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Microstructural evolutions and mechanical properties enhancement of AA

6063 alloy reinforced with Tungsten (W) nanoparticles processed by friction
stir processing

Article  in  Materials Characterization · January 2021

DOI: 10.1016/j.matchar.2021.110903

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 Materials Characterization xxx (xxxx) xxx-xxx

Contents lists available at ScienceDirect

Materials Characterization
journal homepage: http://ees.elsevier.com

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Microstructural evolutions and mechanical properties enhancement of AA 6063 alloy
reinforced with Tungsten (W) nanoparticles processed by friction stir processing
L. Feroz Ali a ,⁎ , N. Kuppuswamy b , R. Soundararajan c , K.R. Ramkumar d , S. Sivasankaran e ,⁎

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a
Department of Mechatronics Engineering, Sri Krishna College of Engineering and Technology, Tamilnadu, India
b
Department of Mechanical Engineering, KIT–Kalaignar Karunanithi Institute of Technology, Tamilnadu, India
c Department of Mechanical Engineering, Sri Krishna College of Engineering and Technology, Tamilnadu, India
d Department of Metallurgical and Materials Engineering, Indian Institute of Technology Madras, India
e Department of Mechanical Engineering, College of Engineering, Qassim University, Buraidah 51452, Saudi Arabia

D
ARTICLE INFO ABSTRACT

Keywords An increase in tensile strength without compromising the ductility is an uphill task in the fabrication of MMCs.
AA 6063 This issue can be overwhelmed by the addition of high temperature withstanding metallic nano-particles limiting
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W nanoparticles solubility at elevated temperatures. The present research work concentrates on (a) the development of AA 6063
Friction stir processing alloy reinforced with Tungsten nanoparticles (0, 3, 6, 9, and 12 vol%) via FSP, (b) examining the phase analysis
Microstructure using XRD technique, and microstructural evolutions through TEM and EBSD, (c) the improvement in mechani-
Tensile properties cal properties (hardness and tensile strength) and investigate the contribution of strengthening mechanisms, and
Work hardening rate
(d) the work hardening rate, intercept (k) and strain hardening exponents (n) through True stress-strain curves.
The results revealed that the uniform dispersion of W nanoparticles is consistent across the stir zone (SZ) of the
AA 6063 matrix. Tensile results were witnessed as improvement in UTS with the function of W nanoparticles
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addition and by elucidating the major loss in ductility. The dispersion strengthening has influenced more to the
total strength of the fabricated MMCs due to the pinning effect produced by nano W particles. AA 6063 alloy re-
inforced with 12 vol% nano W particle specimen has produced superior mechanical properties (Vickers hardness
strength of 1.23 GPa, UTS of 432.58 MPa and, elongation of 18.5%.
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Nomenclature Geometric dynamic recrystallization

HAGB
AMCs High angle grain boundaries
Aluminium matrix composites IMCs
CDRX Intermetallic compounds
Continuous dynamic recrystallization LAGB
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CTE Low angle grain boundaries

Coefficient of thermal expansion MMCs
DRV Metal matrix composites
Dynamic recovery PSN
EBSD Particle stimulated nucleation
Electron backscatter diffraction SEM
EDAX Scanning electron microscopy
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Energy dispersive X-ray spectroscopy SFE

FSP Stacking fault energy
Friction stir processing SHE (n)
GB Strain hardening exponent
Grain boundary TEM
GDRX Transmission electron microscopy

⁎ Corresponding authors.
E-mail addresses: ferozmts@gmail.com (L.Feroz Ali); sivasankarangs1979@gmail.com, s.udayar@qu.edu.sa (S. Sivasankaran)

