International Journal of Lightweight Materials and Manufacture 6 (2023) 129e139

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International Journal of Lightweight Materials and Manufacture

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Original Article

Friction stir surface processing of 6061 aluminum alloy for superior

corrosion resistance and enhanced microhardness
Ibrahim H. Zainelabdeen a, Fadi A. Al-Badour a, b, *, Akeem Yusuf Adesina b,
Rami Suleiman b, Fadi A. Ghaith c
a
Mechanical Engineering Department, King Fahd University of Petroleum and Minerals, 31261, Dhahran, Saudi Arabia
b
Interdisciplinary Research Center for Advanced Materials, King Fahd University of Petroleum and Minerals, 31261, Dhahran, Saudi Arabia
c
School of Engineering and Physical Sciences, Heriot-Watt University, 294345, Dubai, United Arab Emirates

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

Article history: In the current study, friction stir surface processing (FSSur.P) was carried out to alter the surface
Received 14 February 2022 microstructure of 6061 aluminum alloy using a pinless friction stir tool. The impact of rising tool rota-
Received in revised form tional speed from 400 to 1200 rpm while keeping tool traveling speed constant at 250 mm/min on
13 June 2022
surface microstructure, mechanical properties, and corrosion resistance was explored in detail. The
Accepted 14 June 2022
Available online 23 June 2022
microstructural findings revealed a significant reduction in grain size, in addition to a remarkable
improvement in microhardness of processed samples. Approximately 44% increase in microhardness,
compared to unprocessed counterpart was achieved at the lowest rotation speed. The corrosion behavior
Keywords:
Friction stir surface processing
of the processed samples as well as the base sample was evaluated after 15 days of exposure to 3.5% NaCl
Pinless FSW tool using several electrochemical methods such as potentiodynamic polarization technique (PDP), linear
AA6061 polarization method (LPR) and electrochemical impedance spectroscopy (EIS) approach. All electro-
Corrosion resistance chemical techniques results demonstrated an excellent agreement where the unprocessed sample
Electrochemical analysis showed poor corrosion resistance with corrosion current density of (Icorr.) of 3.22 mA, whereas the sample
Grain refinement processed at the highest tool rotating speed exhibited superior corrosion resistance with Icorr. of
approximately 0.057 mA. Based on results it was found that increasing tool rotational speed has minimum
effect on grain size, as well as microhardness; with best improvement achieved at lowest rotational
speed or minimum heat input. On the other hand, the corrosion resistance was found to improve with
increasing tool rotational speed. The use of pinless tool had a great impact on simplifying the process and
achieve required surface enhancement without altering the subsurface material.
© 2022 The Authors. Publishing services by Elsevier B.V. on behalf of KeAi Communications Co. Ltd. This
is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/
4.0/).

1. Introduction
Owing to several superior properties, namely high strength to
weight ratio, good thermal conductivity, good electrical conduc-
tivity and high ductility, aluminum and its alloys have gathered
attention to be utilized in different engineering applications such as
defense, aviation, and automotive industries [1,2]. Despite these
outstanding characteristics, aluminum alloys have shown poor
surface characteristics such as wear resistance and microhardness
* Corresponding author. Mechanical Engineering Department, King Fahd Uni-
versity of Petroleum and Minerals, 31261Dhahran, Saudi Arabia.
E-mail address: fbadour@kfupm.edu.sa (F.A. Al-Badour).
Peer review under responsibility of Editorial Board of International Journal of
Lightweight Materials and Manufacture
which were considered as major drawbacks that may restrict their
usage and applications [2,3]. Therefore, several means of heat
treatments were used for aluminum to make it fit more applica-
tions [4]. It should be mentioned that the grain size of crystalline
materials is considered an important microstructural feature
because of its impact on controlling mechanical properties and
corrosion resistance [5]. Hence, fabricating components with
desired mechanical properties is a consequence of governing grain
size. Currently, a voluminous body of research is concentrated on
the development of materials with ultra-fine grains through
various severe plastic deformation methods which demonstrated
better corrosion resistance, higher strength, improved hardness,
and enhanced wear resistance [6,7].
Presently, friction stir processing (FSP) grabs more attention as a
method for severe plastic deformation, where it is considered as a

