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IF (2019)=4.

652 Q1/JCR/Scopus/ISI 10 ‫ ردﯾﻒ‬-1 ‫ﺑﻨﺪ‬-3 ‫ﺟﺪول‬


MIF (2019)=1.389 ISSN: 0921-5093
Materials Science & Engineering A 722 (2018) 1–7

Contents lists available at ScienceDirect

Materials Science & Engineering A


journal homepage: www.elsevier.com/locate/msea

The effect of solution treatment time on the microstructure and ductility of T


naturally-aged A383 alloy die castings

G. Eisaabadi B.a, GY Yeomb,c, Murat Tiryakioğlud, , Nelson Nettod, R. Beygia, M.Z. Mehrizia,
SK Kimb
a
Department of Materials Science and Engineering, Faculty of Engineering, Arak University, Arak 38138-5-3945, Iran
b
Korea Institute of Industrial Technology, Incheon 406-840, South Korea
c
Department of Materials Science and Engineering, Inha University, Incheon 402-751, South Korea
d
School of Engineering, University of North Florida, Jacksonville, FL 32256, USA

A R T I C L E I N F O A B S T R A C T

Keywords: A383 aluminum alloy high pressure die castings were solution treated at 490 °C for six duration ranging between
Heat treatment 15 and 180 min, subsequently quenched in water and naturally aged for 4 days. The effects of solution treatment
Homogenization time on the evolution of microstructure and tensile properties were determined. As expected, Si particles became
ADC12 alloy larger and rounder with increasing solution treatment time. In all cases, the size and aspect ratio of the Si
Aspect ratio
particles followed the lognormal distribution. Moreover, the coarsening of Si particles during solution treatment
Coarsening
was found to follow the Lifshitz –Slyozov-Wagner model. A new equation was developed for the evolution of the
aspect ratio during solution treatment of Al-Si-Mg alloys. Analysis of tensile properties showed that elongation
and quality index increased steadily with increasing Si particle size, a result that is in contrast with the widely
accepted notion that large Si particles impairs the ductility of cast Al-Si-Mg alloys. The positive correlation
between Si particle size and quality index was interpreted to be due to partial healing of oxide bifilms entrained
in the castings.

1. Introduction can be used in HPDC components without causing blistering [17,18].


Although the results of solution treatment at lower temperatures are
A383 (ADC12) is one of the most widely used aluminum alloys in promising, the effect of the solution treatment time on microstructure
high-pressure die casting (HPDC) of thin-wall components for auto- and tensile properties of HPDC components has not been undertaken, to
motive applications, due to the combination of its high specific the authors’ knowledge. This study is intended to fill this gap.
strength, high fluidity, high corrosion resistance and low volumetric
shrinkage during solidification [1–10]. Typically, the heat treatment 2. Background
schedule for A383 castings involves a solution treatment [11–16] to
homogenize the solutes, dissolve Al2Cu and Mg2Si to maximize the Tensile deformation of cast Al-Si-Mg(-Cu) alloys has been in-
amount of hardening solutes in the aluminum matrix, and finally vestigated extensively [19–28]. In one of the earlier studies, Gangulee
spheroidize eutectic silicon. Solution treatment needs to be long enough and Gurland [29] observed in situ that Si eutectic particles fractured
to dissolve Mg2Si (β) and Al2Cu particles completely. Simultaneously, early in plastic deformation and intense slip bands appeared between
solution treatment time, tST, should be as short as possible to save en- fractured Si particles, which led to cracks and eventually to final frac-
ergy costs. Moreover, HPDC components usually contain internal pores ture. It has been shown [27,29–31] that the fraction of cracked Si
in which gases such as air, hydrogen and/or vapors formed by the de- particles increases linearly with plastic deformation. Moreover, it was
composition of organic die wall lubricants have been entrapped. The shown [32] that the probability of a Si particle to crack at a given
gases entrapped inside the pores expand during conventional solution plastic strain is related to the product of its equivalent diameter (deq)
treatment i.e., temperature above 500 °C for more than 8 h, and result and its aspect ratio (RA). Hence, the statement by Zhang et al. [33] that
in surface blistering and dimensional instability. Recently, it has been ductility in cast Al-7%Si-Mg alloys is determined by morphology and
demonstrated that solution treatment temperatures lower than 500 °C size of Si particles, is widely accepted in the literature.