https://doi.org/10.1016/j.matchar.2021.110903
Received 23 September 2020; Received in revised form 23 December 2020; Accepted 11 January 2021
Available online xxx
1044-5803/© 2021.
L.Feroz Ali et al.
UTS
Ultimate tensile strength
XRD
X-ray diffraction analysis
SZ
Stir zone
TMAZ
Thermomechanical affected zone
HAZ
Hear affected zone
WHR
(Θ)
Work hardening rate
σT
True stress
ɛT
True strain
dσT
Changes in successive values of true stress
dɛT
Changes in successive values of true strain
K ognized as a promising approach for producing sound MMCs (surface
Intercept
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1. Introduction
The combination of high strength and lightweight materials is a vi-
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tal requisite in the aircraft and automobile industries. The reduction in
weight of engineering components leads to an improvement in fuel effi-
ciency and an increase in the payload as described by Dursun and Soutis
[1]. This can be satisfied by AMCs without compromising the mechani-
cal properties. According to [2], AMCs, being a new material of pursuit,
improves the performance of materials, and extend the service life of the
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components. In general, AMCs have combinational properties from both
the matrix and reinforcement. Among the various series of Al alloys, Al
6xxx series alloys are precipitation-hardened alloys comprised of Si and
Mg as major alloying elements as reported by Thangarasu et al. [3] for
instance. Especially, AA 6063 can be weldable, formable, and machin-
able with medium strength. Hence, AA 6063 is applied in bicycle frames
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and bridge rails, and other structural parts as demonstrated by Gangil et
al. [4]. Altogether, MMCs gets strengthened by embedding the ceramic
particles like oxides, borides, nitrides, carbides, and nanotubes reported
by Koli et al. [5]. As per McDanels [6] long back, the hard-ceramic par-
ticles introduced in the soft Al matrix improves the strength, wear, and
corrosion resistance without any addition of weight. Conversely, the ag-
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glomerated/clustered ceramic particulates severely deprive the ductility
and restrict the plastic flow of the composite. The decrease in ductility
is one of the catastrophic failures in the engineering components failing
in service life. The work based on Zhang et al. [7] reported that it is bet-
ter to choose the metallic particles with higher hardness, higher melting
point with limited solubility, as a reinforcement to retain the ductility
incommensurate with increases in strength of the MMCs. At this junc-
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ture, Tungsten (W) is a promising candidate to elect as a reinforcement
particle due to its higher strength, higher stiffness, higher melting point
(3414 °C), and retaining the properties at elevated temperatures which
are also studied by Dixit et al. [8]. The retention of metallic particles
in their elemental form in MMCs is highly a challenging task. Huang
et al. [9] reported IMCs (Al4W, Al5W, and Al12W) are the stable com-
pounds present in the Al – W phase diagram at RT condition. Hence an
appropriate MMCs fabrication technique has to be adopted for real-time
production. Several techniques are in existence to produce MMCs. Stir
casting/squeeze casting is a prominent one for MMCs production in liq
2
Materials Characterization xxx (xxxx) xxx-xxx
uid metallurgy technique. However, the addition of metallic particles in
the molten metal activates the reaction leading to the formation of in-
termetallic phases [10].
Ramakrishnan and Dinda [11] developed the Al – W composite
through a laser melt deposition technique and noticed the formation
of IMCs like Al4W, Al5W, and Al12W was observed. Likewise, Zeng
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et al. [12] observed the Al3Ti phase generation in Ti particles rein-
forced AMCs through the stir casting technique. Powder metallurgy is a
solid-state processing technique; which also forms the unwanted IMCs
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after sintering. Sun et al. [13] reported the formation of Al3Ti IMCs in Al
– Ti composite developed through the pulse discharge sintering process.
Similarly, Feng et al. [14] perceived the formation of Al12W through re-
action sintering technique in Al – W composites. Hence brittle IMCs for-
mation due to the solubility of metallic reinforcement particles in the
Al matrix cannot be eliminated in the aforementioned routes. The for-
mation of IMCs can be nullified by the accumulative roll bonding (ARB)
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technique. Ramkumar and Natarajan [15] used the ARB technique to
fabricate AMCs; in which the absence of IMCs could be found; nonethe-
less, ductility is greatly decreased due to the strain hardening engen-
dered with the increase in rolling passes.
FSP comes under the solid-state processing technique; which has rec-
composites). As per Avettand-Fènoël and Simar [16], during FSP, the
temperature will not reach the melting point of the matrix material lead-
ing to the elucidation of deleterious IMCs. As FSP is energy-efficient,
it produces a fine-grained matrix, the clear interface between matrix,
and reinforcements and uniform dispersion of particles as mentioned by
Salih et al. [17]. Abraham et al. [18] manufactured AA 6063 compos-
ite by dispersing vanadium (V) particles. There was a clear interface be-
tween Al and V interface without any deleterious reaction and formation
of intermetallic layers. In the same way, Selvakumar et al. [19] have
not observed any IMCs such as Al3Mo, Al12Mo, and AlMo in the fabri-
cated Al 6082 composite with the dispersion of Mo particles. In afore-
mentioned both the cases, the ductility of the AMCs has been retained at
an appreciable level.
In recent times, researchers have successfully introduced metallic
particles as reinforcement in MMCs by avoiding the IMCs formation
with improved strength and retention of ductility. Despite significant at-
tempts were done, there is no previous research describing the addition
of W nanoparticles in the AA 6063 matrix through the FSP technique. In
this research, the advanced microscopic techniques are used to examine
the phase formation/transformation behaviour, uniform dispersion of W
particles, generation of dislocations, and fine-grained formation in the
Al matrix. Further, the clear interface between matrix and W nanoparti-
cles along with the mechanical properties evaluation are experimentally
carried out and investigated the behaviour.
2. Experimental procedure
2.1. Starting materials
The matrix material used in this work is AA 6063 (99.5% purity)
with the nominal chemical composition (vol%) of Mg – 0.46, Si – 0.33,
Fe – 0.16, Mn – 0.02, Cr – 0.09, Zn – 0.05, Ti – 0.02, Cu – 0.02 and Al
– Bal. The chosen matrix, AA 6063 in T6 condition (solutionized and ar-
tificially aged) plates (dimension: 100 × 100 × 6 mm) were employed
for this research. This alloy has been procured from Coimbatore Metal
Mart, TN, India. The schematic of the FSP is shown in Fig. 1a. The W
nanoparticles (99% purity), is considered as a reinforcement supplied by
SRL chemicals, India. The morphology of the as-received W nanoparti-
cles is shown in Fig. 1b which ensures that the particles are tetragonal
shaped at the nanoscale level. The inset of Fig. 1b illustrates the fre-
quency distribution of the W nanoparticles. It can be observed from the
inset of Fig. 1b that the majority of the particles are sized between 30
and 40 nm with the average particle size of 38 ± 09 nm.
L.Feroz Ali et al. Materials Characterization xxx (xxxx) xxx-xxx

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Fig. 1. (a) Schematic illustrating the working principle of FSP; (b) FESEM micrograph of W nanoparticles. The inset of (b) illustrates the frequency distribution chart of W nanoparticles;
(d) Macrograph showing the FSP; (d) Samples for tensile test.

