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Journal of Alloys and Compounds 648 (2015) 912e918

Contents lists available at ScienceDirect

Journal of Alloys and Compounds


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

Combining equal-channel angular pressing and heat treatment to


obtain enhanced corrosion resistance in 6061 aluminum alloy
Omid Nejadsey a, *, Ali Shokuhfar a, Amirreza Dabiri b, Amin Azimi a
a
Advanced Materials and Nanotechnology Research Center, Department of Mechanical Engineering, K.N. Toosi University of Technology,
Tehran 19395-1999, Iran
b
Abadan Faculty of Petroleum Engineering, Petroleum University of Technology, Abadan, Iran

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

Article history: The corrosion behavior of 6061 aluminum alloy processed by heat treatment and equal-channel angular
Received 24 March 2015 pressing (ECAP) is investigated. Current transient, potentiodynamic polarization and electrochemical
Received in revised form impedance spectroscopy are used to assess the corrosion resistance of 6061 aluminum alloy in different
22 May 2015
processing conditions. The results conrm that the peak-aged sample after two ECAP passes and
Accepted 27 May 2015
Available online 10 June 2015
annealed sample after four ECAP passes are the most resistant samples against corrosion. Using ECAP
leads to substantial increase in the dislocation density, re-distribution of precipitates, crystallite
renement, alteration of the surface area of the cathodic sites, and increase in the volume fraction of
Keywords:
Corrosion
grain boundaries that affects corrosion resistance. Assessment of the corroded surfaces of the materials
Electrochemical impedance spectroscopy shows that some coarse-grains are corroded selectively in the annealed sample leading to formation of
Metals and alloys deep and large pits on the sample surface. However, after ECAP, shallow and uniform corroded surface is
Potentiodynamic polarization observed that is in agreement with the corrosion diagrams.
Scanning electron microscopy 2015 Elsevier B.V. All rights reserved.
Transmission electron microscopy

1. Introduction different materials after SPD is also investigated. Darmiani et al.


[10] studied the corrosion behavior of AleSiC nano-composite,
One of the main characteristics of aluminum alloys is excellent produced by accumulative roll bonding (ARB). They showed that
corrosion resistance that makes them suitable to be widely used in increasing the ARB cycles led to a decrease in the number of pits
automotive, aerospace, and marine industry. A wide range of heat and an increase in the pitting corrosion resistance. Nie et al. [11]
treatments are also available for aluminum alloys that make it investigated the corrosion behavior of commercial purity tita-
possible to tailor their properties to t specic applications. In nium processed by high-pressure torsion (HPT). They stated that
addition, development of severe plastic deformation (SPD) there is a complicated relation between grain renement and
methods to produce nanostructured (NS) and ultrane-grained corrosion resistance, due to contradictory effects of inhomoge-
(UFG) materials makes it possible to control the microstructure neous microstructure and grain size reduction. Zheng et al. [12]
and properties of heat treatable aluminum alloys. ECAP is one of the investigated the effects of microstructural changes during ECAP
most used SPD processes that induces simple shear deformation to on the corrosion behavior of 304 stainless steel. They reported that
the samples without any cross-sectional change and due to the the corrosion resistance of the samples improved after ECAP due to
constancy of the cross-sectional area of the billet, the process is increase in the stability of the passive lm on 304 stainless steel
repeatable in further passes [1,2]. though the thickness and composition of the passive lms on the
Recently, researchers have widely investigated the strength, as-received and 8-pass samples were very similar. Miyamoto et al.
toughness, wear, and fatigue properties of the samples processed [13] studied the corrosion behavior of copper with and without
by SPD methods [3e9]. More recently, the corrosion resistance of processing by ECAP in a modied Livingstone etchant. Their study
revealed that UFG copper exhibited remarkably lower corrosion
current in comparison with that in the coarse-grained (CG) coun-
terpart. Jiang et al. [14] reported the enhanced corrosion resistance
* Corresponding author. of hypereutectic AleSi alloy subjected to ECAP. They found that in
E-mail addresses: o.nejadsey@sina.kntu.ac.ir, o.nejadsey@gmail.com
(O. Nejadsey), Shokuhfar@kntu.ac.ir (A. Shokuhfar).
UFG structure, the easier formation of an oxide layer with an