https://doi.org/10.1016/j.ijlmm.2022.06.004
2588-8404/© 2022 The Authors. Publishing services by Elsevier B.V. on behalf of KeAi Communications Co. Ltd. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/).
I.H. Zainelabdeen, F.A. Al-Badour, A.Y. Adesina et al.
short route method for grains refinement. Through varying the
processing parameters or tool design, corrosion and wear resis-
tance, mechanical properties can be controlled [8]. Hence, micro-
structural aspects, wear behavior and mechanical properties have
been intensively investigated over the last two decades, corrosion
behavior after FSP was not widely studied so far. For example,
Mehdi et al. [9] have reported that several studies showed corro-
sion resistance enhancement after grain refinement and other
studies outlined a reduction in corrosion resistance. Further, it was
proposed that corrosion resistance after grain refinement mainly
relies on electrolytes, routes of severe plastic deformation and
alloying elements. The impact of both rotational and traveling
speeds during FSP of AA 2219 on corrosion resistance was investi-
gated by Surekha et al. [10]. The results demonstrated a significant
impact of rotational speed on corrosion resistance. It was suggested
that as rotational speed rises, intermetallic particles break and
therefore corrosion resistance improved. The influence of multi-
pass FSP of AA 2219 on corrosion behavior was explored by Sure-
kha et al. [11]. The obtained results confirmed a reduction in
corrosion susceptibility by rising the number of passes. Along with
microstructural refinement, FSP was intensively used to fabricate
metal matrix composite. For example, Barati et al. [12] studied the
impact of adding silica particle to AA6061 via friction stir vibration
processing on mechanical properties, wear behavior and corrosion
resistance. The obtained results indicated an improvement in me-
chanical properties and wear resistance. Further, a reduction of
approximately 78% in corrosion rate was also reported. Similarly,
Kumar et al. [13] investigated the influence of SiC addition to
Al7075 via FSP on mechanical properties and corrosion resistance.
Their results revealed that a remarkable enhancement in me-
chanical properties and corrosion resistance. It is worth mentioning
that most of the research in the FSP area concentrated on the in-
fluence of adding reinforcement particles to various materials and
thereafter exploring different properties. Additionally, the influ-
ence of severe plastic deformation methods i.e. ECAP and/or heat
treatment on the corrosion behavior of Al-Mg-Si alloys was
Table 1
Elemental composition of 6061 aluminum alloy.
Element Mg Si Cu Fe
wt% 0.82 0.71 0.23 0.63
Fig. 1. (a) Schematic diagram for FSSur.P of AA 6061-O, (b) pinless FSP tool.
International Journal of Lightweight Materials and Manufacture 6 (2023) 129e139
explored before [4,14e16]. However, to our knowledge, the impact
of friction stir surface processing (FSSur.P) using pinless tool
without adding ceramic particles to AA6061-O on electrochemical
behavior was not studied so far. The proposed surface processing
has advantage over the conventional friction stir processing with
formation of metal matrix composite in terms of using simpler
setup, reduction of excessive stresses on the tool, and minimize the
surface processing time. This may lead to cost savings in the capital
cost of the setup as well as operational cost. Herein, the influence of
varying rotation speed during FSSur.P of AA6061-O on mechanical
properties, and corrosion behavior is to be addressed.
2. Materials and methods
The AA6061-O aluminum alloy was utilized in the present work
with an elemental composition presented in Table 1. Dimensions of
the workpiece were 190, 90 and 6 mm, for length, width, and
thickness, respectively as shown in Fig. 1a. Research base Three-axis
CNC friction stir welder equipped with sensors and a data acqui-
sition system was used in this study (RM-1-MTI, USA). As the
objective was to only process the workpiece surface, a pinless tool
with two circular grooves shoulder of 23 mm diameter was used as
demonstrated in Fig. 1b. The circular groves are meant to enhance
surface stirring and increase the material flow arm. The tool was
made from 4041 tool steel, heat-treated to achieve a hardness level
of 54 HRC. During FSSur.P, the following processing parameters
were fixed; tool traveling speed of 250 mm/min, tool tilt angle of 3

and tool over plunging of 0.2 mm, while the tool rotational speed
was increased from 400 to 1200 rpm; at 400 rpm increment. All
process parameters are listed in Table 2.
One bead on plate was performed per processing condition with
a total traveled distance of 160 mm. During the process, the sheet
was rigidly clamped to a steel backing plate to avoid its movement.
After FSSur.P, all samples were cut; including the unprocessed
sheet, to suitable dimensions for further microstructural, me-
chanical as well as corrosion evaluation. All samples had been
extracted from the middle of the processed plate to avoid process
transient conditions at starting and ending zones. For microstruc-
tural evaluation samples were prepared following standard pro-
Mn Al
cedure, where SiC papers with grid sizes ranging from 320 to 1200
were used for grinding the processed surface. Thereafter, a dia-
0.14 Bal.
mond paste with a size of 2 mm and alumina solution were used for
130
I.H. Zainelabdeen, F.A. Al-Badour, A.Y. Adesina et al. International Journal of Lightweight Materials and Manufacture 6 (2023) 129e139