2.2. Processing Table 1

FSP conditions.
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A groove was machined in the middle of the specimen using EDM Parameter Values
with a constant length of 100 mm and a depth of 5.5 mm with a width
of 1.5 mm for stuffing the W nanoparticles. The volume fraction was cal- Rotational speed (rpm) 900
Traverse speed (mm/min) 25
culated using the following equations,
Passes 6
Shoulder diameter (mm) 18
(1) Pin diameter (mm) 6
Pin length (mm) 5
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(2) Tool material H13 steel

Groove width (mm) 1.2
Here, the W nanoparticles were incorporated and varied with the Groove depth (mm) 5
AA 6063 matrix to achieve 0, 3, 6, 9, and 12 vol%. The grooves were Pin shape Cubical cone
Axial force (Fz), kN 10 kN
tightly packed with W nanoparticles. The FSP was done using an indige-
Tool Tilt angle, o 0
nously developed FSW machine. Initially, the top surface of the groove
was roofed by processing with a pinless tool (Fig. 1a) to hinder the ex-
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pulsion of W nanoparticles. Then FSP was carried out using a tool with a
cylindrical pin (Fig. 1a). The tools used for processing FSP and the ma-
chine used to carry out the process are displayed in Fig. 1a. The process
parameter of FSP is documented in Table 1. The photographs of the FSP
process and the samples for the tensile test are illustrated in Fig. 1c and
Fig. 1d respectively.
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length of Kα1 with the scan rate of the 30s/step and step size of 0.02°.
Quanta 400 equipment was used for FESEM analysis to observe the
dispersion of reinforcements. HR-TEM analysis was carried out using
JEOL JEM 2100 to observe the nanoparticles, dislocations and to cor-
relate the rings obtained in diffraction pattern with peaks in the XRD
spectrum. The refinement of the matrix grains in the stir zone was ob-

2.3. Characterization and testing
The samples were machined out from the processed plates using
EDM for characterization studies. The specimens were hot mounted
with Bakelite powders for grinding with various grits of emery sheets
starting from 400 grit to 3000 grit followed by alumina wet polish-
ing for getting a smooth scratch-free surface. The polished specimens
were etched using Keller's reagent. PANalytical X'Pert PRO diffractome-
ter was used to analyse the phases that evolved in the specimen. Cu was
the target material used in the diffractometer by considering the wave
served by EBSD analysis. For EBSD analysis, the specimens were elec-
tro-polished for 20 s in perchlorate solution at −12 °C and analysed us-
ing FEI Quanta FEG–SEM installed with TSL–OIM software. The mi-
cro-hardness test was carried out in the cross-section of the specimen
by covering the base metal zone (BMZ), heat affected zone (HAZ), ther-
momechanical affected zone (TMAZ), and stir zone (SZ), and same in
the opposite size (from −12 mm to +12 mm) by applying the load of
100 g with the dwell time 15 s. The tensile test (ASTM-E8 standard, Fig.
1d) was conducted to investigate the mechanical behaviour in terms of
UTS, YS, % Elongation, WHR, strain hardening exponent (n), and inter

3
L.Feroz Ali et al. Materials Characterization xxx (xxxx) xxx-xxx

cept (k) through stress-strain curves. The morphology of the fracture sur-
face from tensile specimen samples was observed using FESEM.
3. Results and discussion
3.1. Al – W reaction during processing
their elemental form. It is hard to maintain the W particles in their el-
emental form in the matrix without any formation of IMCs like Al12W
which usually occurs through casting and powder metallurgy routes. It is
easy to maintain W nanoparticles over the matrix as W has limited solid
solubility in Al. In general, IMCs formation is influenced by the time of
exposure and attainment of maximum temperature within the stir zone.

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The temperature gradient is relying on the traverse speed and rotational
The diffracted pattern received from the Cu target on Al speed of the tool. In FSP, there is an inadequacy for exposing time and
6063–12 vol% W nanocomposites is depicted in Fig. 2. The charac- temperature to cause the substantial diffusion process between matrix

teristic peaks of reinforced W nanoparticles are present in the Al ma-
trix, (i.e.,); both the Al and W peaks are obvious in the obtained re-
sults. The non-existence of other phases or IMCs from the fabricated
composite was not observed. The results ensure the absence of re-
action between the Al matrix and W nanoparticles leading to reten-
tion of W nanoparticles in
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and reinforcements. During processing, peak temperature in the stirred
zone would be (0.6–0.9)Tm for matrix material which is equivalent to
(0.12–0.18)Tm for reinforcement (here, W). Due to inadequate temper-
ature in the stir zone, the chance for the diffusion of W nanoparticles
into the Al matrix is less eliminating the formation of IMCs. Similarly,
Bauri et al. [20] noticed the absence of IMCs through XRD analysis in
the fabricated Al – W composite and reported that there were no chemi-

PR
cal reaction takes place between matrix and reinforcement particles due
to Tm gradient..

3.2. Dispersion of W in the Al matrix

The SEM micrographs of Al 6063 – x vol% W nanocomposite is

displayed in Fig. 3; which explains the different volume fractions of
W nanoparticles (0, 6, and 12 vol%). Fig. 3a shows the unreinforced

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AA 6063 matrix. From Fig. 3b and Fig. 3c, the distribution nature
of the reinforced W nanoparticles in the AA 6063 matrix could be
seen. The stuffed W nanoparticles are uniformly distributed through-
out the stir zone in both the 6 and 12 vol% of W nanoparticles rein-
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forced Al 6063 matrix. The inter-particle spacing among the W nanopar-
ticles is reduced in 12 vol% reinforced specimens than 6 vol% reinforced
specimens due to the addition of more W reinforcement particles. The
schematic representation shows the cross-section of the FSP specimen
(Fig. 3d). To investigate the uniformity of the reinforcement particles
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Fig. 2. X-ray diffraction pattern of Al 6063–12 vol% W nanocomposite.

throughout the stir zone, SEM micrographs were captured in the top,
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Fig. 3. SEM micrograph of Al 6063 – x vol% W nanocomposite: (a) 0, (b) 6, (c) 12. (d) Schematic representation of FSP specimen. SEM micrographs of Al 6063–12 vol% W nanocomposite
at different portion of FSPed zone: (e) top portion, (f) middle portion and (g) bottom portion.

