evolution of binary
aluminum-based alloys. Experimental and theoretical laws of
cellular and dendritic growth have been proposed and duly vali-
dated [7e19]. It has been shown that the dendrite arm spacing is
proportional to (T)_ n where n ¼ 1/2 and 1/3 for the primary and
secondary dendritic arm spacings, respectively. In contrast, this
kind of study on multicomponent alloys are scarce in the literature
[2,12,24].
Heat treatments of aluminum alloys are used with a view to
improving the mechanical strength by the well-known precipita-
tion-hardening mechanism, which occur during appropriate heat-
ing and subsequent cooling. The improvement in mechanical
properties depends upon the change in solubility of the alloying
constituents with temperature [1e7,21e24]. The T6 heat treatment,
consists of [5,6]: (i) solution heat treatment of as-cast samples for
dissolution of certain intermetallic phases such as Al2Cu and for
changing the morphology of the eutectic silicon; (ii) quenching,
usually to room temperature, to obtain a supersaturated solid
solution, and (iii) age hardening: to cause precipitation from the
supersaturated solid solution either at room temperature (natural
ageing) or at an elevated temperature (artificial ageing).
The aim of the present study is to evaluate the role of the so-
lution time during the T6 heat treatment of samples having quite
different dendritic scales, extracted from a directionally solidified
Al-5.5 wt%Si-3.0 wt%Cu alloy casting, considering the secondary
dendritic arm spacing, morphology and distribution of Si particles
and the final effect on microhardness.
2. Experimental procedure
The casting assembly used in the directional solidification
experiment has been detailed in a previous article [10]. This so-
lidification set-up was designed in such way that heat was
extracted only through the water-cooled bottom, promoting ver-
tical upward directional solidification.
The directional solidification experiment was carried out with
an Al-5.5 wt% Si 3.0 wt% Cuealloy, which was prepared using
commercially pure metals: Al (99.72 wt% containing 0.08 wt% Fe),
Cu (99.92 wt%) and Si (99.68 wt%). During the solidification process,
cooling curves at different positions along the length of the DS
casting were measured by fine type K thermocouples and the data
 T.A. Costa et al. / Journal of Alloys and Compounds 683 (2016) 485e494
Fig. 2. Experimental secondary dendrite arm spacing (l2) as a function of: (a) position
P from the cooled bottom of the casting for as-cast and heat treated samples and (b)
solidification cooling rate along the length of the casting. R2 is the coefficient of
determination.
were acquired automatically. These thermocouples were sheathed
in 1.6 mm diameter steel tubes, and positioned in the casting at 5,
10, 15, 20, 30, 50 e 70 mm from the heat-extracting surface.
The directionally solidified (DS) casting was sectioned along its
longitudinal direction, i.e. parallel to the direction of solidification,
mechanically polished with abrasive papers and subsequently
etched with an acid solution composed of 5 mL H2O, 60 mL HCl,
30 mL HNO3 and 5 mL HF to reveal the macrostructure. In order for
characterize and quantify the dendritic structure, selected longi-
tudinal sections of the DS casting were polished and etched with an
acid solution (NaOH 5%) for microstructural analysis. The secondary
dendrite arm spacing was measured by averaging the distance
between adjacent side branches on longitudinal sections of pri-
mary dendrite stalks [10,11].
The T6 heat treatment, which was performed according to the
methodology proposed in the literature [6], consisted of:
a) solution heat treatment for 8 h and 5 h at 490 ± 2
C;
b) quenching in warm water (60 ± 2
C);
c) immediate ageing for 5 h at 155 ± 2
C;
d) air cooling.
The time for heating the samples to the solution treatment
temperature was 20e30 min and was excluded from the presented
487
times. In order to evaluate the effect of solution time on the scale of
the secondary dendrite arm spacing and microhardness, two
different solution times were used: 8 h and 5 h. These times were
sufficiently long to ensure complete dissolution of the alloying el-
ements and of the Al2Cueintermetallic phase into the Al-matrix.
After this treatment, the samples were removed from the furnace
and immediately subjected to water quenching.
Microhardness tests were conducted in each sample using a
300 g load and a dwell time of 10 s. The adopted Vickers micro-
hardness values are the average of at least 20 different measure-
ments on the transverse section of each sample.
3. Results and discussion
3.1. Macrostructure, cooling rate and dendritic spacing
The typical macrostructure of the Al-5.5%Si-3.0%Cu alloy DS
casting is shown in Fig. 1. It can be observed that the water-cooled
mold imposes higher values of cooling rate close to the casting
cooled bottom and a decreasing profile along the casting length,
and remains essentially constant for positions P > 50 mm, as shown
in Fig. 1. From this position, the microstructure is very little affected
by the cooling rate, and this has defined the casting range from
which samples were extracted to be subjected to the T6 heat
treatment.