Table 2
Process conditions and samples designations.

Samples Traveling speed (mm/min) Rotational speed (mm/min)

FS 40 250 400
FS 80 800
FS 120 1200

polishing purposes to obtain a mirror-like finish. Consequently, the

polishing process was followed by a chemical etching whereby the
samples were immersed in a solution containing 2 g of sodium
hydroxide added to 100 mlmL of distilled water. To determine grain
size and morphology of processed surface, an optical digital mi-
croscope (Olympus, DSX 510, Japan) was utilized. Olympus stream Fig. 2. Representative photograph of as-processed surface.
software equipped to the microscope was used to calculate average
grain size according to ASTM 112-13 [17]. X-ray diffraction (XRD)
was also performed on base as well as processed sample to analyze from about 100 to 80 N.m and further increment in tool rotation
the present phases. XRD was performed using Bruker diffractom- speed to 1200 rpm caused the decline of spindle torque to around
eter (D2 PHASER), operated at 30 kV with CuKa (la ¼ 1.54 Å). To 70 N.m. The reduction in generated torque with rising rotation
evaluate the mechanical properties of base and processed samples, speed is ascribed to the heat input increment and thereby dimin-
a mico-indenter (CSM Instruments, Switzerland) was used under a ishing in flow stresses [18]. Moreover, it can be noticed from the
normal load of 2 N and with a loading/unloading rate of 5 N/min. plot that low fluctuation in spindle torque is recorded at 1200 rpm
Six measurements were taken at 6 different locations on the sur- as compared to other conditions. Lower values of spindle torque are
face and the average value was reported. To study the morphology observed at the first stage of the graph which is ascribed to tran-
of corroded surfaces, a field emission Scanning electron microscope sient traveling speed before steady-state condition. The main
(FESEM) (Quanta 250, Czech Republic) was employed. objective of measuring tool torque is the estimation of heat input; H
For electrochemical evaluation, all samples were ground up to (J/mm), which can be calculated based on average recorded torque;
600 grit size to remove developed tool shoulder marks and elimi- Tavg (N.m), tool rotational speed; N (rps), and traverse speed; V
nate the impact of surface roughness on corrosion characteristics. (mm/s), as presented in equation (1) [19];
Thereafter, the base sample, as well as processed samples, were
cleaned using distilled water and acetone to remove any impurities. 2pNTavg
Subsequently, the processed surfaces were masked and only 1 cm2 H¼ (1)
V
of the processed surface was exposed to 3.5% NaCl electrolyte at
room conditions for 15 days. A typical three-electrodes electro-
chemical cell (Gamry-USA) was utilized where the graphite served 3.2. Microstructural analysis
as an auxiliary electrode, sample surface and saturated calomel
electrode (SCE) were serving as working and reference electrodes The impact of FSSur.P of AA6061-O on microstructure in com-
respectively. With an objective of data collection and analysis, the parison to the base metal is illustrated in the optical micrograph in
Gamry instrument (Reference 3000) potentiostat/galvanostat was Fig. 4. It is evident from Fig. 4 that employing FSSur.P substantially
employed. To ensure the stability of electrolyte and samples, open changed the surface grain structure. In addition, considerable
circuit potential (OCP) measurements were allowed for 30 min. refinement can be observed for all processed samples. Further; as
Consequently, the impedance curves were obtained using alter- shown in Table 3, a significant reduction in the grains size from
nating current at a frequency ranging between 10 mHz and 0.1 GHz 94 mm for the base sample to 15.48 mm for the sample processed at
and amplitude of 10 mV at OCP, while a potentiodynamic polari-
zation test was carried out using direct current and with potential
ranging from þ0.25 V to 0.25 V at a scanning rate 0.5 mV s1
against Ecorr. Linear polarization resistance measurements were
carried out by changing the potential of the electrode from 25 mV
to þ25 mV at a scanning rate of 125 mV s1. Thereafter, to fit the
obtained electrochemical data, Analyst 6.0 software was utilized.