4
L.Feroz Ali et al.
middle, and bottom of the stir zone in Al 6063–12 vol% W nanocom-
posite, which are displayed in Fig. 3 (e – g), respectively. It is observed
that the dispersion of W nanoparticles was throughout the stir zone. The
SEM micrographs witnessed the homogeneity of dispersion among the
powder particles and there is no vast particle-free space in the matrix.
It can be observed that the W nanoparticles penetrated up to the depth
of 5.5 mm. In addition, the defects like pores were not detected which
advocates that the flow of plastically deformed material was wetted the
surface of the W nanoparticles without any chance for obstruction.
In conventional techniques, the expected distribution cannot be ob-
tained whereas the FSP can produce the desirable distribution. The ho-
mogenous distribution is vital for higher load-carrying ability. An opti-
mized process parameter must be chosen for processing to get proper
distribution. One of the important parameter providing the proper scat-
tering and eliminates clustering of reinforcements are the number of
passes. It is essential to give multiple passes. In this study, six passes
were given to distribute the nanoparticles. The continual stirring action
and the plastic flow of the matrix lead to the breaking of the agglom-
erated reinforcement particle and distributes the reinforcement particles
over the stir zone effectively. The plasticization of the matrix was caused
by the engendering of frictional heat by the rubbing motion of the tool
shoulder and the shearing action of the pin. During FSP, the occurrence
of plastic deformation takes place in the stir zone owing to the combined
action of frictional heat and movement of the tool from the advanc-
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ing-to-retreating side. The tool rotation mixes the stuffed reinforcements
with the plastically deformed matrix and squeezes out in the space be-
tween the cold base metal and the tool pin. The motion of the tool from
one end to another end and shoulder leads to the forging of the W par-
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ticles over the stir Al 6063 matrix producing proper surface composites.
The frictional heat generated by the tool motion does not melt the sub-
strate material which eludes the altering of physical properties of the
reinforcement particles. The motion of the W nanoparticles is governed
by the rotatory motion of the tool and prohibited after processing. Thus,
the scattering is conserved in the stage cooling. The proper scattering of
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reinforcement is the result of optimized process parameters [21]. In the
substrate, 1 mm of the plate is leftover on the bottom side for the promo-
tion of rapid heat dissipation. Similar kinds of results could be observed
by Selvakumar et al. [19]. The continual stirring action of the tool in
the matrix was expected to broke the clustered reinforcement particles
and scattered the de-clustered and cluster-less particles throughout the
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stir zone helping to improve the load-carrying ability of the fabricated
AMCs.
3.3. Examination of grain refinement
The EBSD micrographs of unreinforced, 6 and 12 vol% W nanoparti-
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cles reinforced AA 6063 nanocomposites are presented in Fig. 4 (a – c).
The unreinforced AA 6063 matrix comprises only coarse-grained struc-
tures with an average grain size of 42 ± 08 μm (Fig. 4a). Likewise, 6
and 12 vol% W nanoparticles reinforced AA 6063 nanocomposites con-
tain ultrafine grains of 2.81 ± 08 μm and 0.97 ± 0.6 μm, respectively.
The considerable reduction in grain size was due to the incorporation
of W nanoparticles in higher volume fractions which meritoriously hin-
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dered the growth of grains during matrix recrystallization owing to the
Zener pinning effect. In addition, by repeating the number of passes (six
times here), reinforcement particles were redistributed homogeneously
throughout the stir zone and cause rigorous refinement of coarser grains.
The refinement of grains has severely occurred in the Al 6063 ma-
trix. This was attributed to multiple phenomena such as DRV, CDRX,
GRDX, and PSN. During processing, the high-temperature deformation
takes place in the stir zone owing to high SFE causing dislocations, an-
nihilation, and generation of sub-grains within a grain. By processing
further, the transformation of LAGs takes place by the gradual increase
of the misorientation angle of their sub-grains. Later, the extremely
5
Materials Characterization xxx (xxxx) xxx-xxx
high-temperature plastic deformation like CDRX occurs and forms the
fine equiaxed grained by the rotation of sub-grains with a sluggish in-
crease in misorientation angle and forms HAGBs. The addition of hard W
nanoparticles as reinforcement contributes effectively recrystallization
mechanism through PSN [22]. Jain and Muthukumaran [23] reported
that the addition of reinforcement particles orients the grains randomly
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by the activation of the Zener-Holloman mechanism and PSN during
processing which led to grain refinement. Fig. 5(a – c) showed that the
misorientation maps of unreinforced, 6 and 12 vol% W nanoparticles re-
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inforced AA 6063 composites. It can be observed that there is a shift to-
wards the misorientation angle (from LAGB to HAGB) with the function
of W nanoparticles which warrants the formation of dynamic recrystal-
lization and grain refinement in the fabricated AMCs.