Measurements were made of the secondary dendrite arm
spacing (l2) on samples extracted from specific positions (5, 10, 15,
20, 25, 30, 40 e 50 mm) from the cooled bottom of the DS casting,
for both as-cast and heat treated samples, as set out in Fig. 2a. It is
observed that l2 increases with the distance from the heat-
extracting surface of the AleCueSi alloy DS casting, and that the
l2 profile has only been slightly affected (it tends to increase
marginally) when the samples were subjected to the T6 treatment
for a solution time of 5 h. However, it can be noted that l2 increases
when the solution time is increased from 5 to 8 h. It seems that the
8 h solution time has been enough to initiate the process of
coarsening of dendrite arms. It is worth noting that the samples
subjected to the T6 heat-treatment had been solidified in a water-
cooled mold, and consequently have relatively low dendrite arm
spacings (relatively low diffusion length). Experimental power laws
(Fig. 2a) correlate l2 as a function of position from where the
samples were extracted from the DS casting for both as-cast and
heat treated samples, i.e.: l2 ¼ constant(P)0.54.
In order to correlate l2 with a solidification thermal parameter,
the solidification cooling rate, (T), _ was determined by considering
the thermal data recorded immediately after the passage of the
liquidus front by each thermocouple. The l2 results are plotted as a
function of T_ in Fig. 2b, where average values with the standard
variation are presented, with the lines representing an experi-
mental power function fit to the experimental points. It is observed
that the use of a water-cooled mold imposes higher values of
cooling rates near the cooled surface of the casting and a decreasing
profile toward the casting top due to the increasing thermal resis-
tance of the solidified shell (according to Fig. 2b solidification
cooling rates from 1 to 30
C/s). It can be seen that the experimental
growth law is characterized by a power function relating l2 toT_
given by l2 ¼ 41(T) _ 1/3. This is in agreement with experimental
results reported by Rocha et al. [10], Peres et al. [23] and more
recently by Costa et al. [24], in which l2 has been reported to vary
with T_ according to power functions having a 1/3 exponent, that
is, l2 a T_ 1/3, along the transient solidification of hypoeutectic
AleCu and AleSi alloys and an Al-6wt%Cu-4wt%Si alloys.
488 T.A. Costa et al. / Journal of Alloys and Compounds 683 (2016) 485e494
Fig. 3. Typical optical microstructures at P ¼ 15 mm: (a) as cast, l2 ¼ 18 mm; (b) and (c) T6-heat treated for solution times of 5 h, l2 ¼ 20 mm and 8 h, l2 ¼ 26 mm, respectively.
3.2. Microstructure features: as-cast and heat-treated samples vs.
position in casting
Fig. 3 presents typical microstructures of longitudinal section of
samples at 15 mm from the bottom of the casting in the following
conditions: as-cast and solution treated for 5 and 8 h, respectively.
It can be seen in the as-cast sample that Si particles in the inter-
dendritic regions have a plate-like morphology and that after the
T6 heat treatment the morphology changed to a mixture of fibers
and spheroids. It can also be noted an increase in size of fibers and
spheroids when the solution time is increased from 5 to 8 h (Fig. 3b
and c).
In order to permit the change in silicon morphology and dis-
tribution upon coarsening during the T6 treatment to be investi-
gated, including the effect of increasing solution time, a more
detailed analysis of the optical microstructures of each sample has
been carried out using an image processing software (Image J). The
area fractions of the Si particles have been determined for each
sample associated with the 7 different positions examined in the DS
casting, based on a dimensionless shape factor (the circularity: C) of
the Si particles, which is defined by a relation between the area of
the particle surface (S) and its perimeter (C ¼ 4pS/P2) [26]. C varies
from 1 for a perfect circle, decreasing up to zero with the increase in
the complexity of the morphology of the Si particles. These area
fractions were determined by computing the light and dark areas in
the corresponding optical micrographs, as shown in Figs. 4 and 5 for
solution times of 5 h and 8 h, respectively, and for samples of po-
sition P ¼ 5 mm and P ¼ 50 mm from the cooled surface of the DS
castings. These samples solidified at maximum and minimum
cooling rates, respectively, of all samples experimentally examined.
In Figs. 4 and 5 the original microstructures can be seen compared
with areas analysed by the software and associated with C varying
between 0 and 0.5 (areas with particles assumed to have a fiber-like
morphology); 0.5e0.7 (areas with particles with shapes with
characteristics of both morphologies) and 0.7e1.0 (areas with
spheroidized particles).