Corresponding author.
E-mail address: m.tiryakioglu@unf.edu (M. Tiryakioğlu).

https://doi.org/10.1016/j.msea.2018.02.103
Received 15 February 2018; Received in revised form 27 February 2018; Accepted 28 February 2018
Available online 02 March 2018
0921-5093/ © 2018 Elsevier B.V. All rights reserved.
G. Eisaabadi B. et al. Materials Science & Engineering A 722 (2018) 1–7

Recently Alexopoulos et al. [34] investigated the effect of Cu in


A357 casting alloy produced by the Sophia process, coupled with Sr, Sm
and Ag additions on microstructure and tensile properties. They found a
correlation between mean particle size and mean elongation (eF):
−3.12
eF = 9.48 deq (1)

where elongation is in percent and Si particle size is in microns. Alex-


opoulos also reported an empirical equation for the relationship be-
tween mean elongation and the product of Si particle size and aspect
ratio:

eF = 25.7 (deq RA)−1.47 (2)

Eqs. (1) and (2) provided respectable fits to data, which is in


agreement with previous results in the literature. However, Alex-
opoulos et al. also observed that the Weibull distribution for elongation
in A357-Cu-Sr castings was bimodal although the lognormal distribu-
tion for Si particle size was unimodal. Consequently, they concluded
that the strong correlations between elongation and Si particle size and
shape were probably incidental and did not indicate causation.
The as-cast microstructure in Al-Si-Cu-Mg alloys has a profound
effect on the response of the alloy to solution treatment [35]: while only
several minutes are necessary to complete dissolution and homo-
genization in fine microstructures [36–39], several hours are necessary
for coarser microstructures. In a study on A356 aluminum alloy, Shiv-
kumar et al. [40] investigated the effect of solution treatment time at
540 °C on the tensile properties of sand and permanent mold castings.
Fig. 1. (a) 3D representation of die cavity illustrating the orientation of the excised
The solution treatment time varied between 25 and 800 min for per-
specimens, and (b) casting produced by HPDC machine. (c) Dimension of tensile speci-
manent mold castings and between 50 and 1600 min for sand castings. mens.
They found that with solution treatment time, Si eutectic particles got
rounder and coarsened and tensile ductility increased even though yield
were produced by using a TOSHIBA cold chamber die casting machine
strength (σY) either remained essentially the same or even increased.
without applying any vacuum to the die cavities. The chill-vent (la-
These results were later confirmed in another study by Shivkumar et al.
byrinth extension) on top of each plate was designed to increase the
[41]. Similar observations about the beneficial effects of prolonged
soundness of the castings. The casting and HPDC machine parameters
solution treatment time on ductility were made by Drouzy et al. [22]
are listed in Table 2.
and Tiryakioğlu [42]. Pan et al. [43] observed that both yield strength
Castings were solution treated at 490 °C [15] for 15, 30, 60, 90, 120
and tensile strength (ST) of A357 alloy castings initially increased, then
and 180 min in an air circulating furnace and were subsequently
decreased with increasing solution treatment time while elongation
quenched in water at 25 °C. Specimens were naturally aged for four
increased steadily in almost every dataset. Highest strength values
days at room temperature. Tensile test specimens were machined ac-
corresponded to the Si morphology obtained at the end of spher-
cording to ASTM B557M-10. The dimensions of the tensile specimens
oidization and in the early stages of particle coarsening. These results
are provided in Fig. 1.c. Four tensile test specimens were prepared for
are in contrast with those of Meyer [44] who found that all tensile
each solution treatment time. Microstructural changes were examined
properties of A357 alloy castings increased with solution time, despite
on polished surfaces of metallographic specimens obtained from the as-
significant coarsening of Si particles during solution treatment. The
cast and solution-treated test bars. The specimens were chemically
beneficial effects on tensile properties, especially ductility, despite
etched using Keller's reagent. A Nikon Eclipse MA 200 optical micro-
coarser Si particles after solution treatment are in contrast with the
scope, a FEI Quanta 200F FE-SEM equipped with EDS and Image-Pro
findings that larger Si particles fracture at lower strains and therefore
Plus software were used to characterize the microstructure of the
reduce elongation. The present study is motivated by this contrast in
samples.
the literature.