3. Results and discussion

3.1. Surface appearance and generated torque

Fig. 2 presents a typical as-processed surface, where excessive

flash was formed due large tilt angle and tool over plunging. Prior
to further testing (i.e microstructure, XRD, microhardness and
electrochemical analysis) the flash was removed and the surface
was ground till shoulder marks were invisible.
The influence of increasing rotational speed from 400 to
1200 rpm on the measured tool torque during FSSur. P is shown in
Fig. 3. It is clearly seen that rising the tool rotational speed from
400 rpm to 800 rpm resulted in decreasing the average tool torque Fig. 3. Generated torque from the samples processed at different rotational speeds.

131
I.H. Zainelabdeen, F.A. Al-Badour, A.Y. Adesina et al.
Fig. 4. Optical micrograph of the grain structure for the (a) base, (b) FS-40, (c) FS-80 and (d) FS-120.
Table 3
Grain size for the base and processed samples.
Samples (Tavg) Average torque (N.m) (H) Heat input (J/mm) Grain size (mm)
Base - -
FS-40 100 1005.31
FS-80 80 1608.5
FS-120 70 2111.15
400 rpm was found. With increasing tool rotational speed, the grain
size demonstrated a slight increment from approximately 15.48
mm at 400 rpm to 19.12 mm at 1200 rpm, while the heat input
increased remarkably from 1005 to 2111 J/mm; calculated based on
equation (1) [19]. A similar observation was extensively reported in
the literature [20,21]. It was suggested that rising tool rotation
speed caused higher heat input and elevated temperature exposure
and thereby increasing the grain size at the surface of these
workpieces [20]. It is worthwhile to mention that the grain
refinement of the processed zone during FSSur.P was ascribed to
the combination of temperature increase and severe plastic defor-
mation resulting from the rubbing action of the tool with the sur-
face of the workpiece [22].
3.3. XRD
Fig. 5-a shows XRD patterns for the base sample as well as
processed ones. It is obvious from the XRD results that four
aluminum peaks are found without any extra peaks which suggests
that no intermetallic phases were formed due to the FSSur.P, except
sample FS-80, where a small peak near (111) appeared and it is
expected to be due Al2O3. It can be noticed also that with increasing
International Journal of Lightweight Materials and Manufacture 6 (2023) 129e139
tool rotational speed the intensity of (200) to (111) plane is
increasing. Relatively narrower bands were found for the base
sample which indicates a higher grain size and a lower lattice
94
distortion [23]. Moreover, a phase shift is clearly observed in Fig. 5-
15.48 b for all processed samples toward a higher diffraction angle. A
17.36 similar observation was reported before after FSP of magnesium
19.12 and copper which was attributed to the existence of compressive
stresses resulted from a reduction in lattice parameter [24,25].
3.4. Evaluation of mechanical properties
Depending on hardening mechanism of base material, condi-
tions i.e processing parameters during FSP may result in decreasing
or increasing the hardness. In this work, the base material was in
annealed form, therefore the hardness level is expected to be in its
minimum levels before the process. The influence of FSSur.P on
surface microhardness, and modulus of elasticity is depicted in
Fig. 6. It is evident from the figure that the average microhardness
was significantly improved, where the base sample average hard-
ness was 49.7 HV and after FSSur.P, the microhardness increased to
71.4, 69.1 and 68.3 HV for the samples processed at 400, 800 and
1200 rpm, respectively. The substantial increment in microhard-
ness after samples processing may be attributed to grain refine-
ment which follows the Hall-Petch relationship [26]. Similarly, a
marginal enhancement in elastic modulus was also attained after
samples processing with 7%, 8% and 6% for samples processed at
400, 800 and 1200 rpm, respectively. Such an increment modulus
of elasticity was reported before and that was ascribed to dynamic
recrystallization [27]. In general, raising the tool rotational speed
from 400 to 1200 rpm, while maintaining other processing
132
I.H. Zainelabdeen, F.A. Al-Badour, A.Y. Adesina et al.
Fig. 5. XRD (a) patterns of the base sample and specimens processed at various rotational speeds, (b) first peak of all samples to demonstrate the phase shift.
Fig. 6. Hardness and modulus of elasticity for the base and processed samples.
conditions fixed didn't have large impact on surface hardness as the
differences in average hardness was within measurement variance.
3.5. Evaluation of corrosion behavior
3.5.1. Electrochemical impedance spectroscopy (EIS)
In order to investigate surface metal oxides, corrosion mecha-
nisms, kinetics, and surface treatment, electrochemical impedance
spectroscopy (EIS) is extensively deployed [28e30,39,40]. There-
fore, EIS measurements were carried out to study the impact of
FSSur.P on AA6061-O corrosion kinetics as compared to the as-
received specimen after immersing all samples in 3.5% NaCl elec-
trolyte for 15 days, moreover, the effect of changing tool rotational
speed from 400 to 1200 rpm. Fig. 7 presents the Nyquist plot for the
base sample as well as the processed ones. As observed from the
plot, all processed samples demonstrate a larger uncomplete arc at
a higher frequency compared to the base sample, which illustrates a