http://dx.doi.org/10.1016/j.jallcom.2015.05.177
0925-8388/ 2015 Elsevier B.V. All rights reserved.
O. Nejadsey et al. / Journal of Alloys and Compounds 648 (2015) 912e918 913

improved adhesion force and protection efcacy improved the sinusoidal AC voltage of 10 mV amplitude. Subsequently, poten-
corrosion behavior. tiodynamic polarization was carried out in the range of 1.2
Several other investigations have been performed to investigate to 0.2 V at a scan rate of 0.25 mVs1. The analysis of current
the inuence of SPD on the corrosion behavior of different mate- transients was another method used to assess the mechanisms of
rials. Akiyama et al. [15] reported improvement of corrosion localized corrosion at a constant voltage, the variation of current
resistance of the AleNi alloy by ECAP, Hosseini et al. [16] investi- density was recorded during 1200s. This test was used to analyze
gated the effects of grain size and texture on the corrosion behavior pit initiation and re-passivation processes in different samples. All
of commercial purity titanium processed by ECAP, and Vra tna et al. tests were repeated at least three times in order to maintain a high
[17] reported enhanced corrosion resistance in AZ31 magnesium statistical accuracy.
alloy processed by ECAP. In addition, Shi et al. [18] studied the effect XRD analysis was performed using Cu Ka radiation
of Sc and Zr addition on the corrosion behavior of AleZneMgeCu (l 0.15406 nm) at a voltage and electrical current of 40 kV and
alloys, Canakci et al. [19] assessed the inuence of milling time in 30 mA, respectively. The XRD patterns were recorded in the 2q
mechanical alloying on the formation of a protective coating layer, range of 0e100 . Corroded surfaces were investigated using scan-
and Hockauf et al. [20] stated that the solid-solution heat treated ning electron microscopy (SEM) to observe the microscopic fea-
6082 aluminum alloy combined with post-ECAP aging showed tures of corrosion in each case. Optical microscopy (OM) and high-
excellent corrosion resistance. resolution transmission electron microscopy (HR-TEM) were also
In this study, corrosion behavior of 6061 aluminum alloy pro- used in order to obtain the microstructure of the processed mate-
cessed by a combination of heat treatment and ECAP is investigated rials before and after ECAP.
to reveal the simultaneous effects of grain renement and heat
treatment on corrosion resistance. In order to compare the results, 3. Results
the tests were performed in four processing conditions and the
inuence of heat treatment, severe plastic deformation, and a 3.1. Current transient test results
combination of heat treatment and severe plastic deformation are
discussed. The results of different corrosion tests on the annealed Fig. 1 shows the graphs of the current density versus immersion
material were used as the reference case. The aim is to address the time for the samples of four groups where the magnitude of the
individual and combined effects of heat treatment and ECAP on voltage remained constant. The variation of electrode current with
corrosion resistance of 6061 aluminum alloy. The information ob- immersion time is depicted to investigate the pit initiation and
tained from these analyses can be used to address failure reasons repassivation processes. In all samples, the current magnitude is
due to corrosion and propose an appropriate method for materials increased during the initial stages of immersion. However, after
processing to promote corrosion resistance. about 200s, the current values remain almost stable with very little
uctuation. It is shown that the highest current is obtained for
annealed sample showing the lowest pitting corrosion resistance
2. Experimental procedure
for this sample. After processing the annealed sample by ECAP, the
current values are decreased showing improved pitting corrosion
Four groups of cylindrical billets with a diameter of 10 mm and a
resistance. The heat-treated sample also shows an improved pitting
length of 60 mm were machined from an ingot of aluminum alloy
corrosion resistance compared to the annealed sample. However,
6061. The composition of this alloy is presented in Table 1. All billets
one ECAP pass on the annealed specimen seems to be more effec-
were initially annealed in 686 K for ve hours. The billets of rst
tive in improving the pitting corrosion resistance than peak aging
group, named as group A, were kept in the annealed condition (O
(T6 heat treatment). It is also shown that the pitting corrosion
temper). The billets of the second group, named as group B, were
resistance for both annealed and peak-aged samples after two ECAP
solution heat treated and articially aged to achieve the T6 temper.
passes is very similar and the annealed specimen after four ECAP
Solution heat treatment was performed by heating the billets to the
passes is the most resistant sample against pitting corrosion.
super-saturated condition at around 800 K for 30 min followed by
Nevertheless, the formation of the protective layer in the peak-aged
rapid quenching in cold water. Articial aging was also performed
sample after two ECAP passes is immediate after immersion, while
at 433 K for 18 h. Third group contained the billets of O temper,
the oxide layer in the annealed sample after four ECAP passes needs
which were pressed using an ECAP die by route C up to four passes.
more time to be formed.
(Group C). The last group contained the billets in T6 condition that
Careful inspection of these curves conrms that after 200s, there
were ECA pressed up to two passes using route C. A split die with an
is gradual increase in the current value for the annealed and peak-
internal angle of 90 and an arc of curvature of 20 was imple-
mented to conduct ECAP at room temperature. MOS2 was used as
lubricant in order to reduce friction [21]. Punch speed was chosen
to be 5 mms-1.
Prior to corrosion tests, small disks were prepared from the
center of each billet and were polished using SiC papers and pol-
ishing powders. Electrochemical measurement was performed at
room temperature for each specimen in a solution containing 3.5%
NaCl. A reference electrode of Ag/AgCl was used for electrochemical
impedance spectroscopy (EIS) using an auxiliary electrode of plat-
inum. The frequency range was from 105 to 102 Hz using

