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Combining Heat Treatment and High-Pressure Torsion to Enhance the

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Article in Metals · May 2022

DOI: 10.3390/met12050853

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 metals
Article
Combining Heat Treatment and High-Pressure Torsion to
Enhance the Hardness and Corrosion Resistance of A356 Alloy
Mohamed Abdelgawad Gebril 1, *, Mohd Zaidi Omar 2 , Intan Fadhlina Mohamed 2 , Norinsan Kamil Othman 3
and Osama M. Irfan 4,5, *
Citation: Gebril, M.A.; Omar, M.Z.;
Mohamed, I.F.; Othman, N.K.; Irfan,
O.M. Combining Heat Treatment and
High-Pressure Torsion to Enhance the
Hardness and Corrosion Resistance
of A356 Alloy. Metals 2022, 12, 853.
https://doi.org/10.3390/met12050853
Academic Editors: Marta Cabeza
Simo and Babak Shalchi-Amirkhiz
Received: 21 March 2022
Accepted: 12 May 2022
Published: 17 May 2022
Publisher’s Note: MDPI stays neutral
with regard to jurisdictional claims in
published maps and institutional affil-
iations.
Copyright: © 2022 by the authors.
Licensee MDPI, Basel, Switzerland.
This article is an open access article
distributed under the terms and
conditions of the Creative Commons
Attribution (CC BY) license (https://
creativecommons.org/licenses/by/
4.0/).
Metals 2022, 12, 853. https://doi.org/10.3390/met12050853
1 Department of Mechanical Engineering, Faculty of Engineering, Benghazi University, Benghazi 16063, Libya
2 Department of Mechanical and Manufacturing Engineering, Faculty of Engineering and Built Environment,
Universiti Kebangsaan Malaysia, UKM, Bangi 43600, Malaysia; zaidiomar@ukm.edu.my (M.Z.O.);
intanfadhlina@ukm.edu.my (I.F.M.)
3 Department of applied physics, Faculty of Science and Technology, Universiti Kebangsaan Malaysia, UKM,
Bangi 43600, Malaysia; insan@ukm.edu.my
4 Department of Mechanical Engineering, College of Engineering, Qassim University,
Buraydah 51452, Saudi Arabia
5 Mechanical Department, Beni Suef University, Beni Suef 62746, Egypt
* Correspondence: mohamed.almalki@uob.edu.ly (M.A.G.); osamaerfan@qec.edu.sa (O.M.I.);
Tel.: +218-9208-51348 (M.A.G.); +966-556-280-516 (O.M.I.)
Abstract: A356 aluminium alloy is subjected to heat treatment and high-pressure torsion (HPT)
processing to investigate the impact of the combined treatments on the alloy’s microstructure refine-
ment, corrosion resistance and hardness. The high-pressure torsion process was performed at room
temperature for 0.75 and 5 turns. Subjecting the A356 Al alloy to a heat treatment and subsequent
HPT processing produced a more refined microstructure, which has the effect of enhancing the
alloy hardness and corrosion resistance under fragmentation and the homogenous redistribution of
the intermetallic compounds and the Si particles. The results of the treatment show that there is a
marked increase in hardness when imposing a strain from 61 HV to 198 HV on the A356 Al alloy,
which has been HPTed and heat-treated for five turns. The polarisation curves show that there is a
considerable improvement in the corrosion resistance rate of the alloy from 0.043 mm·year−1 for the
A356 Al alloy sample to 0.003 mm·year−1 after five turns of HPT. In this work, the microstructure
refinement resulted in the improvement of both the mechanical strength and corrosion resistance of
the aluminium 356 alloy after heat treatment in comparison to the untreated alloy.
Keywords: A356 Al alloy; HPT; heat treatment; hardness; corrosion resistance
1. Introduction
Aluminium alloys are lightweight materials that are used in the automotive and
aerospace industries instead of cast iron and steel. Because of their desirable properties,
such as excellent castability, high strength, high thermal conductivity, low thermal expan-
sion coefficient and good corrosion resistance, Al-Si cast alloys (300 series) are increasingly
used in the manufacturing of engine components, such as pistons, cylinder heads, engine
blocks and crankcases [1–3]. The cast alloy A356 Al is widely utilised in the manufacture
of automotive powertrain components. For its propensity to improve castability, Si is a
primary alloying element in the A356 Al alloy. However, because of its low solubility in
aluminium, it precipitates as coarse flakes with sharp edges, compromising the alloy’s
mechanical characteristics [1,4–7]. The microstructure of these casting alloys is dominated
by α-Al dendrites surrounded by eutectic Si particles in the form of platelets or flakes, as
well as some intermetallic phases, such as Fe-intermetallic phases, Mg2 Si and Al2 Cu.
The size, distribution and shape of the eutectic mixture components affect the me-
chanical properties of the alloys [8,9]. Within an aluminium matrix, Si and intermetallic
https://www.mdpi.com/journal/metals
Metals 2022, 12, 853 2 of 12

compounds display cathodic behaviour, resulting in the development of micro-galvanic

