Materials Characterization 108 (2015) 102–114

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Materials Characterization

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

Friction stir processing of an aluminum-magnesium alloy with

pre-placing elemental titanium powder: In-situ formation of an
Al3Ti-reinforced nanocomposite and materials characterization
F. Khodabakhshi a,⁎, A. Simchi b,c, A.H. Kokabi b, A.P. Gerlich d
a
Department of Materials Science and Engineering, School of Engineering, Shiraz University, Zand Boulevard, Shiraz, Iran
b
Department of Materials Science and Engineering, Sharif University of Technology, P.O. Box 11365-9466, Azadi Avenue, 14588 Tehran, Iran
c
Institute for Nanoscience and Nanotechnology, Sharif University of Technology, P.O. Box 11365-9466, Azadi Avenue, 14588 Tehran, Iran
d
Department of Mechanical and Mechatronics Engineering, University of Waterloo, Waterloo, ON, Canada

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

Article history: A fine-grained Al–Mg/Al3Ti nanocomposite was fabricated by friction stir processing (FSP) of an aluminum-magne-
Received 19 May 2015 sium (AA5052) alloy with pre-placed titanium powder in the stirred zone. Microstructural evolutions and formation
Received in revised form 13 August 2015 of intermetallic phases were analyzed by optical and electron microscopic techniques across the thickness section of
Accepted 27 August 2015
the processed sheets. The microstructure of the nanocomposite consisted of a fine-grained aluminum matrix
Available online 29 August 2015
(1.5 µm), un-reacted titanium particles (b40 µm) and reinforcement particles of Al3Ti (b100 nm) and Mg2Si
Keywords:
(b100 nm). Detailed microstructural analysis indicated solid-state interfacial reactions between the aluminum ma-
Friction stir processing trix and micro-sized titanium particles to form Al3Ti intermetallic phase. The hard inclusions were then fractured
Intermetallic nanocomposite and re-distributed in the metal matrix by the severe thermo-mechanical conditions imposed by FSP. Evaluation of
Aluminum–magnesium alloy mechanical properties by hardness measurement and uniaxial tensile test determined significant enhancement in
Al3Ti the mechanical strength (by 2.5 order of magnetite) with a high ductility (~22%). Based on a dislocation-based
Microstructure model analysis, it was suggested that the strength enhancement was governed by grain refinement and the pres-
Mechanical properties ence of hard inclusions (4 vol%) in the metal matrix. Fractographic studies also showed a ductile-brittle fracture
mode for the nanocomposite compared with fully ductile rupture of the annealed alloy as well as the FSPed speci-
men without pre-placing titanium particles.
© 2015 Elsevier Inc. All rights reserved.

1. Introduction
Particulate-reinforced metal matrix composites (PMMCs) are of
great interest for structural and electrical applications considering
their industrially feasible processing, low cost, and isotropic proper-
ties [1,2]. Advances in processing and applications of PMMCs relate to
utilizing nanometric reinforcements and refining the grain structure in
order to activate higher strength with reasonable ductility [3,4]. Numer-
ous studies have been performed on the microstructure-property rela-
tionship in various metal-matrix nanocomposites [1,2,5,6]. In
particular, aluminum matrix nanocomposites (AMMNCs) have been in-
tensively studied [7,8]. These nanocomposites are fabricated by various
techniques that can be classified in solid-state, liquid-state and deposi-
tion processes [9–12]. One of the most widespread methods to prepare
AMMNCs is the powder metallurgy route [13–18]. By employing this
method, a fine distribution of the reinforcement nanoparticles in the
aluminum matrix with no or limited reactions between the metal
⁎ Corresponding author.
E-mail address: farzadkhodabakhshi83@gmail.com (F. Khodabakhshi).
matrix and the nanoparticles are achievable [12]. An alternative ap-
proach is friction stir processing (FSP), which has recently attracted a
great attention for the fabrication of PMMCs at surfaces of base metals
[19–21]. Many feasibility studies have been performed on processing
of AMMNCs [19,21,22] as well as many other systems [13,23–31]. In
this process, a non-consumable tool with a concentric shoulder and spe-
cific pin design is plunged into the metal matrix workpiece [32]. By
adding second phase nanoparticles ahead of the tool during processing,
surface modifications are attained [33,34]. Solid-state chemical reac-
tions may also occur upon processing, which can lead to the in-situ for-
mation of reinforcing particles [12]. The advantage of this process a
more homogeneous microstructure with stronger interfacial bonding
of the nanoparticles to the metal matrix [8]. The role of FSP is to provide
the following functions: (i) severe plastic deformation to promote
mixing and refining of the constituent phases in the material, (ii) elevat-
ed temperature to facilitate the chemical reactions, and (iii) hot consol-
idation to form a fully dense solid [35].
It is well known that aluminide intermetallics such as Al3Ni, Al3Ti,
Al3Fe, and Al2Cu have high wear resistance, hardness, specific strength,
specific modulus, and excellent stability both at ambient and elevated
temperature [36]. Therefore, aluminum alloys reinforced with