Table 1
Composition of the Al6061 Alloy in weight percentage.

Al Mg Si Fe Cu Mn

Base 0.807 0.669 0.627 0.23 0.12


Fig. 1. Current density versus immersion time at a constant voltage.
914 O. Nejadsey et al. / Journal of Alloys and Compounds 648 (2015) 912e918

aged samples. However, for the ECA pressed samples the current
becomes more stable during higher immersion times. This phe-
nomenon suggests that the annealed and heat-treated samples
need more immersing time to form a protective passive lm, which
indicates that pitting occurs gradually. This observation can be
related to the quick dissolution of the oxide lm in the aggressive
solution. However, the current density remains almost constant in
the samples processed by ECAP. Although practical information can
be obtained from these curves, other electrochemical tests are still
needed to accurately judge the corrosion resistance of different
samples.

3.2. Potentiodynamic polarization Fig. 3. Corrosion current and potential extracted from potentiodynamic polarization
diagrams.
Determining corrosion rate and evaluation of corrosion prop-
erties is usually performed by potentiodynamic polarization test.
Fig. 2 illustrates the polarization curves for the samples of each against corrosion. Peak aging leads to a gradual improvement in the
group. Corrosion current and potential extracted from potentio- corrosion resistance of aluminum alloy. However, one ECAP pass is
dynamic polarization diagrams is also illustrated in Fig. 3. It is more effective in improvement of the corrosion resistance than
shown that the corrosion current of the annealed specimen after peak aging. These observations accompany the obtained results in
ECAP is more than that of the unprocessed specimen. A reverse the current transients. It is notable that the corrosion resistance of
trend is observed for the peak-aged sample before and after ECAP. both annealed and peak-aged specimens increases when the
Complex passive corrosion behavior in NaCl solution is observed in number of passes are increased. However, the peak-aged sample
both annealed and peak-aged samples. The corrosion current obtains exceptional corrosion resistance after two ECAP passes.
density and corrosion potential are evaluated using the Tafel slope This observation could be directly related to the microstructural
tting from the polarization curves and the corrosion rates are evolution, distribution, size and volume fraction of the precipitates
included in Table 2 and Fig. 3. For the annealed sample, the [20].
corrosion rate is increased after processing by ECAP. In addition, Fig. 5 shows X-Ray diffraction (XRD) patterns for the samples of
heat treatment leads to increase in the corrosion rate. However, four groups. The constituting phases and the relative amount of
these modications are very narrow in the polarization curves and these phases could be distinguished by comparing the ratio of the
actually preceding cathodic reaction on the sample surface may intensities. Therefore, it is notable that the relative amount of AlFeSi
compromise the accuracy of the obtained results [11]. Therefore, it phase increases after heat treatment. This observation conrms the