relatively smaller uncomplete semi-circle at a higher frequency. It
was suggested that the uncomplete capacitive arc for processed
samples refers to charge transfer resistance at the border between
133
International Journal of Lightweight Materials and Manufacture 6 (2023) 129e139
passive film formed, sodium chloride electrolyte and the metal [31].
Consequently, the charge transfer resistance occurred when the
passive film exists at the interface between the electrolyte and
metal surface. It is worth mentioning that the existence of the
second uncomplete arc may be attributed to diffusion-controlled
processes [32]. It can be clearly seen in Fig. 7 that the radius of
the capacitive arc significantly increases with rotational speed rises
and all processed samples displayed a larger radius as compared to
the base metal. Interestingly, the radius of the capacitive arc for the
base sample was not able to be captured without enlarging. A vast
variation in capacitive arc radius between the base and processed
samples demonstrated that the corrosion resistance was altered by
FSSur.P. In addition, a raise in arc radius after processing is ascribed
to improvement in surface protectiveness which resulted from
stability and compactness increment of the passive film
[33,34,43,44].
Fig. 8 presents the impedance-frequency graph for all samples
after 15 days of surface exposure to 3.5% NaCl electrolyte. It is
noticed from the graph that the total impedance at the low fre-
quency of 0.01 Hz for all processed samples is greatly higher than
that of the base sample which revealed the surface protectiveness
provided by FSSur.P. Furthermore, a rise in total impedance could
be noticed with increasing rotation speed, where FS-120 sample
reveals the highest corrosion resistance compared to FS-80 sample
which showed lower corrosion resistance. Moreover, the sample
processed at the lowest rotational speed demonstrated the lowest
corrosion resistance among all processed samples. It is, however,
showed markedly higher corrosion resistance when compared with
the base sample.
Phase angle-frequency for the base sample as well as processed
samples after 15 days of immersion in 3.5% NaCl are shown in Fig. 9.
As clearly seen in the figure, the base sample exhibits a phase angle
maxima of 78.5
at a frequency of 25 Hz. Further, observing
maxima at such a high frequency revealed a weakening in the
stability of the barrier at high frequency [35]. In contrast, all FS-40,
FS-80 and FS-120 samples demonstrated a shift in phase angle
maxima toward 76.2
, 84
and 81.9
at a frequency of 12.4, 6.3
and 6.3 Hz respectively. It is evident from Fig. 9 that the base
sample shows the narrowest phase peak; however, after deploying
FSSur.P further widening was captured with rising the rotational
speed which could account for two times constant interaction [36].
In addition, peak widening after surface processing may be ascribed
to improvement in a passive layer over a wide range of frequencies
I.H. Zainelabdeen, F.A. Al-Badour, A.Y. Adesina et al.
Fig. 7. Nyquist graph for both base and processed samples in 3.5% NaCl.
Fig. 8. Impedance plot for the base as well as processed samples in 3.5% NaCl.
and thereby enhancing corrosion resistance [35,37]. It should be
emphasized that the shifting of phase angle maxima to a higher
frequency demonstrates that the corrosion would have launched
on the sample for a long exposure time [38]. Thus, a severe corro-
sion attack is expected on the surface of the unprocessed sample
and consequently a higher corrosion rate when compared with
other processed samples.
With an objective of numerical estimation for the character-
istics of the barrier for the base sample as well as processed
samples, all curves were fitted to equivalent circuits. Conse-
quently, two corresponding circuits were utilized to mimic the
corrosion behavior of base and processed surfaces. Fig. 10-a il-
lustrates the corresponding circuit that simulates the corrosion
behavior on the surface of the base sample which consists of
polarization resistance (Rp) connected in series with Warburg
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International Journal of Lightweight Materials and Manufacture 6 (2023) 129e139
Fig. 9. Phase angle graph for the base and processed samples in 3.5% NaCl.
resistance (W) and both are connected in parallel to the constant
phase element of double-layer capacitance, and the previous
configuration is serially connected to the solution resistance (Rs).
On the other hand, to simulate the behavior of corrosion of pro-
cessed samples, a circuit involve charge transfer resistance (Rct)
serially connected to Warburg resistance (W) and both are par-
allelly linked to constant phase element of double-layer capaci-
tance and all are serially connected to polarization resistance
which connected in parallel to constant phase element and the
whole previous circuit is connected in series to the solution
resistance (Rs) as depicted in Fig. 10-b.
It should be noted that pure capacitance was replaced by con-
stant phase elements due to non-ideal capacitive behavior that was
revealed by the deviation from 90
in the phase angle. Thus, to
calculate the double layer capacitance eq. (2) was used,
I.H. Zainelabdeen, F.A. Al-Badour, A.Y. Adesina et al. International Journal of Lightweight Materials and Manufacture 6 (2023) 129e139