3.4. Generation and interaction of dislocations in Al with W
Fig. 6(a – g) presents the TEM micrograph of Al 6063–12 vol% W
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nanocomposite. Fig. 6a warrants the dispersive nature of W nanopar-
ticles within the stir zone of Al 6063 matrix. The dispersion is uniform
throughout the stir zone in ultrafine and nanosized. A little amount of
clustering was observed on the reinforcement with the size of ~1 μm
in dark contrast colour indicating more than one particle settled in the
same place. Besides, fewer precipitates were identified in the micro-
graph confirming that the substrate material (AA 6063) is a precipi-
tation hardened alloy. From Fig. 6b, generation of dislocation could
be observed within the coarser grain and divided into the number of
sub-grains; it is an array of dislocations within the grain (Fig. 6c); it can
be summarised that the grains are in the stages of DRV process due to
high SFE stored in the Al matrix. Dislocations can be generated by ei-
ther the SPD process or the addition of second phase particles. Fig. 6d
shows the inhibition of dislocation motion by the W nanoparticle due to
the thermal mismatch coefficient between W and Al. The W nanoparti-
cle hindered the GBs by acting as nucleation sited for DRX. Such hin-
drance generates the GDRX promoting the strength of the matrix by the
PSN mechanism. The pinning of dislocation that occurred in the matrix
material could be identified in Fig. 6d. Jain and Muthukumaran [23]
noticed the formation of sub-grain boundaries by the pile-up of disloca-
tions. A continuous and clear interfacial bonding between the reinforce-
ment and matrix acts as a vital role in the load-carrying capacity of the
MMCs. In this work, the interface between the reinforcement and matrix
is coherent. The coherency engenders the strains in the matrix improv-
ing the mechanical properties of the MMCs. Fig. 6(f1 and f2) show the
BFI and DFI of the trapezoidal-shaped W nanoparticle. A crystal clear
interface with void-free nature could be observed in the interface ensur-
ing that the developed composite is a promising candidate for load-car-
rying application. Yadav and Bauri [24] reported that a clear interface
could allow the transfer of both the tensile and compressive loads from
the matrix to the reinforcement. The SAED pattern was captured from
Fig. 6a, and the same is shown in Fig. 6g. The continuous rings in the
SAED pattern warrant that the ultrafine or nanosized grains present in
the system. In this work, the reinforced W nanoparticles were redistrib-
uted with increases in the number of passes and produce ultrafine grains
in the matrix [23,24]. The rings are indexed using (hkl) values; which
are highly correlating with the peaks obtained in the XRD pattern. In
order to observe the elements present in the developed composite, EDS
was carried out in Fig. 6a. The matrix material of Al and reinforcement
of W are available with the traces of the alloying elements (Fig. 6h).
3.5. Vickers microhardness examination and mechanism of microstructural
models
Micro-hardness profiles of Al 6063 – x vol% W (x = 0, 3, 6, 9, and
12) composite after FSP is shown in Fig. 7. The hardness was mea-
sured in the cross-section of the specimen after 6 passes. The average
hardness of the unreinforced Al 6063 matrix is found to be 74.25 HV.
L.Feroz Ali et al.
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Fig. 4. EBSD image of (a) unreinforced Al 6063 matrix, (b) Al 6063–6 vol% W nanocomposite, and (c) Al 6063–12 vol% W nanocomposite.
The hardness values such as 94.26, 105.09, 114.40, 126.136 HV are ob-
tained for 3, 6, 9, and 12 vol% W nanoparticles reinforced specimen, re-
spectively. The deflection among the values is reduced by increasing the
reinforcement particles; this was due to the decrease in the gap between
particle-free zones. The factors influencing the hardness of the unrein-
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forced AA 6063 matrix are grain refinement and the existence of pre-
cipitates. The significant improvement in hardness values in AMCs was
due to: (a) addition of hard metallic W nanoparticle as reinforcement,
(b) existence of precipitates, (c) refinement of grains to ultrafine level,
(d) superior bonding between the Al and W nanoparticles, (e) clear in-
terface between Al and W nanoparticles, and (f) absence of defects like
voids or cracks in the interface and the surface which is also noticed by
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Huang et al. [25].
Microstructural mechanisms in the various zone (BMZ, HAZ, TMAZ,
and SZ) are developed to identify the reasons for improved hardness in
various zones. Fig. 8 shows the development of various microstructures
in different regions. In FSP, the heat will be produced in between the
rotating shoulder and the workpiece owing to friction due to which the
revolving pin deforms the material plastically. Hence, more grain refine-
ment occurs in SZ. The moment after stirring in SZ, grains start to re-
crystallize due to DRV, followed by the continuous stable recrystalliza-
tion (called CDRX), and then nucleated grains start to form during fast
air cooling. Therefore, the grain refinement occurs in SZ after FSP.
6
Materials Characterization xxx (xxxx) xxx-xxx
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Fig. 8a explains the graphical illustration of microstructural develop-
ment in SZ. For the same rotational speed and increasing of W par-
ticles, the volume of matrix materials to be deformed starts to de-
creases due to decreasing of inter-particle spacing of W particles lead-
ing to form more heat in a smaller volume consequently temperature