is suggested to use the EIS technique, which is more sensitive in increase in corrosion resistance after heat treatment compared
characterizing the corrosion behavior of the materials of different with that of the annealed sample. As expected, processing by ECAP
groups accurately. reduces the size of precipitations and leads to a uniform distribu-
tion of the second phase particles [22,23]. The induced strain, grain
renement mechanism and induction of high amount of disloca-
3.3. Electrochemical impedance spectroscopy
tion density are almost identical in both annealed and peak-aged
samples after ECAP. The peak broadening in all cases shows that
Although polarization curves have been used widely for corro-
the average crystallite size of the soft and hard phases decreases
sion analysis, preceding cathodic reaction on the sample surface
after two ECAP passes. However, signicant difference between the
may compromise the accuracy of the obtained results. Therefore, it
corrosion behavior of annealed and peak-aged samples after two
is better to use EIS technique to characterize the electrochemical
ECAP passes may arise from the presence of the ne second phase
interface between electrodes and electrolytes, which is more sen-
particles with a uniform distribution in the aluminum matrix. It is
sitive. Fig. 4 shows representative Nyquist plots obtained for
also notable the inuence of the presence of ne second phase
different samples in 3.5% NaCl solution. The results show that,
particles and their uniform distribution is more effective than
increasing the number ECAP passes leads to increase in the corro-
repeating ECAP and gradual conversion of low angle grain bound-
sion resistance. The annealed sample has the lowest resistance
aries to high angle grain boundaries. In other words, the corrosion
resistance of the peak-aged sample after two ECAP passes is even
higher than that of the annealed sample after four ECAP passes.

3.4. Microstructure and corroded surface

In the previous sections, the results of different corrosion tests


were presented. This section aims to clearly represent the under-
lying mechanisms in the corrosion. Fig. 6 illustrates the micro-
structure of the annealed specimen before and after ECAP. As
shown in this gure, the average grain size is reduced from 20 to
30 mm to below 500 nm after only two ECAP passes. In addition to
that, a high number of dislocations and sub-grain boundaries that
appear as dark lines in Fig. 6b are easily detectable. A high dislo-
cation density together with rened grains is the main reason that
improves corrosion resistance of the sample. In addition, Fig. 5
Fig. 2. Potentiodynamic polarization curves for different samples. showed the constitutive phases and their relative amount before
O. Nejadsey et al. / Journal of Alloys and Compounds 648 (2015) 912e918 915

Table 2
Data extracted from potentiodynamic polarization diagrams.

Sample Ecorr/V Icorr/A cm2 ba/V dec1 bc/V dec1 Rp/ohm Vcorr/mm y1

Anneal 0.623 8.588  107 0.688 0.014 3.284  103 1.009  102
Anneal 2Passes 0.696 3.133  106 0.278 0.014 3.433  102 3.680  102
Anneal 4Passes 0.680 6.613  106 0.778 0.015 4.989  102 7.767  102
Peak age 0.707 3.446  106 0.428 0.021 7.312  102 4.048  102
Peak age 2Passes 0.728 3.723  107 0.166 0.018 2.264  103 4.384  103