Fig. 4. Examples of distinct Si morphologies as determined by an image processing software and microstructure area fractions of each Si morphology as a function of position (P)
from which the samples were extracted from the DS casting: T6-heat treated for solution time of 5 h.
Fig. 5. Examples of distinct Si morphologies as determined by an image processing software and microstructure area fractions of each Si morphology as a function of position (P)
from which the samples were extracted from the DS casting: T6-heat treated for solution time of 8 h.
 T.A. Costa et al. / Journal of Alloys and Compounds 683 (2016) 485e494
Fig. 6. Effect of solution time on area fractions of spheroidized and fiber-like particles
of samples from different positions along the length of the DS casting.
As depicted in Fig. 6, the plots of area fractions (AF) of particles
as a function of position in the DS casting from where the samples
were extracted, shows increase and decrease in AF with increasing
P for fibers and spheroids, respectively, for both 5 h and 8 h solution
times. The AF for particles having a mixed morphology remained
essentially constant with P at AF about 2% and decreased from
about 4% to 2.5% for solution times of 5 h and 8 h, respectively. The
samples from positions closer to the casting surface have also lower
dendritic spacings (Fig. 2) and hence lower diffusion length, which
491
favour not only the spheroidization process but also the coales-
cence of spheroids during the T6 treatment. However, a comparison
of AF evolution with P for particles of similar morphologies,
depicted in Fig. 6, shows decrease and increase in AF of Si fibers and
Si spheroids, respectively, with the increase in solution time (which
favours the diffusion process). It can also be seen that the AF of
spheroidized particles exhibit a similar trend for the two initial
positions experimentally analysed, i.e., the two positions having the
lowest dendritic spacings of all samples examined.
The literature reports that the result of dissolution and ho-
mogenization processes depends on the coarseness of the micro-
structure, the type of diffusing elements and the stability of phases
in combination with the temperature and time used along the heat
treatment [3,5,6]. In the case of non-ferrous alloys, the secondary
dendrite arm spacing is often used as a measure of the coarseness
of the microstructure and the scale of l2 is known to influence the
time needed for dissolution and homogenization [3]. The Al2Cu
phase is the main Cu-containing phase in the as-cast AleCueSi
samples, as can be observed in Fig. 7a. Associating the results of
Fig. 7a with the microstructures shown in Fig. 8, it can be seen that
the scale of l2 (~10 a 35 mm) obtained in this work in the as-cast
condition was sufficient to achieve the complete dissolution of
Al2Cu into the Al-rich matrix for both solution times of 8 h and
5 h at 490
C. Sjo
€ lander [3] reported that for three samples of an as-
cast AleCueSi alloy, which were submitted to solution heat treat-
ment, and having l2 values equal 10, 25 and 50 mm, respectively, a
solution time about 30e40 min at 495
C was enough for the
complete dissolution and homogenization of Al2Cu intermetallics
into the Al-rich matrix for the sample having the finest micro-
structure (10 mm), while more than 10 h were needed for the
coarsest microstructure (50 mm).
Iron-containing phases are only present in low fractions in the
alloy investigated, induced by the low Fe concentration that is al-
ways present in commercially pure Al and these phases were not
dissolved by the T6 heat treatment conditions used in the present
study. It can be noted by the solidification path, calculated by using
a computational thermodynamics software and shown in Fig. 7b
and c, that these Fe particles are stable at 490
C, which was the
solution temperature used in the present investigation. Fig. 8a and
b depict detailed images of the microstructures of heat-treated
samples obtained by SEM-EDS mapping, in which Fe intermetallic
particles can be observed. Undissolved Fe intermetallic phases were
also reported in studies conducted by Sjo € lander [3] and Mohamed
et al. [5], who applied the T6 heat treatment to an AleSi alloy
containing Cu and Mg as alloying elements.