starts to increases locally. Therefore, the area of SZ slightly larger than
the actual pin area (as mentioned in Fig. 8), more structural refine-
ment occurs with the increasing of w particles in addition to Zener pin-
ning consequently the hardness at SZ was very high (Fig. 7). How-
ever, more hardness values in SZ were expected to fail easily during
tensile load which was discussed in the subsequent section. The cen-
tral zone surrounds the pin and below the shoulder would also be sub-
jected to plastic deformation due to friction and heat which is called
a thermomechanical affected zone (TMAZ). The heat surrounds the SZ
and TMAZ is called as HAZ. During FSP, some of the W particles were
expected to occupy in TMAZ leading to an increase in the hardness
value with increasing W particles for the same rotational speed and tra-
verse speed (Fig. 7). Fig. 8b illustrates the microstructural variation in
TMAZ and HAZ. In HAZ, little grain refinement was expected to occur
due to sudden/fast cooling by air medium leading to a slight increas-
ing of hardness in HAZ. The increasing of hardness values in TMAZ and
HAZ (Fig. 7) with increasing of W particles were expected to increase
L.Feroz Ali et al.
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Fig. 5. EBSD misorientation map of: (a) unreinforced Al 6063 matrix, (b) Al 6063–6 vol% W composite, and (c) Al 6063–12 vol% W composite.
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of heat and grain refinement produced by some W particles in TMAZ
and sudden air cooling in HAZ.
3.6. Investigation of uniaxial tensile behaviour
Fig. 9a and Table 2 display the engineering stress-strain of AA 6063
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- x vol% W nanoparticle reinforced AMCs. The YS of 128.85, 145.06,
140.67, 162.46, 178.68 MPa and UTS of 208.37, 240.07280.66, 319.83,
360.45 MPa were obtained for 0, 3, 6, 9 and 12 vol% reinforced in
Al6063 matrix respectively. The improvement in tensile properties (YS
and UTS) is due to the inhibition of GBs nucleation by uniformly W
scattering nanoparticle addition and a strong interface between matrix
and reinforcement (Fig. 8) as reported by Dinaharan et al. [21]. The
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reaction free interface allows the tensile load to transfer effectively to
the particle from the matrix. The W nanoparticles improve the plas-
tic flow of the Al 6063 matrix, as reported by Bauri et al. [20]. The
ductility of the fabricated Al 6063 matrix value is retained to an ap-
preciable level. The % elongation values are 25, 24, 22, 21 and 18.5
for 0, 3, 6, 9 and 12 vol% reinforced Al 6063 matrix-based compos-
ites respectively. The reasons for retaining the ductile nature are due
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to W reinforcement owns greater CTE value and highly ductile. Dur-
ing tensile loading, the higher ductility aids to deform the nanoparti-
cle. According to Abraham et al. [18] recently, the higher CTE value
property does not hinder the frictional heat flow mitigating the thermal
strain at the Al – W interface and the accompanying dislocation filled
strain fields. Therefore, the elongation of the fabricated AMCs can be in-
creased to a longer extend. In the present work, the tensile test of all
the FSPed samples was failed in the stir zone due to grain refinement
and more hardness values. In general, during the tensile test (pulling
load), the sample starts to fail in the strain hardened/work-hardened
area like refined grain area produced by severe plastic deformation of
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Materials Characterization xxx (xxxx) xxx-xxx
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FSP process as this area possesses more grain boundaries, defects, and
dislocations. The crack begins easily in this area compared to TMAZ,
HAZ, and BMZ where the defects are expected to be minimum/nil. In ad-
dition, the incorporation of W particles in the Al 6063 matrix produces
more refined grains with more surface defects. Therefore, the failure of
the FSPed tensile sample occurs at SZ compared to other zones provided
the tensile samples are to be cut perpendicular to the traverse direction
of FSP for understanding the improvement of strength with the incorpo-
ration of W particles and effect of FSP process. More ductile/soft struc-
ture present in the base metal zone whereas hard structure appears in
the SZ. Hence, the crack starts to propagate from the outer surface of SZ
to the end of the base metal as illustrated in Fig. 9b.
3.7. Investigation of fracture morphology
The fractured surface morphologies of AA 6063 – x vol% W (x = 0,
6 and 12) composite are exhibited in Fig. 10 (a–c). To identify the
various mode of fractures (brittle or ductile), the fractured surface af-
ter tensile loading was observed using SEM analysis. Overall, the dim-
ple structures and cleavage planes denote the mode of ductile fracture
and brittle fracture, respectively. The unreinforced Al 6063 matrix pos-
sesses network dimples with larger sized with cleavage planes within
and nearby the dimples endorsing the mixed modes fractures (both brit-
tle and ductile, Fig. 10a). From Fig. 10 (b and c), the fracture morphol-
ogy of 6 and 12 vol% W AMCs is presented with a large population of
dimples. Fig. 10 d shows the EDS results of 12 vol% W particles incor-
porated sample which exhibited the peaks corresponds to Al 6063 com-
position (peaks of Al, Fe, Cr, Mg, & Si) and three major peaks of W. In
6 vol% W specimen, the size of the dimples was fine and ultrafine level
whereas in 12 vol% W specimen only ultrafine dimples could be ob
L.Feroz Ali et al. Materials Characterization xxx (xxxx) xxx-xxx