and after precipitation hardening and ECAP. Fig. 7 depicts the


corroded surfaces of the samples of each group to show how the
microstructural features affect the pitting on the samples during
the test.
For the annealed sample (Fig. 7a), there are a lot of local envi-
ronmental attacks. Large and deep pits are easily detectable in this
case. After peak aging, these local environmental attacks reduce,
but the size and depth of the pits remain relatively large (Fig. 7b).
Most of the sample surface remained intact, while there are se-
lective corrosion areas on the surface. Both annealed and peak-aged
sample after two ECAP passes show relatively small pits as shown
in Fig. 7c and d. Nevertheless, they are well-distributed in the peak-
aged sample. This might have originated from the uniform distri-
bution of the second phase particles. Finally, the annealed sample
after four ECAP passes represents shallow and uniformly corroded
surface (Fig. 7e).
Fig. 4. Electrochemical impedance spectroscopy diagrams for different samples. Selective corrosion of grains can be attributed to the differences
in the crystallographic orientations of specic grains. When some
coarse-grains are corroded selectively, deep and large pits are
formed on the sample surface. That is why in the annealed sample
deeper and larger pits are detectable than the other samples. A
closer inspection of the pits in Fig. 8 conrms the presence of
abundant and deeper corrosion pits on the corroded surface of the
annealed sample in which the grain size is more than 40 times
bigger than that of the annealed sample after two ECAP passes.
Fig. 9 shows the EDS analysis of point A and B shown in Fig. 7. As
shown in this gure, the concentration of Na and Cl around the pit
is detectable. The Mg element is totally solved on point B. However,
the formation of oxide layer on point B protects the surface and the
major alloying elements are retained.

4. Discussion

The graphs of the current densities versus immersion time for


the samples of four groups in a constant voltage are shown in Fig. 1.
These curves showed that there was gradual increase in the current
value for the annealed and peak-aged sample. Aluminum alloys
Fig. 5. X-ray diffraction (XRD) patterns.
exhibit relatively good corrosion resistance due to spontaneous
formation of an oxide lm in an atmospheric environment.

Fig. 6. The microstructure of (a) annealed specimen and (b) annealed specimen after two ECAP passes using route C.
916 O. Nejadsey et al. / Journal of Alloys and Compounds 648 (2015) 912e918

Fig. 7. Corroded surfaces of (a) annealed specimen, (b) peak-aged sample, (c) annealed specimen after two ECAP passes using route C, (d) peak-aged sample after two ECAP passes
using route C, and (e) annealed specimen after four ECAP passes using route C.

Fig. 8. Three dimensional images from the corroded surfaces of (a) annealed specimen, 1500, and (b) annealed specimen after two ECAP passes, 1500X (To view this image
correctly, the reader is recommended to refer to the web version of the article and to wear a passive 3-D red-cyan glasses.).

However, they are prone to pitting corrosion mainly in chloride- leads to gradual increase in current value. However, for the ECA
rich solutions in which the oxide lm is attacked by chloride ions. pressed samples the current becomes more stable in the initial
For both annealed and peak-aged samples some immersing time is immersion times as it was observed previously [12]. The relative
needed to form a protective passive lm once pitting occurs grad- dissolution or passivation of a surface can be linked to the total
ually. Quick dissolution of the oxide lm in the aggressive solution length of the grain boundary. As shown by Orlov et al. [24], a change
O. Nejadsey et al. / Journal of Alloys and Compounds 648 (2015) 912e918 917