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 F. Khodabakhshi et al. / Materials Characterization 108 (2015) 102–114 103

Fig. 1. (a) SEM image and (b) atomic absorption analysis result for the titanium particles. (c) Schematic representation of sample extraction from FSPed Al–Mg alloy and Al–Mg–Ti
composite for different microstructural analysis techniques, hardness measurements, and tensile testing.

aluminide particles have attracted much attention during the last two
decades due to their interesting mechanical properties [37–40]. Prepa-
ration of these nanocomposites by FSP is also attractive because the
aluminide reinforcing particles can efficiently be fractured, refined,
and dispersed by the thermo-mechanical processing conditions. Re-
cently, Al–Al2Cu [41,42], Al–Al3Ni [29,43], Al–Al3Fe [44] and Al–Al3Ti
[42,45–47] composites have been successfully fabricated by employing
FSP on Al–Cu, Al–Ni, Al–Fe and Al–Ti elemental powder mixtures, re-
spectively. As compared to the other aluminide phases, aluminum-
rich titanium intermetallic (Al3Ti) is very attractive due to its unique
properties, such as high melting point (~1350 °C), relatively low density
(~3.4 g.cm−3), high Young's modulus (~216 GPa), and low coarsening
rate at elevated temperatures [48]. Studies on Al–Al3Ti composites fab-
ricated by ingot metallurgy [49], mechanical alloying [50,51], rapid so-
lidification [52] and combustion synthesis [53] have shown the
potential of Al3Ti particles to improve the stiffness of aluminum alloys.
Recently, Hsu et al. [42,47] and Zhang et al. [45,46,54] have examined
the in-situ formation of Al3Ti particles during FSP of Al/Ti powder mix-
tures. More recently, we have also shown the in-situ formation of Al3Ti
nanoparticles upon FSP of an Al–Mg alloy with pre-placed TiO2 nano-
particles [55–62]. The role of the in-situ formed particles on the micro-
structural evolutions and mechanical properties have been reported in
details.
In the present work, elemental titanium powder is employed instead
of TiO2 nanoparticles. Our previous results have shown that several
chemical reactions between the constituents (Al, Mg, Si, Ti and
O) occur during FSP that form different phases including MgO and
Al3Ti. Although enhanced mechanical strength was attained, magne-
sium oxidation reduces the age hardening potential of the aluminum
matrix. Analysis of the strengthening mechanisms were also difficult
as multiple and complex phases were formed. The aim of this work is
to study the fragmentation and dissolution of titanium particles in the

Table 1
The atomic absorption chemical analysis results from the initial titanium reinforcing particles (conditions for atomic absorption analysis were set as; accelerating voltage of 20 kV, beam
current of 500 pA, magnification of 60, live time of 40 s, preset time of 40 s, Nb channels of 2048, Ev/channel of 10, offset of 0 keV, and width of 20 keV).

Element Line Int Error K Kr W% A% ZAF Formula Ox% Pk/Bg Class LConf HConf Cat#

Ti Ka 1952.7 2.7983 1.0000 1.0000 100.00 100.00 1.0000 0.00 125.24 A 99.28 100.72 0.00
1.0000 1.0000 100.00 100.00 0.00 0.00

# These numbers are the outputs of atomic absorption chemical analysis.

104 F. Khodabakhshi et al. / Materials Characterization 108 (2015) 102–114
Fig. 2. Stereographic macro-images display the stir zone flow pattern of friction stir
processed (a) Al–Mg alloy and (b) Al–Mg–Ti composite.
Al–Mg matrix during severe plastic deformation and heat flow upon
FSP. The effect of magnesium on the in-situ chemical reactions and its
role on the formation of intermetallic phases are elaborated. Additional-
ly, the mechanical properties of the nanocomposites are examined and
Fig. 3. Optical microstructures for BM, HAZ, TMAZ and SZ of FSPed Al–Mg alloy at different magnifications.
compared with the base metal, as well as the nanocomposites prepared
by pre-placed TiO2 nanoparticles in previous studies.
2. Experimental procedure
2.1. Materials
Commercial aluminum–magnesium alloy (5052-H32 rolled and
tempered sheet) with a chemical composition of Al–2.23 Mg–
0.292Fe–0.163Cr–0.147Si–0.114Mn–0.0077Zn–0.0065Cu (in wt.%) and
thickness of 5 mm was supplied from Arak Aluminum Company, Arak,
Iran. The sheet was cut into 210 × 70 mm2 specimens and solution-
treated by annealing at 500 °C for 2 h followed by water quenching. Ti-
tanium powder with a commercial purity of 99.9%, and an average par-
ticle diameter of 40 μm was purchased from Merck Company
(Germany). Morphological and chemical analyses of the titanium pow-
der are presented in Figs. 1a,b and Table 1, respectively.
2.2. Friction stir processing
A groove with a width of 1.2 mm and depth of 3.5 mm was machined
in the middle of the sheets and filled with the titanium powder (~0.6 g).
After tapping with hand, a capping FSP pass was performed by employing
a tool with a shoulder (12 mm diameter) having no pin. A modified mill-
ing machine was used to conduct the FSP experiments. By trail-and-error,
it was found that the suitable parameters for the accomplishment of the
capping pass without severe vibrations were: rotational speed (w) of
1125 rpm and traverse velocity (v) of 30 mm/min. The FSP tool was
made of H13 steel with a concave shape shoulder (diameter of 18 mm
and concave angle of 2.5°) and a cylindrical threaded pin (height of
 F. Khodabakhshi et al. / Materials Characterization 108 (2015) 102–114 105