Fig. 10. Equivalent circuits utilized to fit: (a) the base sample, (b) all processed samples.

As clearly seen in Table 4, all processed samples have shown a

lower value of double-layer capacitance (Cdl) and therefore a higher
Cdl ¼ Y0 ðumax Þ n1
(2)
protective film thickness when compared with the base sample. It
is also demonstrated from Table 4 that the charge transfer resis-
where Y0 is the component of constant phase elements (admit-
tance (Rct) revealed a significant enhancement with rotational
tance), n corresponding to the surface roughness, u max is fre-
speed increment and the sample processed at the lowest traveling
quency when the imaginary part of the impedance is at its highest
speed (FS-40) demonstrated a higher Rct compared with that of the
level. Table 4 presents the electrochemical parameters derived
base. In addition, the raise in charge transfer resistance may be
from the two electric circuits. It is evident from Table 4 that double-
interpreted by the formation of the passive film at the border be-
layer capacitance (Cdl) of constant phase element demonstrates a
tween the electrolyte and surface of the metal. Therefore, the ex-
significant drop for all processed samples as compared to the base
istence of such a passive film protects the metal surface from ions
metal and the order of reduction for the samples was the base, FS-
attack and thereby impeding the addition of charge or mass
80, FS-120 and FS-40. It is worthwhile to know that the diminishing
transfer [42]. Commonly, Warburg resistance (W) is added to
in double-layer capacitance after surface processing suggests an
stimulate the influence of diffusion and it is signaled by a straight
improvement in the corrosion resistance which may be ascribed to
line in the Nyquist plot near to 45
to the real axis of impedance. It
the decline in the activeness of the surface as a result of passive film
is clear from the table that most of processed samples illustrated a
formation [39,40]. Accordingly, a reverse relationship between the
low value when compared with the base sample. It should be
double-layer capacitance (Cdl) and the thickness of the protective
mentioned that a lower value of this resistance implies a dimin-
film was disclosed in the Helmholtz model (eq. (3)) [41].
ishing in the flow of chloride ions across the passive film and
thereby enhancing corrosion resistance [38,43].
εεo
d¼ (3)
Cdl
3.5.2. Potentiodynamic polarization (PDP)
where d is the thickness of the passive film, Cdl is the value of Fig. 11 presents typical potentiodynamic polarization curves of
double-layer capacitance of constant phase elements, ε and εo are the base as well as processed samples after immersing in 3.5% NaCl
the dielectric constant of the medium and the permittivity of the electrolyte for 15 days. Table 5 reveals different parameters ob-
vacuum respectively. tained from the fitting of potentiodynamic curves for all samples,

Table 4
Electrochemical parameters derived from Nyquist plot.