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Fig. 6. TEM micrograph of Al 6063–12 vol% W nanocomposite, (a) Uniform distribution of W nanoparticles (b) Dislocation present in the grain, (c) array of dislocations, (d) interaction
of dislocations with W nanoparticles, (e) dislocation pinning, (f1 and f2) BFI and DFI of tetragonal shaped W nanoparticle with a clear interface, (g) SAED pattern and (h) EDS of (a).

served with a larger network. The dispersion of W nanoparticles could ticles could be observed confirming that there were an extensive defor-
be observed from the fractured surface. The tensile load is transferred mation and flow of the Al matrix before failure. The results revealed
uniformly to the reinforcements from the matrix owing to the presence that the strong interfacial bonding was achieved in between the Al ma
of strong interfacial bonding. The fracturing and pull out of W nanopar

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L.Feroz Ali et al.
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Fig. 7. Microhardness profile across the cross-section AA 6063 matrix reinforced with the function of W nanoparticles.
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trix and W nanoparticle reinforcements which is also achieved else-
where [26].
3.8. Ductility examination
The ductility can be examined through cold workability/strain hard-
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ening/work hardening when the materials produce plastic deformation
as reported by Sivasankaran et al. [27]. As a whole, grains get strength-
ened by the generation and motion of dislocations. The WHR can be
computed using Eq. (3).
(3)
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The variation of WHR versus true strain for the AA 6063 – x vol%
W composite is displayed in Fig. 9b. There is a progressive increase
in WHR with reinforcement addition. AA 6063–12 vol% W composite
contains higher WHR than other AMCs specimens (0 to 9 vol% W).
The unreinforced AA 6063 matrix exhibited lower WHR attributed to
the absence of W nanoparticles and inadequate dislocations generation.
Whereas AA 6063–12 vol% W composite exhibited excellent interfacial
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strength, refined ultrafine grains, gathering of more ordered dislocation,
and the addition of W nanoparticles as reinforcement. Altogether, higher
elongation of the material can be obtained by higher WHR delaying the
necking during tension.
The SHE (n) is determined using the Hollomon equation (Eq. (4))
by plotting double logarithmic curves on obtained true stress-true strain
values of AA 6063 – x vol% W (x = 0, 3, 6, 9 and 12) composites (Table
3).
(4)
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The n values are calculated by plotting a graph of Log (εT) in the
x-axis versus Log (σT) in the y axis. A linear fit was chosen for the
drawn scattered plot in Origin software and the slope value was de-
termined. The obtained n values are 0.567, 0.605, 0.607, 0.599 and
0.670 for 0, 3, 6, 9 and 12 vol% reinforced AMCs, respectively. Ac-
cording to Sivasankaran et al. [27], the n value should lie between 0.2
and 0.6, for metallic materials.. The higher and lower value of n spec-
ifies the deformation is elastic and plastic, respectively. For the fab-
ricated AMCs, AA 6063–12 vol% W composite achieves a higher SHE
value (n = 0.670) than the unreinforced matrix, and other W nanopar-
ticles reinforced AMCs. A strong interface between matrix and reinforce-
ment and embedment of W nanoparticles in the Al matrix are the factors
contributing to the enhancement of n value [27].
3.9. Strengthening mechanism
The obtained tensile strength of the Al 6063 – x vol% W compos-
ites are correlated with various strengthening mechanisms aiding for the
improvement of properties. Table 4 shows the nomenclatures involved
in strengthening mechanism calculation, their corresponding units, and
values. The various strengthening mechanisms occurred in the fabri-
cated Al 6063 – x vol% W composites to boost up their strength are:
(a) Grain refinement strengthening (σGB), (b) dispersion strengthening
(σdisper), and (c) dislocation strengthening (σdis). In the present research
work, the Al 6063 plate was microstructurally modified by severe plas-
tic deformation of the FSP process and incorporation of W particles.
Here, there is no possibility of solid solution formation of W particles
as it has a high melting point which never dissolves in Al 6063 ma-
trix. However, the incorporated W particles act as an effective dispersing
agent. Hence, in the theoretical calculation, three strengthening mech-
anisms (σGB, σdisper, and σdis) were accounted for calculation and corre
L.Feroz Ali et al. Materials Characterization xxx (xxxx) xxx-xxx

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Fig. 8. Schematic representing the microstructural mechanisms developed during FSP of AA 6063 matrix reinforced with the function of W nanoparticles: (a) Traverse direction 1-BMZ,
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2,3&4-SZ; (b) Perpendicular to traverse direction 5-TMAZ, 6-HAZ.

lated with the total obtained yield strength. The σGB is the outcome of
the refinement of grains and the pinning of GBs (Fig. 4, Fig. 6, and Fig.
8). The fine-grained materials are harder than the coarse-grained ones
(here, from Fig. 7, high hardness in SZ, low hardness in BMZ). As the
fine-grained materials have a larger surface area of the grain boundary,
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of dislocation around the particles (Fig. 6d). The migration of disloca-
tion is prevented by generated loops (Fig. 6e). The increase in mechan-
ical strength by reinforcement addition can aid as a dispersion strength-
ening (σdisper, Eqs. (7), (8)) as demonstrated by Sivasankaran et al. [29],

this has a higher ability to impede the dislocation motion. In addition, (7)
the finer grains comprise high-angle grain boundaries (Fig. 5) which al-
lows the dislocations to pile up at the grain boundaries. These pile-ups
generate the stress concentrations over the slip planes which creates new
(8)
dislocations in their neighbouring grains. The introduced nanoparticles
hinder the dislocation motion in the GBs. σGB can be expressed using the
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Hall – Petch Eq. (5) as explained by Clinktan et al. [28]:
(5)
During solidification, the variation of CTE between the Al matrix
and W nanoparticle causes dislocations like strain fields on the GBs. The
strain fields can inhibit the motion of dislocation by tensile or compres-
sive loads. It is well known that the dislocation density and YS of any
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The computed σdisper for 6 and 12 vol% W reinforced composites are
67.27 MPa and 98.02 MPa, respectively. With the addition of the W
nanoparticle, the involvement of σdisper increases owing to a decrease in
particle-free zones in the AMCs. According to the linear superposition
model, the overall strength (∆σ) of the FSPed AMC is estimated by (9)
[29]:

material are directly proportional to each other. σDis can be calculated
using the following Eq. (6) as reported by Ramkumar and Natarajan
[15]:
(6)
The dislocation motion of the Al matrix due to externally apply-
ing load can be hindered by the addition of second phase reinforce-
ment particles by their uniform scattering. In the fabricated AMCs, W
nanoparticles obstructed the dislocations and generate a loop/pinning
(9)
From Table 5, it can be seen that the contribution of dispersion
strengthening is more towards the strengthening of AMCs on total
strength. In this research work, the sequence of strengthening contribu-
tion on total strength is σdisper, σdis, and σGB.
Abundant research works were conducted in the field of FSP by re-
inforcing ceramic particles as reinforcement. The main limitation in ce-
ramic particle addition is the reduction in % elongation and poor wet-
tability. Hence, in recent times, researchers introduced high-tempera

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Fig. 9. Mechanical behaviour of Al 6063 – x vol% W (x = 0, 3, 6, 9 and 12) nanocomposites: (a) engineering stress-strain curves; (b) schematic representing the failure that occurs in SZ
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during tensile test; (c) variation of work hardening rate against the true strain.

Table 2 4. Conclusions
Tensile properties obtained from the engineering stress-strain curves.