3.3. The effect of microstructural features on hardness
The microhardness profile along the DS casting length (as-cast
condition) is shown in Fig. 9, compared with those corresponding
to results obtained after subjecting the samples extracted from
different positions to the T6 heat treatment. It can be seen that
hardness increases of about 15% from the as-cast samples to those
heat-treated using a solution time of 5 h. It is worth noting that for
both conditions the dendritic spacing, for each position, is essen-
tially the same (see Fig. 2a). This indicates that the increase in
hardness for the heat-treated samples is associated with the
complete dissolution of the Al2Cu phase into the Al-rich dendritic
matrix. However, the samples that were heat-treated using a so-
lution time of 8 h exhibit a decrease in hardness with the increase
in position. These samples were shown to have also a complete
dissolution of the Al2Cu particles into the alloy matrix, however, the
dendritic spacings are higher when compared with those of sam-
ples of the two other conditions (as-cast and solution treated for
5 h), as shown in Fig. 2a. Moreover, as shown in Fig. 9 the change in
492 T.A. Costa et al. / Journal of Alloys and Compounds 683 (2016) 485e494

Fig. 7. SEM micrograph (backscattered electron image) at P ¼ 30 mm: (a) as-cast, l2 ¼ 25 mm, (b) Solidification path and (c) zoom of the temperature region where Si and Fe phases
are formed during solidification of the Al-3.0 wt%Cu-5.5 wt%Si-0.08 wt%Fe alloy.

morphology of Si particles with the position P of each sample Bi solder alloys reported a sudden increase in tensile strength
examined, and coarsening of such particles are also affecting the associated with the extensive presence of tertiary dendritic
decrease in hardness for samples subjected to 8 h of solution branches that developed from the secondary branches [29].
treatment. As reported in the literature for hypoeutectic AleCu
alloys, the increase in l2 is associated with decrease in mechanical
4. Conclusions
strength [9]. This seems to be only one of the factors affecting
hardness results of the samples that were subjected to a solution
Experiments were conducted in order to analyze the effect of
treatment for 8 h in the present study. Additionally to the above-
solution time during the T6 heat treatment on microstructure and
mentioned factors related to the Si particles, by analyzing the
microhardness of a directionally solidified Al-5.5 wt% Si-3.0 wt% Cu
samples microstructure, a collapse of tertiary dendritic arms can
alloy. The following major conclusions can be drawn from the
been noted for the 8 h/treated samples. This makes the dendritic
present study:
network less complex, which seems also to affect hardness. Some
recent studies highlighted the differences in mechanical properties
 The dendritic growth of the alloy was shown to be characterized
for directionally solidified castings after the onset of tertiary den-
by an experimental power function relating l2 to T_ given by
dritic branches. Studies on SneAgeCu solder alloys reported that _ 1/3; l2 [mm] and T[
_
C/s]. It was shown that the profile
l2 ¼ 41(T)
the more complex microstructure that resulted after the onset of
of secondary dendrite arm spacing values obtained along the
tertiary dendritic branches allowed the intermetallic compounds to
length of the DS casting, increased only when the solution time
be more homogeneously distributed throughout the interdendritic
adopted in the T6 heat treatment was increased from 5 to 8 h.
regions increasing the tensile strength [27] and positively affecting
 The microstructure in the as-cast samples was shown to be
the resulting hardness [28]. An investigation correlating tensile
characterized by an Al-rich dendritic matrix with Si particles
properties and microstructural interphase spacing of a Sn-52 wt%
disseminated into the interdendritic regions having a plate-like
 T.A. Costa et al. / Journal of Alloys and Compounds 683 (2016) 485e494
Fig. 8. SEM micrographs and microanalysis at P ¼ 30 mm with solution time: (a) 8 h,
l2 ¼ 42 mm/backscattered electron image and (b) 5 h, l2 ¼ 27.7 mm/secondary electron
image.
morphology, which after the T6 heat treatment changed to a
mixture of fibers and spheroids.
 Solution times of 8 h and 5 h at 490
C were shown to be enough
to achieve the complete dissolution of Al2Cu in the Al-rich
matrix. On the other hand, stable iron-intermetallic phases
have been found in the interdendritic regions after the T6 heat
treatment.
 It was shown that hardness increased of about 15% from the as-
cast samples to those heat-treated using a solution time of 5 h,
493
Fig. 9. Microhardness as a function of position in casting for the as-cast and heat
treated samples. R2 is the coefficient of determination.
and this has been attributed to the complete dissolution of Al2Cu
particles in the Al-rich matrix, since the dendritic spacings of
samples in both conditions were quite similar. The samples that
were heat-treated using a solution time of 8 h exhibited a
decrease in hardness when compared with the hardness of
those that were subjected to a solution time of 5 h. This was
shown to be associated with the corresponding increase in the
dendritic arm spacing, coarsening of Si particles and collapse of
tertiary dendritic arms that makes the dendritic network less
complex.
Acknowledgements
The authors acknowledge the financial support provided by IFPA

),
(Federal Institute of Education, Science and Technology of Para
FAPESP e S~ ao Paulo Research Foundation, Brazil (grants 2013/
09267-0; 2013/23396-7 and 2014/50502-5) and CNPq (The Brazil-
ian Research Council).
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