couples [10–13]. Pitting corrosion resistance can be improved by lowering the area ratio of
Fe-intermetallic compounds and noble Si particles to a less noble Al matrix. In other words,
a lower cathode to anode area ratio (Ac/Aa) lowers the corrosion current density and
makes it easier to produce a protective layer [14,15]. The heat treatment of A356 Al alloy
can be used to modify the eutectic Si particle and the morphology of various intermetal-
lic compounds in order to improve the corrosion resistance by reducing micro-galvanic
action [11,16,17] and increase the strength of the alloy by precipitating Mg2 Si particles [18].
High-pressure torsion has been shown to be one of the most effective severe plastic de-
formation processes for achieving a more refined grain structure in a range of alloys [19–25].
Several studies have shown that the HPT process improves the mechanical properties of
aluminium alloys [26–28], while other have looked into the impact of grain refinement on
the corrosion performance of aluminium alloys [29–35]. However, there is little agreement
on whether the HPT technique can improve the corrosion performance of Al-7Si-3.89Cu-
3Ni [36], Al-Fe system [37] and Al-4 Si wt.% [38].
Furthermore, there is a scarcity of studies on the effects of combining heat treatment
with the refining process and severe plastic deformation. Nguyen et al. [39] investigated
the effect of Al-6wt.% Si to a combination of annealing heat treatment and cooling slope
prior to processing by equal channel angular pressing (ECAP) on the hardness and wear
resistance of the alloy. The hardness of semi-solid cast ECAP samples improved as a result
of the findings. The effect of combining ECAP processing with heat treatment in improving
the corrosion resistance of 6061 Al alloy was investigated by Nejadseyfi et al. [40]. The
results showed that the ECAP process created a shallow and uniform corroded surface.
Natori et al. [41] studied the effect of combining a semi-solid and the ECAP method
on Al-7.14Si-0.4 Mg (wt.%) and the mechanical properties that formed. The research
revealed that combining semi-solid casting with the ECAP process resulted in Si particle
refinement, primary phase grain refinement and a reduction in the hardness difference
between the primary phase and the eutectic phase. Several severe plastic deformation
methods, including as ECAP and accumulative roll bonding [42–45], can be used to refine
microstructures. The T6 heat treatment combined with high pressure torsion (HPT) can
be an effective approach for obtaining highly refined microstructures [40]. However, little
research has been conducted on the interaction of these two processes and, as a result, they
have consequences on microstructure and corrosion resistance.
The effects of T6 heat treatment and subsequent HPT on the microstructure, hardness
and corrosion resistance of A356 Al cast alloy are investigated in this work. This research is
significant because it clarifies the impact of the heat treatment performed to change the form
of flaky silicon particles prior to refinement by using severe plastic deformation processes.

2. Materials and Methods

The material used in this study was a commercial A356 Al-7Si-0.178Ti-0.126Fe-0.149Mg-
0.01Cu-0.006Zn-0.002Mn-0.001Cr (wt.%) with initial ingot dimensions of 80 × 40 × 140 mm
(width–thickness–length). The materials were supplied by Vistec Technology Services Sdn
Bhd in the form of ingots and pieces. The specimens were prepared for T6 treatment, which
was accomplished at 535 ◦ C for 8 h, and then the samples were quenched in water. Fol-
lowing this, the samples were further aged at 180 ◦ C for 3 h [46]. A wire-cutting electrical
discharge machine (EDM) was used to cut the A356 Al alloy samples into rod shapes with
a 10 mm diameter, and the rods were then sliced into disks with a 1 mm thickness. The
applied pressure was 6.0 GPa with a 1 rpm rotation speed in the HPT process, which was
carried out at room temperature for 0.75 and 5 turns. A field emission scanning electron
microscope (FESEM, Zeiss, Oberkochen, Germany), a field emission transmission electron
microscope (FETEM, JEOL, JEM-2100F, Tokyo, Japan) and an optical microscope were used
to study the microstructure of the samples (OM, Olympus Corporation, Tokyo, Japan). A
microhardness tester (Zwick, Germany; ZHV) was used to measure the microhardness
with an applied load of 100 g and a dwell time of 15 s. Indentations were made in the eight
 process, which was carried out at room temperature for 0.75 and 5 turns. A field emission
scanning electron microscope (FESEM, Zeiss, Oberkochen, Germany), a field emission
transmission electron microscope (FETEM, JEOL, JEM-2100F, Tokyo, Japan) and an
Metals 2022, 12, 853 optical microscope were used to study the microstructure of the samples (OM, Olympus 3 of 12
Corporation, Tokyo, Japan). A microhardness tester (Zwick, Germany; ZHV) was used to
measure the microhardness with an applied load of 100 g and a dwell time of 15 s.
Indentations
radial were
directions, made
with eachinindentation
the eight radial
havingdirections, with each
an equal distance fromindentation having
the centre of an
the disk
equal
to distance
the edge from
of the the
disk, ascentre
shownof inthe disk1.toThe
Figure themeasurements
edge of the disk,
wereastaken
shown in Figure
as the average 1.
The
of measurements
three samples perwere
case,taken as the average
and indentations of three
were madesamples per radial
in the eight case, and indentations
directions, with
each
wereindentation
made in thehaving an equal
eight radial distance
directions, from
with theindentation
each centre of the disk to
having anthe edge
equal of the
distance
disk,
from astheshown
centreinofFigure 1. to the edge of the disk, as shown in Figure 1.
the disk

Figure 1. Schematic illustration of the HPT disk and the location of the micrograph, hardness
Figure 1. Schematic illustration of the HPT disk and the location of the micrograph, hardness
measurement
measurement and
and corrosion
corrosionarea.
area.