Samples Rs (U) Y01 (Ssa) 106 a1 Rp (kU) Y02 (Ssa) 106 a2 Rct (kU) Cdl (mF) W Ss(1/2)106 Goodness 10e4

Base 12.38 23.5 0.92 6.14 34 413 0.29

FS-40 10.2 11 0.90 1.89 1.61 0.97 29.4 1.65 527 4.64
FS-80 11.54 12.94 0.96 0.044 5.77 0.94 80.7 7.6 57.6 6.19
FS-120 12.92 7.39 0.92 0.118 4.04 0.94 144 5.32 41.5 5.5

135
I.H. Zainelabdeen, F.A. Al-Badour, A.Y. Adesina et al. International Journal of Lightweight Materials and Manufacture 6 (2023) 129e139

achieved a reduction in grain size to 100 nm, and the polarization

test in 3.5% NaCl should some improvement in corrosion potential,
on the other hand minor improvement on the corrosion current
density were attained.

3.5.3. Linear polarization resistance (LPR)

Fig. 12 illustrates linear polarization curves for all samples after
immersing in 3.5% NaCl for 15 days. Accordingly, polarization
resistance was observed as the slope of corrosion potential vs
current. Consequently, the Stern-Geary equation was used to obtain
the corrosion current density (Icorr) knowing the polarization
resistance (Rp) according to eq. (4) [46].

ba bc
Icorr ¼ (4)
2:303 RP ðba þ bc Þ

where ba and bc are anodic and cathodic Tafel slopes, and Rp is the
polarization resistance.
Subsequently, to calculate the corrosion rate (mpy), eq. (5) was
Fig. 11. Potentiodynamic polarization curves after 15 days of exposure to 3.5% NaCl for
used
the base and processed samples.

0:131  Icorr  EW
CR ¼ (5)
Table 5 r
Corrosion parameters derived from Tafel curves fitting.
where r is the sample density, and EW is sample equivalent weight.
Samples ba bc Icorr (mA) Ecorr (V) corrosion rate (mpy)
Inspecting Table 6 reveals that the corrosion current density of
Base 1.856 2.56E-01 3.22 0.832 1.469 all processed samples is lower than that of the base metal and the
FS-40 6.62E-01 1.74E-01 0.914 0.93 3.92E-01
sample processed at the highest rotational speed displayed the
FS-80 1.830 1.52E-01 0.468 1.18 2.13E-01
FS-120 4.43E-01 1.25E-01 5.68E-02 0.906 2.59E-02 lowest corrosion current density and therefore the lowest corrosion
rate.

namely corrosion potential (Ecorr.), corrosion current density (Icorr) 3.6. SEM images
and both cathodic and anodic Tafel slopes (bc &ba ). Interestingly,
corrosion potential exhibits a significant shift to the positive di- To study the morphology of the corroded surfaces and to
rection after rising the tool rotation speed from 400 to 1200 rpm, compare the influence of processing samples using FSP, various
however, the base sample shows more positive potential. Despite scanning electron images were taken from the area that was
the lower corrosion potential (Ecorr) of the processed samples when exposed to 3.5% NaCl for 15 days and after the potentiodynamic
compared with the base counterpart, the samples processed at 400 polarization test. As depicted in Fig. 13 a, Deeper corrosion pits were
and 1200 rpm showed a lower pitting potential as depicted in noticed for the base sample especially around the corrosion prod-
Fig. 11 which reveals an enhancement in pitting resistance for these ucts. Additionally, as compared to processed samples, the base
processed samples. metal demonstrates a severe corrosion attack which confirmed the
The inspection of Table 5 demonstrates that the corrosion cur- results obtained from the phase angle-frequency plot (Fig. 9).
rent density of the base sample is 3.22 mA and after employing
FSSur.P the corrosion current density sharply drops. Additionally,
with increase tool rotation speed from 400 to 800 rpm, the corro-
sion current density drastically reduced from 0.914 to 0.468 mA.
Interestingly, the sample processed at the highest tool rotation
speed of 1200 rpm revealed the maximum resistance to corrosion
with a corrosion current density of 0.057 mA. Hence, a considerable
reduction in (Icorr) and therefore corrosion rate revealed that the
FSSur.P has a great potential in reducing the corrosion susceptibility
of AA6061-O. Compared to other sever plastic deformation i.e.
equal-channel angler pressing (ECAP) and shot peening applied to
AA6061, it was found that FSSurf.P had a greater reduction in
corrosion susceptibility. Nejadseyfi et al. [44] investigated a com-
bined multi pass ECAP with heat treatment seeking to improve
corrosion resistance of AA606. The best results against corrosion
resistance were achieved using 2 passes and peak-age heat treat-
ment. The authors reported a drop in corrosion current density in
3.5% NaCl electrolyte by 2.3 times, where corrosion current density
of unprocessed and processed under optimum conditions were
0.86 mA and 0.37 mA, respectively. Another investigation by Bin
Chen at al [45] studied the influence of grain refinement on Fig. 12. Linear polarization curved for all samples after immersing in 3.5% NaCl for 15
corrosion performance of AA6061 after shot peening. The authors days.