local galvanic cells. Additionally, abundant and deeper corrosion


pits on the corroded surface of the as-cast sample were replaced by
shallow corrosion grooves. The main reason was the uniform dis-
tribution of ne secondary-phase Si particles on the UFG Al matrix
that weakened the susceptibility to pitting corrosion, while it
inhibited general microgalvanic reactions as observed in this study.
Fig. 7 clearly showed that how the precipitation hardening as well
as the size and distribution of precipitates can alter the corrosion
mechanisms. Such an observation was also reported by Akiyama
et al. [15] who performed ECAP on Al-5 wt% Cu alloy and stated that
the size and the total area of Al2Cu particles reduced with the
repetition of ECAP passes. The renement of Al2Cu particles, which
acted as cathode and the Cu-depleted zone surrounding Al2Cu
particles where pitting preferentially took place had been dimin-
ished. These changes in microstructure of the processed samples
seemed to be responsible for improvement in the pitting resistance
after ECAP. The dissolution of Al8Fe2Si inclusions that were within
grain boundaries together with the existing grain boundaries were
also introduced as a main reason for changing the morphology of
pitting corrosion from low-density deep pits to high-density
shallow pits which led to transition from inter-granular corrosion
to pitting corrosion [26].
In addition to that, comparing Fig. 7c, d and e indicated that the
microstructural homogeneity achieved after repeating the ECAP
process up to four passes was also benecial in achieving enhanced
corrosion resistance, because it can reduce the localized corrosion
in some grains. In fact, the homogeneity of corrosive damages
seems to be the main advantages of ultrane-grained materials in
comparison with conventional polycrystals, which are susceptible
to highly localized corrosion [27]. Figs. 7 and 8 clearly showed the
differences between the highly localized corrosion and shallow pits
Fig. 9. EDS analysis of points A and B shown in Fig. 7. on the surface of annealed sample before and after ECAP,
respectively.
in grain boundary length can either increase or decrease the The results of potentiodynamic polarization test shown in Figs. 2
corrosion rate, which depends on specic material/environment and 3, and specically the corrosion volume calculated in Table 2
combinations. In their potentiodynamic polarization study on Mg suggested that the predictions of this test in different processing
alloy ZK60, icorr appeared to decrease as the grain size was reduced. conditions vary slightly. In other words, the variation of corrosion
Additionally, corrosion behavior could not be exclusively attributed rate obtained for annealed, peak-aged, and annealed sample after
to the grain size while ignoring solute population throughout the ECAP is very narrow, which also can be affected by experimental
microstructure [24]. Nevertheless, in the absence of precipitates in errors and preceding cathodic reaction on the sample surface [16].
high-purity materials, the grain boundaries will play the key role in The only conclusion that can be made condently is improvement
controlling the corrosion behavior. Such an investigation was one of of the corrosion resistance of peak-aged sample after two ECAP
the main challenges addressed in this study. X-ray diffraction pat- passes, because the corrosion rate obtained for this specimen is
terns shown in Fig. 5, showed that the relative amount of second about one tenth of the corrosion rate obtained for the rest of the
phase particles in the annealed sample was very low and ECAP led samples.
to decreasing corrosion rate. However, the peak-aged sample, in In addition, it seems that ECAP deteriorates the corrosion
which the relative amount of second phase particles was higher resistance of annealed sample in this test. These differences are
than that of the annealed sample, showed improved corrosion usually explained considering various and counteracting effects of
resistance after ECAP. Similar observation was reported for the ECAP on different samples. The processing by ECAP leads to sub-
corrosion resistance of two Mg alloys [25]. The corrosion resistance stantial increase in the dislocation density, re-distribution of pre-
of AE21 alloy decreased after ECAP while the corrosion resistance of cipitates, crystallite renement, alteration of the surface area of the
AE42 alloy increased. As the grain size of both alloys after ECAP was cathodic sites, and increase in the volume fraction of grain
nearly the same, the variation in the corrosion resistance of these boundaries. Each of these microstructural changes modies the
alloys originated from variation of the alloying elements and the cathodic sites prone to corrosion, formation of passive lm, and in
uniform spatial distribution of the alloying elements in AE42 led to general, the corrosion behavior of the samples [26]. Nevertheless, it
enhanced corrosion resistance. is suggested that results of the EIS technique be used, being a
As indicated, peak-aged sample after ECAP with ne dispersion sensitive method in the investigation of the corrosion behavior.
of second phase particles showed improved corrosion resistance. The results of the EIS tests on the samples of four groups shown
Jiang et al. [14] observed such a phenomenon for cast Al-26 wt% Si in Fig. 4 exhibit a little bit difference with the data obtained in
alloy. The improved corrosion resistance was related to grain polarization curves. While potentiodynamic polarization suggested
renement that provided more nucleation sites to form denser and that the corrosion resistance of the annealed sample after ECAP
thicker natural oxide lm resulting in higher impermeability to reduced, the EIS technique indicated that the corrosion resistance
aggressive media [14]. Macroscopic assessments also showed that of that sample is improved similar to the current transient test
the samples were generally eroded with coincident pitting corro- results. As mentioned, preceding cathodic reaction on the sample
sion due to the presence of large secondary phases that created surface may compromise the accuracy of the obtained results.
918 O. Nejadsey et al. / Journal of Alloys and Compounds 648 (2015) 912e918

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