The as-cast A356 Al alloy samples and HPT disks were ground with a silicon carbide
The as-cast A356 Al alloy samples and HPT disks were ground with a silicon carbide
paper (SiC) with grits ranging from 180 to 1200 before being polished to a mirror-like
paper (SiC) with grits ranging from 180 to 1200 before being polished to a mirror-like
surface with 1 m of diamond paste before being evaluated for microstructure (Al2 O3 ).
surface with 1 m of diamond paste before being evaluated for microstructure (Al2O3). The
The sample was then dipped for 15 s in a Keller solution, rinsed under running water,
sample was then dipped for 15 s in a Keller solution, rinsed under running water, and
and dried by using a blower. The microstructure of the disks was assessed both in the
dried by using a blower. The microstructure of the disks was assessed both in the centre
centre and at the edges. To quantify the grain size, a quantitative metallography study
and at the edges. To quantify the grain size, a quantitative metallography study was
was performed in accordance with ASTM E112. The width and length of the Si particles
performed in accordance with ASTM E112. The width and length of the Si particles were
were measured using the Smart Tiffv2 software, with at least 220 particles considered in
measured using the Smart Tiffv2 software, with at least 220 particles considered in each
each case. The corrosion test was carried out at room temperature with a GAMRY 3.2
case. The corrosion
potentiostat test aerated
in a naturally was carried out atNaCl
3.5 percent room temperature
electrolyte with
solution a GAMRY
in order 3.2
to mimic
potentiostat in a naturally aerated 3.5 percent NaCl electrolyte solution
a seawater environment [11,12]. After approximately 15 min of immersion in 3.5 percent in order to mimic
a seawater
NaCl, environment [11,12].
the potentiodynamic After
test was approximately 15 min of immersion in 3.5 percent
performed.
NaCl, Tothe potentiodynamic
analyse test was performed.
the surface appearance of the sample, immersion tests were carried out for
To analyse the surface
ten days in a 3.5 wt. percent NaCl appearance
naturalof the sample,
aerated immersion
solution. testswas
Each sample were carriedon
adhered out
a
for ten days in a 3.5 wt. percent NaCl natural aerated solution. Each sample
piece of epoxy that had been air-dried for 24 h. Before conducting each corrosion test, the was adhered
on a piece
samples of epoxy
were groundthat hadup
with been air-driedSiC.
to 1200-grit for 24 h. Before conducting each corrosion test,
the samples were ground with up to 1200-grit SiC.
3. Results and Discussion
3. Results
3.1. and Discussion
Microstructure Pre- and Post-Heat Treatment
3.1. Microstructure
Figure 2a depicts Pre- and Post-Heat
optical Treatmentof an A356 Al alloy sample containing a
micrographs
dendritic-shaped primary α-Al phase
Figure 2a depicts optical micrographs surrounded
of anbyA356a coarse eutectic
Al alloy mixture.
sample The den-
containing a
dritic primary grain is approximately 172 µm with a coarse Si particle.
dendritic-shaped primary α-Al phase surrounded by a coarse eutectic mixture. The Figure 2b shows the
enlarged
dendriticmorphology
primary grain ofisaapproximately
flake-like shape with
172 µmsharp
with aedges.
coarseFigure 2c shows
Si particle. Figurethe2bcharac-
shows
teristics of the microstructure after the T6 heat treatment of the
the enlarged morphology of a flake-like shape with sharp edges. Figure 2c shows A356 Al alloy. The flaky
the
Si particles were
characteristics oftransformed into angular-
the microstructure after thetoT6
spherical-shaped
heat treatment of crystals
the A356andAlshowed the
alloy. The
presence of intermetallic
flaky Si particles compoundsinto
were transformed after the application
angular- of the T6 solution
to spherical-shaped heat
crystals andtreatment.
showed
the presence of intermetallic compounds after the application of the T6 solution heat
treatment.
Metals 2022, 12, x FOR PEER REVIEW 4 of 12
Metals 2022,
Metals 2022, 12,
12, 853
x FOR PEER REVIEW 44 of
of 12

Figure 2. Microstructural features of the A356 Al alloy of (a) as-cast, (b) enlargement of eutectic Si
and (c) 2.
Figure eutectic
2. Si after T6.features of the A356 Al alloy of (a) as-cast,
Microstructural as-cast, (b) enlargement
enlargement of eutectic Si
and (c) eutectic Si after T6.
3.2. HPTed Microstructure after 0.75 Turn Pre- and Post-T6
3.2. HPTed Microstructure
3.2. HPTed after
after 0.75 Turn
TurnPre-
Pre-and Post-T6
FigureMicrostructure
3 shows the optical 0.75
micrographs and
of Post-T6
the centre and the edge of the HPTed A356
Figure
Al alloy 33 shows
sample
Figure pre-the
shows optical
andoptical
the post-T6micrographs of
of the
after 0.75 turn.
micrographs the centre
centre and
and the edge of
the edge of the
the HPTed
HPTed A356
A356
Al
Al alloy
alloy sample
sample pre-
pre- and
and post-T6
post-T6 after
after 0.75
0.75 turn.
turn.

Figure 3.
Figure 3. Microstructure of the HPTed
HPTed A356
A356 Al
Al alloy
alloy pre-T6
pre-T6 at
at the
the (a)
(a) centre
centre and
and (b)
(b) edge,
edge, and post
T6 at
Figure(c)
3.centre and (d)
Microstructure the
ofedge
the by 0.75
HPTed turns.
A356
T6 at (c) centre and (d) the edge by 0.75 turns.Al alloy pre-T6 at the (a) centre and (b) edge, and post
T6 at (c) centre and (d) the edge by 0.75 turns.
These images were taken at two two different
different locations:
locations: (a,c) were taken at the centre of
the disk andimages
These were
(b,d) were taken
weretaken close
takenclose to the
to
at two the edge of
edge
different of the disk,
the disk,(a,c)
locations: as shown
as shown in Figure
in Figure
were taken 3. The
3.
at the large
centre of
primary
primary α-Al
α-Al phase
phase grain
grain size
size can be observed
the disk and (b,d) were taken close to the edge of at the centre of the A356 Al alloy
alloy specimen,
specimen,
disk, as shown in Figure 3. The large
while
while the
primary primary
theα-Al phaseα-Al
primary α-Al
grainphase with
size can bethe longitudinal
observed shape of
at the centre canthebeA356
seenAlat alloy
the edge of the
the
specimen,
sample due
while the to applied
primary α-Alstrain.
phaseThe
withsize
theoflongitudinal
the α-Al phase decreases
shape at theatdisk
can be seen the edge
edge under
of the
the imposed
sample due tostrain, as shown
applied in Figure
strain. The size of3a,b. The original
the α-Al large andatcoarse
phase decreases the diskA356
edge Alunder
alloy
Metals 2022, 12, x FOR PEER REVIEW 5 of 12
Metals 2022, 12, 853 5 of 12