3. Experimental details 4. Results and discussion

The chemical composition of the recycled A383 alloy used in the The as-cast microstructure is presented in Fig. 2 which shows that
study, as determined by optical emission spectrometry, is provided in the Si phase has a coral structure. Image analysis of the as-cast micro-
Table 1. The alloy was received as five kg ingots, which were then structure revealed that the average diameter of α-Al dendrites was
melted at 750 °C in an electric furnace. Even though no Sr was added to
the melt, residual Sr was in the melt (0.015 wt%) because the alloy was Table 2
recycled. The melt was subsequently held at 680 °C in a holder. Plates Casting and HPDC machine parameters.

with the dimensions of 65 mm × 120 mm× 3 mm, as shown in Fig. 1, Parameter Level

Table 1 Pouring temperature 690 ± 10 °C


Chemical composition of the alloy used in this study. Mold temperature 120 °C
Clamping force 350 ton
Element Si Fe Cu Mn Mg Ni Zn Ti Al Plunger Diameter 50 mm
Initial speed 0.23 m/s
wt% 11.83 0.827 2.365 0.169 0.255 0.054 0.516 0.028 Bal Injection speed 3.74 m/s

2
G. Eisaabadi B. et al. Materials Science & Engineering A 722 (2018) 1–7

3
d3 − d 0 = k∙t ST (5)
where d is the average diameter, d 0 is the initial diameter, k is a tem-
perature dependent constant and tST is solution treatment time. By
using the equivalent diameter averages in Table 3 and taking as-cast
size as the initial diameter, LSW coarsening model was fitted to ex-
perimental data. Results are presented in Fig. 5, which shows that the
change in the volume of particles with solution treatment time becomes
linear after 30 min, consistent with the LSW model.
The change in average aspect ratio of Si particles, given in Table 3,
with solution treatment time is presented in Fig. 6. The best fit curve,
indicated in Fig. 6, has the following form:
n
t
RA = RA0 − (RA0 − RAL) ∙exp ⎡−⎛ ST ⎞ ⎤
⎜ ⎟
⎢ ⎝ t0 ⎠ ⎥ (6)
⎣ ⎦
where RA0 is the aspect ratio of the as-cast condition, RAL is the aspect
ratio limit, t0 is the time constant and n is the exponent. The fit as
shown in Fig. 6 with RAL = 1.69, t0 = 65 min, n = 1.35, has a coeffi-
cient of determination, R2, of 0.999, which implies an almost perfect fit
Fig. 2. The as-cast microstructure showing coral-like Si eutectic phase.
to the data. To the authors’ knowledge, Eq. (6) is the first equation
developed for the evolution of aspect ratio with solution treatment
time.
12.4 µm. It is noteworthy that there was no primary Si particles, most The change in tensile properties with solution treatment time is
probably due to the residual Sr in the melt [45], which inhibits het- presented in Fig. 7. Note that there is a drop in tensile and yield
erogeneous nucleation of Si on inclusions, such as oxide bifilms. strengths after a solution treatment of 90 min. The exact reason for this
The evolution of the size and shape of Si particles during solution drop is unknown. It can be speculated that the natural aging time of
treatment is presented in Fig. 3. The coral structure observed in the as- four days may not have been sufficient to develop a steady strength
cast condition transformed rapidly to fine and fibrous particles in so- level after 90 min of solution treatment. Also note that elongation in-
lution treated samples. Si particles became larger and more spherical creases with solution treatment time even for times less than 90 min.
with increasing solution treatment time, which is consistent with pre- To evaluate whether solution treatment time has any effect on the
vious results [16,46–49]. It is also noteworthy that no blisters were structural quality, the quality index proposed by Tiryakioǧlu et al.
observed in the solution treated specimens. [57–59] for Al-7%Si-Mg alloys was used:
Micrographs were analyzed digitally to determine the size and as-
eF
pect ratio of each Si particle. The size and aspect ratio of Si particles QT =
were shown [16] to follow the lognormal distribution, the density β0 − β1σY (7)
function (f) for which is written as; where β0 and β1 are 36.0 and 0.064 MPa −1
for Al-7%Si-Mg alloys, re-
spectively. Tensile properties presented in Fig. 7 were converted to the
1 −(ln(x − τ)−μ)2
f(x) = exp ⎡ ⎤ quality index values by using Eq. (7). The results are shown in Fig. 8.
(x − τ)σ 2π ⎢
⎣ 2σ 2 ⎥
⎦ (3) Note that the trend in the structural quality is the same as in elongation;
where τ is the threshold, σ is the shape parameter and μ is the scale solution treatment, even for low durations, increases the structural
quality of A383 alloy die castings. The magnitude of this beneficial
parameter. Therefore, lognormal distributions were fitted to the data by
using the maximum likelihood method. The estimated parameters for effect increases with solution treatment time. This result is consistent
with the finding in previous studies [22,40–44].
the lognormal distributions for Si particle size and aspect ratio are given
in Table 3. Note that the threshold, τ, for equivalent diameter fits are Possible correlations between quality index and Si particle size and
aspect ratio are also investigated. The results are presented in Fig. 9.
zero, effectively reducing Eq. (3) to a two-parameter lognormal dis-
tribution. Results of the Anderson-Darling [50] goodness-of-fit tests The correlation between average equivalent diameter of Si particles and
quality index is shown in Fig. 9.a. The structural quality of the castings
showed that lognormal distributions in Table 3 could not be rejected.
increases with larger Si particles, which can be anticipated from the
The lognormal distributions for the size of Si particles plotted by
discussion above and previous results in the literature [22,40–44].
using Eq. (3) and the estimated parameters in Table 3 are presented in
However, when Eq. (1) is plotted in Fig. 9.a after converting elongation
Fig. 4.a. Note that the distributions shift right to larger Si particle sizes
to QT values for the A357 alloy used by Alexopoulos et al. (indicated
with increasing solution treatment time. The lognormal distributions
with dashed lines), the two correlations are opposite of each other.
for aspect ratio of Si particles are presented in Fig. 4.b. The peaks of the
Hence as an improvement in structural quality can be expected with
distributions shift to lower aspect ratio values with increasing solution
larger Si particles due to coarsening during solution treatment, the
treatment time.
same increase in average Si particle size will produce a significant re-
The average of a three-parameter lognormal distribution, x , is found
duction in structural quality, as in insufficient or no modification
by;
[32,34]. The contrast between the two correlations is remarkable. It is
σ2 well known that correlation between two variables does not necessarily
x = τ + exp ⎡μ+ ⎤ mean causation [60]. Hence, the ductility (and therefore the structural