136
I.H. Zainelabdeen, F.A. Al-Badour, A.Y. Adesina et al.
Table 6
Polarization resistances values obtained from LPR curves.
Samples Rp (kohms) Icorr. (mA)
Base 35.87 2.724
FS-40 119 0.503
FS-80 322.8 0.1889
FS-120 379.4 0.1115
However, after deploying FSP, the severity of corrosion attack is
substantially reduced as clearly seen in Fig. 13b, c and d.
To sum up, besides scanning electron images, all electro-
chemical tests show a strong agreement in the trend of corrosion
resistance where the base sample revealed the highest corrosion
rate and a further reduction in corrosion susceptibility was
observed upon rising the tool rotational speed. A similar observa-
tion has been disclosed by Surekha et al. and Navaser et al. upon FSP
of 2219 AA and 7075 AA respectively [10,47]. For both cases, the
enhancement in corrosion resistance with rotation speed increase
was ascribed to precipitation dissolution. It is worth mentioning
that the impact of rising the tool rotational speed during friction
stir welding of 6xxx Al-Mg-Si family was reported before and it was
suggested that at a higher tool rotation speed and therefore a
higher temperature, the second phase particles (Mg2Si) dissolved
and became finer [48,49]. Indeed, the corrosion behavior of this
precipitate relative to the aluminum matrix was extensively stud-
ied in the literature [50e52]. There was a strong agreement be-
tween all authors that Mg2Si has cathodic behavior and therefore it
is expected that its dissolution will have a positive impact on
Fig. 13. Scanning electron images of (a) base, (b) FS-40, (c) FS-80, (d) FS-120 samples after 15 days of immersion in 3.5% NaCl.
International Journal of Lightweight Materials and Manufacture 6 (2023) 129e139
corrosion resistance by forming strong passive film. It should be
emphasized that the corrosion behavior after grain refinement is
CR (mpy) not yet fully understood. Nevertheless, according to electro-
1.168
chemical results, the authors strongly believe that a combination of
0.2157 both grain refinement and precipitation dissolution are the main
0.0389 reasons for superior corrosion resistance obtained after processing
0.0291 the samples surfaces.
4. Conclusions
The impact of FSP of 6061 AA on microstructure, mechanical
properties and corrosion resistance was investigated and the
following conclusion can be derived:
(1) It was observed that FSSur.P resulted in considerable grain
refinement with a more homogenous distribution. Besides,
the results demonstrated that rising rotational speed resul-
ted in a marginal grain coarsening.
(2) A significant enhancement in microhardness was reported
for all processed samples with a negligible variation. Also, a
noticeable improvement in elastic modulus was obtained for
all processed samples.
(3) A substantial improvement in corrosion resistance was
revealed for all processed samples over the base metal. In
addition, further corrosion resistance enhancement was
noticed upon increase rotational speed. Moreover, a strong
agreement was observed between all electrochemical
approaches.
137
I.H. Zainelabdeen, F.A. Al-Badour, A.Y. Adesina et al.
Author contribution
Fadi A. Al-Badour: Conceptualization, Methodology, Supervi-
sion. Ibrahim H. Zainelabdeen: Investigation Data curation,
Writingeoriginal draft. Rami Suleiman: Data curation, Validation,
Akeem Y. Adesina: Data curation, Visualization, Validation. Fadi A.
Ghaith: Visualization, Writingereview & editing.
Data availability
The raw/processed data required to reproduce these findings
cannot be shared at this time as the data also forms part of an
ongoing study.
Conflicts of Interest
The authors declare that there is no conflicts of interest.
Acknowledgements
The authors thank King Fahd University of Petroleum and
minerals (KFUPM) for providing All support. The financial support
by the deanship of scientific research at KFUPM through project no.
DF201013 is gratefully acknowledged.
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