the imposed strain, as shown in Figure 3a,b. The original large and coarse A356 Al alloy
primary α-Al
primary α-Alphase
phase and
and lowlow
shearshear
strainstrain imposed
imposed through
through 0.75 turn0.75 turn contribute
contribute to
to retention
retention of the large α-Al phase in the A356 Al alloy sample. The Si
of the large α-Al phase in the A356 Al alloy sample. The Si particles are heterogeneouslyparticles are
heterogeneously
distributed in thedistributed
Al matrix ofinthe
theA356
Al matrix of the
Al alloy. A3563c,d
Figure Al shows
alloy. Figure 3c,d shows the
the microstructure of
microstructure
the of the HPTed
HPTed heat-treated A356heat-treated A356
Al alloy after 0.75Alturn.
alloyThe
after
Si0.75 turn. at
particles ThetheSi edge
particles at
of the
the edge of the
heat-treated heat-treated
A356 A356
Al alloy are Al alloy are heterogeneously
heterogeneously distributed. distributed.

3.3. HPTed Microstructure

Microstructure after
after Five
Five Turns
TurnsPre-
Pre-and
andPost-T6
Post-T6
Figure
Figure 44 shows
showsthethemapping
mappingofofthethecentre and
centre andthethe
edge of the
edge HPTed
of the A356
HPTed Al alloy
A356 pre-
Al alloy
T6 afterafter
pre-T6 five turns. In the
five turns. InHPT processing
the HPT of theofA356
processing Al alloy
the A356 samples,
Al alloy the primary
samples, α-Al
the primary
phase can becan
α-Al phase observed at the centre
be observed at theofcentre
the disk
of as
theshown in Figure
disk as shown4a. in The grain
Figure 4a.boundaries
The grain
of α-Al phase are non-obviously at the edge due to the greater shear resulting
boundaries of α-Al phase are non-obviously at the edge due to the greater shear resulting from the
higher number of turns; this produced the homogeneously and
from the higher number of turns; this produced the homogeneously and uniformly uniformly distributed Si
particles shown in Figure 4b. Figure 4b shows the presence of relatively
distributed Si particles shown in Figure 4b. Figure 4b shows the presence of relatively large eutectic
Si particles
large at Si
eutectic theparticles
edge ofatthethedisk
edgeof of
thethe
A356
diskAl of alloy. The Al
the A356 eutectic
alloy. Si
The particles
eutecticare
Si
homogeneous within the aluminium
particles are homogeneous within thematrix in thematrix
aluminium A356 Al alloy
in the sample.
A356 Thesample.
Al alloy Si particles
The
are fragmented
Si particles into significantly
are fragmented smaller sizes.
into significantly smaller sizes.

Figure 4.
Figure 4. Mapping
Mapping of
of the
the HPTed
HPTed A356
A356 Al
Al alloy
alloy pre-T6
pre-T6 at
at the
the (a)
(a) centre
centreand
and(b)
(b)edge
edgeby
by55turns.
turns.

Figure
Figure 55 shows
showsthe themapping
mappingofofthethecentre
centreand
andedge
edge ofof
the HPTed
the HPTed heat-treated A356
heat-treated Al
A356
alloy sample
Al alloy underunder
sample an applied pressure
an applied of 6.0 GPa
pressure of after five turns.
6.0 GPa The samples
after five turns. Thesubjected
samplesto
the combined
subjected to theheat treatmentheat
combined andtreatment
HPT processandcauses the fragmentation
HPT process causes the of the Si particles
fragmentation of
due toparticles
the Si the high due
strainto imposed
the high on them.
strain The fraction
imposed on them. of small Si particles
The fraction is considerably
of small Si particles
higher, and the microstructure
is considerably higher, and theismicrostructure
more homogeneously
is moredistributed.
homogeneously This isdistributed.
consistent with
This
the findings made by [47]. The eutectic Si particles are more homogenously
is consistent with the findings made by [47]. The eutectic Si particles are more distributed in
the heat-treated samples than in the untreated samples. The edges of the processed
homogenously distributed in the heat-treated samples than in the untreated samples. The samples
have
edgesaoffiner
themicrostructure
processed samples than have
the centre ofmicrostructure
a finer the samples as athanresult
theofcentre
the greater
of thetorsional
samples
strain during
as a result the greater
of the HPT process as shown
torsional in Figure
strain during the5b.
HPT process as shown in Figure 5b.

Figure 5. Mapping of the HPTed

HPTed A356
A356 Al
Al alloy
alloy post-T6
post-T6 at
at the
the (a)
(a) centre
centre and
and (b)
(b) edge
edge by
by 55turns.
turns.

Figure 6 shows the mapping

mapping of the
the Si
Si particles
particles and
and intermetallic
intermetallic compounds at the
centre and the
the edge
edge of
of the
theHPTed
HPTedheat-treated
heat-treatedA356
A356Al Alalloy
alloysample.
sample.TheThe initial
initial flaky
flaky Si
Si particles in the A356 Al alloy sample are no longer present after processing, and the
Metals 2022, 12, x FOR PEER REVIEW 6 of 12
Metals 2022, 12, 853 6 of 12

particles in the A356 Al alloy sample are no longer present after processing, and the
extensive breakage of the Si phases and intermetallic phases can be observed after the T6
heat treatment that was followed by high compression pressure and strain. These results
indicate that the sample subjected to heat treatment before HPT processing has a strong
effect on the size and dispersion of the large silicon
silicon particles
particles after
after processing.
processing.