Reinforcement (vol%) YS, (MPa) UTS, (MPa) Elongation (%) • The Aluminium matrix composites using AA 6063 alloy as matrix
and W nanoparticles were effectively fabricated through the FSP tech-
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0 128.85 208.37 25
nique. The vol% of reinforcement was varied from 0 to 12% with the
3 145.06 240.07 24
6 140.67 280.66 22
variation of 3 vol%.
9 162.46 319.83 21 • The W nanoparticles reinforced in the AA 6063 matrix were retained
12 178.68 360.45 18.5 in elemental form after processing which confirms the inhibition of
reaction between Al and W nanoparticle due to a huge mismatch be-
tween the melting point of Al and W.
• The reinforced W nanoparticles were dispersed uniformly throughout
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ture metallic material; which is highly difficult to soluble in a matrix

material to retain the ductility of the material. Table 6 exemplifies
the comparison of similar works illustrating the addition of metallic
particles (W, Va, Mo, Ti, Ni) in the Al matrix through the FSP tech-
nique. Huang et al., [25] had achieved 432 MPa of UTS with reasonable
ductility of 23.2% with the addition of 8 vol% Ti particles. Nonethe-
less, in this present research, the authors achieved the maximum UTS
of 360.45 MPa and 18.5% elongation with the addition of 12 vol% W
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the stir zone of the Al matrix. A clear interface was observed between
the matrix and reinforcement particles without any inhibition of reac-
tion regarding the diffusion of W nanoparticles in the Al matrix.
• Extraordinary grain refinement was observed in Al 6063 – x vol%
W composite (x = 0, 6 and 12). The grain size of the 0, 6, and
12 vol% W reinforced specimens are 42 ± 08 μm, 2.81 ± 08 μm, and

nanoparticles. Based on the literature reviewed by the authors and by
considering the obtained results in the present work, it can be sum-
marised that the second phase metallic particle (high temperature melt-
ing element) incorporation in the matrix can inhibit the grain growth
during recrystallization due to the Zener pinning effect. The FSP tech-
nique can refine the matrix grains from coarser to ultrafine level with
a clear interface and excelling bonding without any defects. Hence, FSP
is a promising technique to produce AMCs to obtain higher mechanical
properties without a huge loss in ductility.
0.97 ± 0.6 μm, respectively. The strength of the AMCs was obtained
from reinforced W nanoparticles, grain refinement, and accumulation
of dislocations in GBs.
• In this research of AMCs, the strengthening mechanisms were calcu-
lated to identify individual strengthening (i.e.). It can observe that
the obtained strength was highly correlating with the YS of the scope.
The sequence of strengthening contribution on total strength is disper-
sion strengthening, dislocation strengthening, and grain size strength-
ening.

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Fig. 10. Fracture morphology of tensile test specimen (a) unreinforced Al 6063 matrix, (b) Al 6063–6 vol% W nanocomposite, (c) Al 6063–12 vol% W nanocomposite; (d) EDS results of
(d).
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Table 3 Table 4
Intercept and strain hardening exponents obtained from true stress -true strain curves. Parameters with their nomenclature used in strengthening mechanism.

Strain hardening Parameter Nomenclature Values Unit

Reinforcement (vol%) Intercept, K, (MPa) exponent, n
σO Friction stress MPa
0 782.61 0.3666 K Constant 0.04 MPa
3 943.91 0.3111 m 1/2
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6 1268.41 0.4711 d Average grain size μm

9 1040.32 0.3724 α Constant 0.3
12 1810.66 0.3638 G Shear modulus 26.9 GPa
b Burgers vector 0.28 Nm
ΔT Processing peak and ambient temperatures K
variation
Author contributions ΔC CTE mismatch between Al and W. 19.3 × 10 − 6 K−1
(CTEAl = 23.6 × 10 − 6;
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L. Feroz Ali: Formal analyses, Investigation and Writing; N. Kup- CTEw = 4.3 × 10 − 6)
Vp Vol. fraction of W particles %
pusamy: Supervision, Funding acquisition; R. Soundararajan: Resources, dp Avg. size of W particles Nm
Methodology; K.R.Ramkumar: Conceptualization, Ideology, Data cura- υ Poisson's ratio
tion, Correcting original draft; S.Sivasankaran: Validation; Visualization, ro Dislocation core radius ro = 4b
Writing - review & editing. λ Inter-particle spacing
V Vol. fraction of W particles %
M Taylor factor 3
Data availability statement
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The experimental datasets obtained from this research work and then
the analysed results during the current study are available from the cor-
responding author on reasonable request.

Declaration of Competing Interest

The authors declare no conflict of interest.

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L.Feroz Ali et al. Materials Characterization xxx (xxxx) xxx-xxx

Table 5
Contribution of various strengthening mechanism to the total strength.

Reinforcement σgs σDisper σDis σCal Obtained YS

(vol%) (MPa) (MPa) (MPa) (MPa) (MPa)

6 55.72 67.24 39.21 95.73 143.34

12 88.14 98.02 60.25 144.93 180.12

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Table 6
Comparison of similar works conducted by various researchers with this present work.

No. Authors System Size of the reinforcement Grain size after processing UTS, (MPa) % elongation Ref.
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1. Dixit et al. Al – 3.6 vol% W 550 nm 3 μm 128.8 ± 6.8 21.4 ± 3.3 [8]
2 Huang et al. Al 1060–24 vol% W 5 μm – 126.41 24.73 [9]
3. Abraham et al. Al 6063 / Vandium 18 μm 7.6 μm 268 20 [18]
4. Selvakumar et al. Al 6082–18 vol% Mo 18 μm 6 μm 303 14 [19]
5. Bauri et al. Al 5083–10 vol% W 10 μm 3.6 μm 404 ± 23 30 ± 1 [20]
6. Yadav and Bauri AA 1050–7 vol% Ni – 3 μm 127 25 [24]
7. Huang et al. Al 5083–8 vol% Ti 23 μm 1 μm 432 23.2 [25]
8. Present work Al 6063–0 vol% W 38 ± 09 nm 42 ± 08 μm 208.37 25 –
Al 6063–3 vol% W 38 ± 09 nm - 240.07 24
Al 6063–6 vol% W 38 ± 09 nm 2.81 ± 04 μm 280.66 22
Al 6063–9 vol% W 38 ± 09 nm - 319.83 21
Al 6063–12 vol% W 38 ± 09 nm 0.97 ± 0.6 μm 360.45 18.5

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L.Feroz Ali et al.
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