⎣ 2⎦ ⎥ (4)
quality) of cast Al-Si-Mg(-Cu) alloys is determined by factors other than
The estimated averages of the lognormal distributions are also Si particles size, as suggested by Alexopoulos et al. [34] and Tiryakioğlu
provided in Table 3. et al. [57]. Consequently, it can be stated that the intrinsic effect of Si
The coarsening of Si particles during solution treatment of Al-Si particle size is not known at this point. A similar conclusion can be
alloys was investigated in several studies [16,51–54] and was found to made about the product of Si particle size and aspect ratio, as presented
follow the coarsening model developed by Lifshitz and Slyozov [55] in Fig. 9.b. The trend in change in QT is similar to the one in Fig. 9.a; QT
and Wagner [56] (LSW): increases with increasing the product of Si particle and aspect ratio.

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G. Eisaabadi B. et al. Materials Science & Engineering A 722 (2018) 1–7

Fig. 3. The evolution of microstructure with solution treatment time: (a) 15, (b) 30, (c) 60, (d) 90, (e) 120, and (f) 180 min.

This trend is the reverse of what would be expected from the literature; performance of cast Al-Si-Mg alloys are determined mainly by extrinsic
the probability of fracture of Si particles is related to deq. RA [32], and if factors, namely oxide bifilms that get entrained into the melt during
the elongation of cast Al-Si alloys is determined by the fractured Si mold filling and/or melt processing. Therefore, it is extremely chal-
particles as suggested by Zhang et al. [33], then an increase in deq. RA lenging to determine the intrinsic effects of processing variables such as
should reduce ductility, as shown by the dashed lines for the data of solution treatment time and/or microstructural factors such as particle
Alexopoulos et al. The reverse trend reported in the present study is also size and aspect ratio on mechanical properties in the presence of the
consistent with the results of Shivkumar et al. for the A356 alloy [40]. strong effect of oxide bifilms, masking the true effect of the micro-
Recent research [61,62] showed that the mechanical properties and structure. This challenge has been demonstrated by the trends in the

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G. Eisaabadi B. et al. Materials Science & Engineering A 722 (2018) 1–7

Table 3
Estimated parameters of the lognormal distributions for the size and shape of the Si particles.