Figure 6. Mapping of the HPTed heat-treated as-cast A356 Al alloy (a) at the centre and (b) at the
Figure 6. Mapping of the HPTed heat-treated as-cast A356 Al alloy (a) at the centre and (b) at the
edge and
edge and alloying
alloying elements
elements at
at the
the edge
edge (c)
(c) Al,
Al, (d)
(d) Si,
Si, (e)
(e) Mg,
Mg, (f)
(f) Fe,
Fe, (g)
(g) Ti
Ti and
and (h)
(h) Cu,
Cu, after
after 55 turns.
turns.

The imposition of higher strains on the A356 Al alloy during the HPT process via
The imposition of higher strains on the A356 Al alloy during the HPT process via
increased rotational turns causes the breakdown of the intermetallic compounds and the
increased rotational turns causes the breakdown of the intermetallic compounds and the
Si particles in the A356 Al alloy. This process, in consequence, reduces the average of
Si particles in the A356 Al alloy. This process, in consequence, reduces the average of the
the Si particles size and the homogeneous dispersion of the eutectic phase. The T6 heat
Si particles size and the homogeneous dispersion of the eutectic phase. The T6 heat
treatment and the subsequent HPT process produced a more refined Si particle due to the
treatment and the subsequent HPT process produced a more refined Si particle due to the
fragmentation process that occurred during heat treatment as well as to the higher torsional
fragmentation process that occurred during heat treatment as well as to the higher
straining during the HPT process.
torsional straining during the HPT process.
3.4. Hardness of the HPT of the A356 Al Alloy Pre- and Post-T6
3.4. Hardness of the HPT of the A356 Al alloy Pre- and Post-T6
Figure 7 shows the average Vickers microhardness across the diameter of each A356 Al
alloyFigure
sample7pre/post
shows the T6average
via HPTVickers
under 6.0 microhardness
GPa through across
0.75 and the diameter
5 turns. Theof each A356
difference in
Al alloy sample pre/post T6 via HPT under 6.0 GPa through
hardness was determined along the diameter of the disk with a constant 0.5 mm separation 0.75 and 5 turns. The
difference
between each in hardness
processedwas determined
disk. A significant along the diameter
increase of the disk
in the hardness with
of the a constant
A356 Al alloy0.5
is
mm separation between each processed disk. A significant increase
noted after the HPT process, although it should be emphasised that the increase in hardness in the hardness of the
A356
at the Al
edgealloy is noted
of the disk isafter
morethe HPT process,
pronounced thanalthough it should
in the centre. Applyingbe emphasised
the HPT processthat the
to
increase
the A356 in Al hardness at the edge
alloy significantly of the
increases its disk
initialishardness.
more pronounced
The values than in the are
of hardness centre.
low
Applying
in the centre theofHPT process
the disk to the
at the A356 Al
beginning ofalloy significantlybut
the deformation, increases
increase itswith
initialthehardness.
increase
The
in thevalues
applied of strain.
hardness The are low in
variation in the centreis of
hardness the disk upon
dependent at the thebeginning
number ofofturns the
deformation,
and the position but from
increase
the with
centre thetoincrease
the edgeinofthe theapplied strain.
disk. The The variation
increase in hardness in hardness
is more
apparent
is dependent afterupon
5 turns, in contrast
the number to 0.75,
of turns andand theisposition
more apparent
from thethrough
centre tothe thecentre
edge to
of the
edge. The
disk. The increase
figure also in shows
hardness thatisthe
moreedgeapparent
of the disk shows
after a homogeneous
5 turns, in contrast to distribution
0.75, and ofis
hardness
more valuesthrough
apparent after 5 HPT, which
the centre tocauses
the edge.enhanced hardness.
The figure Afterthat
also shows the heat treatment,
the edge of the
brittleshows
disk Si particles were broken
a homogeneous up and turned
distribution into spheroids,
of hardness values which
after 5 made
HPT, themwhichstronger
causes
enhanced hardness. After the heat treatment, brittle Si particles were broken upofand
and harder [48,49]. Moreover, with the increased number of HPT turns, the error bar the
average microhardness for the HPTed heat-treated A356 Al alloy
turned into spheroids, which made them stronger and harder [48,49]. Moreover, with the sample became smaller,
which
increasedindicates
numberthat the microstructural
of HPT turns, the error bar homogeneity
of the averageof the HPTed heat-treated
microhardness A356
for the HPTed
Al alloy samples
heat-treated A356 is further
Al alloy enhanced
samplethroughbecame more HPT revolutions.
smaller, which indicates This outcome
that the is
 Metals2022,
Metals 2022,12,
12,xxFOR
FORPEER
PEERREVIEW
REVIEW 77ofof12
12

Metals 2022, 12, 853 7 of 12

microstructuralhomogeneity
microstructural homogeneityofofthe theHPTed
HPTedheat-treated
heat-treatedA356 A356AlAlalloy
alloysamples
samplesisisfurther
further
enhanced through more HPT revolutions. This
enhanced through more HPT revolutions. This outcome is consistent with theoutcome is consistent with the
consistent with
microstructure the microstructure
observed in Figuresobserved
3–6, in
which Figures
shows 3–6,
thatwhich
the
microstructure observed in Figures 3–6, which shows that the eutectic Si particles and shows
eutectic that
Si the eutectic
particles and
Si particles and
intermetallic
intermetallic intermetallic
compounds
compounds ininthecompounds
the in the sample
sampleprocessed
sample processed through
through processed
55turns
turnsare through
are smaller
smaller 5 and
turns
andmoreare
more
smaller
uniformlyand more uniformly
distributed than distributed
the sample than the
subjected sample
to a subjected
0.75 turn
uniformly distributed than the sample subjected to a 0.75 turn of HPT processing. The of to a
HPT 0.75 turn
processing.of HPTThe
processing.
hardnessofoftheThe hardness
theA356
A356Al of
Alalloy the A356
alloysample Al alloy
sampleincreased sample
increasedafter increased
after0.75
0.75and after
and55turns 0.75
turnsafter and
afterbeing 5 turns
beingsubjectedafter
subjected
hardness
being subjected to heat treatment and the subsequent HPT.inThe increase in be
hardness can
to heat treatment and the subsequent HPT. The increase in hardness can be ascribed toto
to heat treatment and the subsequent HPT. The increase hardness can ascribed
be ascribed to
thefragmentation the
fragmentationand fragmentation
andredistribution and redistribution
redistributionofofboth botheutectic of both
eutecticSiSiand eutectic
andintermetallic Si and
intermetalliccompounds,intermetallic
compounds,the the
the
compounds,
increased the increased
dislocation dislocation
density and density
the grain and the grainresulting
refinement refinement fromresulting
the from
high the
strain
increased dislocation density and the grain refinement resulting from the high strain
high strain
induced induced
during HPTduring HPT processing.
processing. Asmentioned
mentioned Asabove,
mentioned above, a higher number ofin
induced during HPT processing. As above, aahigher
higher number
number ofofrevolutions
revolutions in
revolutions
the HPT in
HPT process the HPT
process generate process generate
generate significant
significant shear significant
shear stress shear stress
stress associated
associated withassociated
with aa high with a high
high dislocation
dislocation
the
dislocation
density,which density,
which which
could could be attributed
beattributed
attributed to grain refinement as inshown in 8Figure 8 and
density, could be totograin
grainrefinement
refinement asshown
as shown Figure
in Figure andgreater
8 and greater
greater microhardness
microhardness [26,47,50–52]. [26,47,50–52].
[26,47,50–52]. The The
The combinedcombined
combined T6 T6
T6 heat heat treatment
heat treatment
treatment and and
and HPT HPT processing
HPT processing
processing
microhardness
resulted
resulted ininthe
the refinement
refinement ofofSiSiparticles.
particles.
resulted in the refinement of Si particles.

250
250
HV
Microhardness,HV

200
200
Microhardness,

150
150
100
100
50
50 A-C,0.75T
0.75T H-T,A-C,0.75T
0.75T
A-C, H-T,A-C,
A-C, 5T
A-C, 5T H-T,A-C, 5T
H-T,A-C, 5T
00
0.5 11 1.5
0.5 1.5 22 2.5
2.5 33 3.5
3.5 44 4.5
4.5 55
Distancefrom
Distance fromcenter,
center,mm
mm
Figure7.7.Microhardness
Figure Microhardnessplotted
plottedagainst
againstdistance
distancefrom
fromthe
thedisk
diskcentre
centreofofthe
theA356
A356Al
Alalloy
alloypre-T6
pre-T6
(A-C) and post-T6 heat treatment (H-T,
treatment (H-T,
(A-C) and post-T6 heat treatment A-C)
(H-T, A-C) after
A-C) after 0.75
after0.75 and
0.75and 5 turns.
and55turns.
turns.

Figure
Figure8. TEM ultrafine
ultrafinegrains
grainsmicrograph
micrographof the
theHPTed
HPTedheat-treated
heat-treatedA356
A356Al
Alalloy
alloysample.
Figure 8.8.TEM
TEMultrafine grains micrograph ofofthe HPTed heat-treated A356 Al alloy sample.
sample.
3.5. Corrosion Resistance of the HPTed A356 Al Alloy
3.5.Corrosion
3.5. CorrosionResistance
Resistanceofofthe
theHPTed
HPTedA356
A356Al
Alalloy
alloy
3.5.1. Surface Morphology
3.5.1.Surface
3.5.1. Surface Morphology
Figure 9 Morphology
shows the top and side view micrograph of the HPTed A356 Al alloy pre-
and post-heat treatment. Figure 9a shows the surface micrograph of the A356 Al alloy
before HPT processing, while Figure 9b shows the surface micrograph of the HPTed A356
Metals 2022, 12, x FOR PEER REVIEW 8 of 12

Metals 2022, 12, 853 Figure 9 shows the top and side view micrograph of the HPTed A356 Al alloy8 pre- of 12
and post-heat treatment. Figure 9a shows the surface micrograph of the A356 Al alloy
before HPT processing, while Figure 9b shows the surface micrograph of the HPTed A356
Al alloy sample
Al alloy sample after
after five
five turns
turns and
and immersion
immersion for for ten
ten days
days inin 3.5%
3.5% NaCl
NaCl solution.
solution. The
The
corrosion
corrosion generally spread along with the eutectic phase as a result of localised corrosion,
generally spread along with the eutectic phase as a result of localised corrosion,
while the silicon
while the siliconparticles
particlesandandα-Al
α-Alinterface
interface were
were notnot affected
affected by the
by the treatment
treatment [53,54].
[53,54]. The
The HPTed heat-treated samples show a smaller size and number
HPTed heat-treated samples show a smaller size and number of pits as well as the of pits as well asarea
the
area around
around thethan
the pits pits those
than those
withinwithin
the A356 the Al
A356
alloyAlsample
alloy sample
and theand HPTthe HPT sample
as-cast as-cast
sample duedistribution
due to the to the distribution of the smaller
of the smaller cathodiccathodic particles
particles afterT6
after the the T6 heat
heat treatment
treatment and
and HPT processing. The presence of an area free of corrosion around
HPT processing. The presence of an area free of corrosion around the pits indicates that the pits indicates
that cathodic
cathodic reaction
reaction occursoccurs
in theincorrosion-free
the corrosion-free area, while
area, while the anodic
the anodic reaction reaction
occurs occurs
within
within the pit due to the concentration of galvanic cells [49,55].
the pit due to the concentration of galvanic cells [49,55]. Figure 9b,d shows that,Figure 9b,d shows
whenthat,
the
when the heat-treated
heat-treated sample istocompared
sample is compared the A356 Al to alloy
the A356
sample,Al the
alloy sample, samples
processed the processed
with a
samples with a higher
higher number of HPTnumber of HPT
turns have a lessturns have
pitting a less pitting
surface. surface.
The higher numberThe higher
of HPTnumber
turns is
of HPT turns
associated withisreduced
associated with reduced
Si-containing Si-containing
particles in the alloy, particles in the alloy,
while a decrease while a
in the cathodic
decrease
area causesin athe cathodic
decrease area
in the causes
anodic a decrease
current density;inthistheeventually
anodic current
results density;
in improvedthis
eventually results in improved
corrosion resistance [56,57]. corrosion resistance [56,57].