As cast 15 min 30 min 60 min 90 min 120 min 180 min

deq τ (μm) 0 0 0 0 0 0 0
μ −0.8572 −0.3032 0.2027 0.3501 0.5347 0.6155 0.6926
σ 0.6189 0.4278 0.6714 0.5556 0.3485 0.3971 0.4167
x (μm) 0.5139 0.8092 1.5343 1.6561 1.8138 2.0024 2.1802
RA τ 0.8887 0.9089 0.8470 0.9187 0.9398 0.9678 0.9946
μ 0.0993 −0.0520 −0.0201 −0.3149 −0.3649 −0.5269 −0.7493
σ 0.7405 0.8238 0.7619 0.8350 0.7115 0.7427 0.9007
x 2.3414 2.2418 2.1572 1.9530 1.8340 1.7457 1.7038

Fig. 5. The change in the size of Si particles with solution treatment time.

Fig. 6. The change in the average aspect ratio of the Si particles with solution treatment
Fig. 4. (a) Si size and (b) aspect ratio distributions for as cast and all solution treatment
time.
times investigated in this study.

bifilms, which have been shown [65] to act as heterogeneous nuclea-


quality index with Si particle size found in this study, that are the op-
tion sites for Si particles.
posite of those found in an investigation on the effect of modifying
Although correlations between QT and the two Si particle para-
additions. The increase in the quality index of the A383 castings found
meters in Fig. 9.a and b reported in this study is the opposite of those
in this study can be attributed to the healing of bifilm defects with
found by Alexopoulos et al., the results of the two studies are re-
solution treatment. Although coarse “old” bifilms coming from the melt
markably consistent when QT is plotted as a function of aspect ratio, as
are resistant to healing [63,64], “young” bifilms that are created during
presented in Fig. 9.c. The best fit curve to the data is also shown in the
mold filling can be healed. Therefore, the positive correlation between
figure. The consistency between the two studies may be due to the true
Si particle size and quality index is not because of the coarsening of Si
underlying effect but more research is needed to validate it.
particles but as a result of oxide bifilms healing with longer solution
treatment times. It can also be stated that the true relationship between
Si particle size and ductility is not completely known. Research is 5. Conclusions
needed to determine the exact relationship in the absence of oxide
The present study aimed to investigate the effect of solution

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G. Eisaabadi B. et al. Materials Science & Engineering A 722 (2018) 1–7

Fig. 7. The change in tensile properties with solution treatment time.

Fig. 8. The effect of solution treatment time on the quality index, QT.

treatment time on the microstructure, tensile properties and structural


quality of the AlDC12 alloy high pressure die castings. Microstructural
evolution was assessed by digital image analysis of the micrographs
obtained from the samples solution treated from 15 to 180 min.
Analysis of microstructural data showed that (i) Si particles got larger in
size and rounder with increasing solution treatment time, (ii) size and
aspect ratio of the Si particles followed the lognormal distribution for
each solution treatment condition, (iii) Si particles coarsened during
solution treatment according to the LSW model. Moreover, a new
equation was proposed for the evolution of the aspect ratio of the Si
particles with solution treatment time:
n
t
RA = RA0 − (RA0 − RAL) ∙exp ⎡−⎛ ST ⎞ ⎤ ⎜ ⎟
⎢ ⎝ t0 ⎠ ⎥
⎣ ⎦

that yielded an R2 value of 0.999, which implies an almost perfect fit to


the data.
Analysis of tensile properties revealed that with increasing of the Fig. 9. The change in the quality index with (a) average size of Si particles, (b) the
solution treatment time, the yield strength and tensile strength of the product of mean size and aspect ratio of Si particles, and (c) aspect ratio of Si particles.
alloy remained essentially unchanged but elongation increased. To
evaluate the effect of solution treatment time on the structural quality conclusions can also be made about the product of Si particle size and
of the alloy, the tensile data were converted to the quality index. Result aspect ratio, a parameter used in the literature to measure the prob-
of these analysis showed a positive correlation between quality index ability of cracking of a Si particle. It is the authors’ opinion that it is
with the size of Si particles. This result is in contrast to several studies in impossible to evaluate the intrinsic effect of the size and aspect ratio of
which a negative correlation between the two was reported. Therefore, the Si particles on tensile properties of cast Al-Si-Mg alloys in the pre-
the ductility (and therefore the structural quality) of cast Al-Si-Mg(-Cu) sence of oxide bifilms. The positive influence of solution treatment on
alloys is determined by factors different from Si particles size. Similar

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G. Eisaabadi B. et al. Materials Science & Engineering A 722 (2018) 1–7

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