Figure 9. Surface appearance of the (a) A356 Al alloy; (b) HPTed heat-treated A356 Al alloy; side
Figure 9. Surface appearance of the (a) A356 Al alloy; (b) HPTed heat-treated A356 Al alloy; side
view of the
view of the (c)
(c) A356
A356 Al
Al alloy
alloy and
and (d)
(d) HPTed
HPTed heat-treated
heat-treated A356
A356 Al
Al alloy
alloy after
after immersion
immersion for
for 10
10 days.
days.

Figure 9c shows the side view of the pitting corrosion sample of the A356 Al alloy. It
Figure 9c shows the side view of the pitting corrosion sample of the A356 Al alloy. It
is worth noting that the enlarged eutectic mixture phase leads to more extensive surface
is worth noting that the enlarged eutectic mixture phase leads to more extensive surface
corrosion of the alloy. This finding indicates that the micro-galvanic cells between the
corrosion of the alloy. This finding indicates that the micro-galvanic cells between the
cathodic high Si and Al matrix may contribute to the development of pitting corrosion in
cathodic high Si and Al matrix may contribute to the development of pitting corrosion in
the high Si particles area. Figure 9c shows the pitting corrosion of the HPTed heat-treated
the high Si particles area. Figure 9c shows the pitting corrosion of the HPTed heat-treated
A356 Al alloy sample after five turns of HPT processing. The difference in the area of
A356 Al alloy sample after five turns of HPT processing. The difference in the area of the
the eutectic mixture phase, the depth of corrosion and the spread of eutectic Si particles
eutectic mixture phase, the depth of corrosion and the spread of eutectic Si particles and
and intermetallic compounds before and after HPT processing between the A356 Al alloy
intermetallic compoundsA356
and HPTed heat-treated beforeAland after
alloy HPT processing
samples enhanced the between the A356
corrosion Al alloy
resistance and
values
HPTed
shown inheat-treated
Figure 9c,d A356 Al alloy
and Table 1. Thesamples
reducedenhanced the corrosion
eutectic phase, as well as resistance values
the redistribution
shown in Figure 9c,d and Table 1. The reduced eutectic phase, as well as the redistribution
and homogeneity of the eutectic phase, contribute to the reduction in the corrosion rate of
and homogeneity
the HPTed combinedof the eutectic
heat phase,
treatment ofcontribute
the A356 Alto the
alloyreduction
sample,in
inthe corrosion
contrast rate of
to those of
the HPTed combined heat treatment of the A356 Al alloy sample, in
the A356 Al alloy before HPT processing. The FESEM and microhardness measurementscontrast to those of
the A356that
indicate Al alloy
there before HPT processing.
is an apparent evolutionThe FESEM
in the and microhardness
microstructure homogeneity measurements
of the A356
indicate
Al alloy samples with higher turn numbers of HPT processing, where the size of Sithe
that there is an apparent evolution in the microstructure homogeneity of A356
particles
Al alloy samples with higher turn numbers of HPT processing, where the
is reduced, the intermetallic particles are broken down and the refined Si and intermetallicsize of Si
particles become more uniformly distributed within the eutectic matrix.
Metals 2022, 12, x FOR PEER REVIEW 9 of 12

Metals 2022, 12, 853 particles is reduced, the intermetallic particles are broken down and the refined Si9 of
and12
intermetallic particles become more uniformly distributed within the eutectic matrix.

3.5.2. Potentiodynamic
3.5.2. Potentiodynamic Test Test
Potentiodynamicpolarization
Potentiodynamic polarizationwas was carried
carried outout to evaluate
to evaluate the impact
the impact of eutectic
of eutectic phase
phase refinement and the microstructure homogeneity resulting
refinement and the microstructure homogeneity resulting from HPT processing on the from HPT processing on
the corrosion resistance of the A356 Al alloy. The electrochemical behaviour
corrosion resistance of the A356 Al alloy. The electrochemical behaviour of the A356 Al alloy of the A356
Al alloy
was was investigated
investigated by exposing bythe
exposing
samplesthe to samples
a corrosive to environment
a corrosive environment at room
at room temperature
temperature
using a 3.5% NaClusing electrolyte
a 3.5% NaCl electrolyte
solution [58]. solution
The Tafel [58]. The Tafel extrapolation
extrapolation method was used method to
was usedthe
measure to rate
measure the ratetoofestablish
of corrosion corrosion thetocorrosion
establish resistance
the corrosion resistance
of both the A356 of both the
Al alloy
A356the
and Alcombination
alloy and the combination
of the heat-treated of A356
the heat-treated
Al alloy and A356 Al alloy and the
the HPT-processed HPT-
(HPTed
processed (HPTed heat-treated) A356 Al alloy samples. Figure
heat-treated) A356 Al alloy samples. Figure 10, which shows the polarization curves of the 10, which shows the
polarization curves of the A356 Al alloy samples before and after
A356 Al alloy samples before and after HPT processing, is used as a basis to compare the HPT processing, is used
as a basisBased
samples. to compare the samples.
on the above curves, Based on the above
the estimated average curves, the estimated
corrosion potentials average
of both
corrosion
samples arepotentials of bothwith
almost similar, samples
only are
minoralmost similar, The
differences. withresults
only minor differences. that
also demonstrate The
results
the lower also demonstrate
corrosion thata the
rate after lower corrosion
combination of the T6 rate
heatafter a combination
treatment and HPTofprocess
the T6 mayheat
treatment
be attributed andtoHPT process may
the modified shapebe of
attributed to the
Si particles modified
after shapetreatment
the T6 heat of Si particles
as well after
as
the
the grain
T6 heatrefinement
treatmentand as redistribution
well as the grainof eutectic
refinementphase andafter HPT processing.
redistribution Thesephase
of eutectic may
be associated
after with a reduced
HPT processing. These maycathodic to anodicwith
be associated ratio.a The 0.0424
reduced mm.year
cathodic to −anodic
1 corrosion
ratio.
rate − 1
The of0.0424
the A356 Al alloy corrosion
mm.year −1 was reduced ratetoof0.00205 mm.year
the A356 Al alloy afterwas
fivereduced
turns of HPT. With
to 0.00205
the fine-grained
mm.year −1 after structure
five turnsofoftheHPT.α-Al and the
With the fine-grained
eutectic phase, as wellof
structure as the
the α-Al
higher and grain
the
boundaries,
eutectic phase, theasconcentration of chloride
well as the higher grain per grain boundary
boundaries, is reduced,oflowering
the concentration chloride the per
current density [59,60].
grain boundary This results
is reduced, in the
lowering theformation
current of a more[59,60].
density stable passive film, which
This results in the
enhances corrosion resistance. The results of this study are consistent
formation of a more stable passive film, which enhances corrosion resistance. The results with those made
by [61–64]. This results in the formation of a more permanent and intact
of this study are consistent with those made by [61–64]. This results in the formation of a passivation coating,
which improves corrosion
more permanent and intact resistance.
passivation coating, which improves corrosion resistance.

Figure 10.
Figure 10. Polarization
Polarization curves
curves of
of the
the A356
A356 Al
Al alloy
alloy(as-cast)
(as-cast)before
beforeand
andafter
afterHPT
HPTprocessing.
processing.

Table1.1.Average
Table Averageofofthe
thecurrent
currentdensity
density(I(Icorr ), corrosion
corr), corrosion rate
rate (CR)
(CR) and
and polarization
polarizationresistance
resistance(Rp).
(Rp).
Samples Ecorr (V) Icorr A/Cm2 Rp (Ω·cm2) Βc (V·dec−
Bc
1) Βa (V·dec−1) CR (mm·year−1)
Ba CR
Samples Ecorr −0.698
(V) Icorr A/cm 2 (Ω·cm
Rp5.212 2
As-cast 3.894 × 10−6 × 10)3 0.642
(V·Dec )− 1 (V0.0504
·Dec−1 ) (mm0.0424
·Year−1 )
As-cast T6, 0.75 turn −0.708 1.021 × 10−6 2.977 × 104 0.421 0.0375 0.012
As-cast −0.698 3.894 × 10−6 5.212 × 103 0.642 0.0504 0.0424
As-cast T6, 5 turns −0.710 2.233 × 10−7 8.870 × 104 0.332 0.0354 0.00295
As-cast T6,
−0.708 1.021 × 10−6 2.977 × 104 0.421 0.0375 0.012
0.75 turn
4. Conclusions
As-cast T6, 5
−0.710 2.233 × 10−7 8.870 × 104 0.332 0.0354 0.00295
turns
Metals 2022, 12, 853 10 of 12

4. Conclusions
In this study, the effect of microstructural refinement on the corrosion resistance and
hardness of the A356 Al alloy processed by a combination of the T6 heat treatment and
HPT processing was investigated. The following conclusions were reached:
1. An ultrafine-microstructure hypoeutectic A356 Al alloy with a homogenous distri-
bution of eutectic intermetallic and Si particles was achieved by combining heat
treatment and HPT processing through five revolutions at room temperature.
2. The hardness of the hypoeutectic A356 Al alloy was significantly improved with the
increasing number of HPT turns.
3. The corrosion resistance of the HPTed heat-treated A356 Al alloy sample was sig-
nificantly enhanced due to the microstructure refinement and redistribution of the
eutectic phase in the Al matrix, which resulted in a reduced galvanic potential differ-
ence. The HPTed A356 Al alloy has the lowest current density 2.233 × 10−7 A/cm2 ,
due to the combination of heat treatment and HPT process. The favourable corrosion
resistance was attributed to the refined microstructure and the redistribution of the
eutectic phase that prevented the occurrences of micro-galvanic cells on the alloy
surface’s protective layer.

Author Contributions: M.A.G. carried out the experimental works, analysis and writing under the
supervision of M.Z.O., I.F.M., N.K.O. and O.M.I. All authors have read and agreed to the published
version of the manuscript.
Funding: The APC was funded by the Deanship of Scientific Research, Qassim University, KSA.
(This work was supported in part by GUP-2018-150 grant under Universiti Kebangsaan Malaysia for
materials processing in Kyushu University, Japan) .
Institutional Review Board Statement: Not applicable.
Informed Consent Statement: Not applicable.
Data Availability Statement: Not applicable.
Acknowledgments: The authors wish to express their gratitude to the Deanship of scientific Re-
search, Qassim University for funding the publication of this work.
Conflicts of Interest: The authors declare no conflict of interest.

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