Fig. 4. Optical microstructures for BM, HAZ, TMAZ and SZ of FSPed Al–Mg–Ti composite at different magnifications.

4 mm, diameter of 5 mm, M5 threads). A counterclockwise rotational kept around 2.5°. Multi-passes FSP was performed to incorporate the
speed of 1200 rpm and a traverse velocity of 100 mm/min were used. Ti particles into the Al matrix uniformly and to pursue Al/Ti solid-state
The nuting angle with respect to the normal axis of sample plane was chemical reactions. The processing conditions were not changed for

Fig. 5. Optical micrographs showing the distribution of reinforcement particles within the grain interior as well as along the grain boundaries of the Al–Mg metal matrix.
106 F. Khodabakhshi et al. / Materials Characterization 108 (2015) 102–114
Fig. 6. FE-SEM images display the titanium particles dispersion through the aluminum matrix.
repeated passes but 100% overlap was considered. The pressing depth
of tool shoulder for each FSP passes was set to ~0.2 mm via a displace-
ment control unit. Based on the groove dimensions and the weight of
the Ti powder, the amount of the Ti incorporated in the matrix was
about ~ 3 vol.%. The base Al–Mg alloy was also FSPed at the same pro-
cessing conditions to explore the role of Ti addition. The results of mi-
crostructural evaluations and mechanical examinations were also
compared with the nanocomposites prepared by pre-placing TiO2
nanoparticles [55,58–60,62] in order to highlight the effect of additive
type.
2.3. Microstructural characterization
The processed samples were cross-sectioned perpendicular to the
FSP direction by electron discharge machining to examine the micro-
structure as schematically shown in Fig. 1c. Standard metallographic
procedures were employed through grinding with SiC papers followed
by polishing with diamond pasts. The polished cross-sections were
chemically etched by modified Poulton's reagent consisting of two solu-
tions (H2O (1 ml)–HNO3 (6 ml)-HF (1 ml)–HCl (12 ml)/HNO3 (25 ml)–
H2CrO4 (1 g)–H2O (10 ml)). Microstructural studies of different zones
including base metal (BM), heat affected zone (HAZ), thermo-
mechanical affected zone (TMAZ) and stir zone (SZ) were examined
using stereographic (Nikon, USA) and optical (Olympus, Germany) mi-
croscopes. The average grain size of different regions was measured
by the mean linear intercept method. Further microstructural exam-
inations were performed by field emission-scanning electron
microscopy (FE-SEM, JEOL 7600, Japan). Line-scan and elemental
concentration profiles for the dispersed initial reinforcing particles
and newly formed intermetallic phases were investigated by energy
dispersive X-ray spectroscopy (EDS) analysis. For characterization
and identifying in situ reactions and new formed phases scanning
transmission electron microscopy (STEM; JEM-2100 F STEM, JEOL,
Japan) and high resolution-transmission electron microscopes
(HRTEM; Philips, Netherlands) were utilized. The sample prepara-
tion approach for FESEM samples was similar to that used for STEM
and HRTEM samples comprehensively explained in prior works [58,
62].
2.4. Mechanical testing
Details of samples extraction for different mechanical testing are in-
dicated in Fig. 1c, schematically. The hardness profile along different
zones of the FSPed specimens was recorded on the metallographic
cross-sections utilizing a Vickers micro-hardness indenter (Bohler,
Germany). The measurement was performed underneath the top sur-
faced with 2 mm distance. The applied load was 200 g with a 15 s
dwell time. Thin rectangular specimens (3 mm thickness) with a gage
length of 32 mm and a width of 6 mm were prepared in longitudinal
and perpendicular directions (relative to the FSP line) according to
ASTM E8M standard. The stir zone was located in the gage length. A
Universal Tensile Loading Machine (Model H10K, Tinius Olsen, USA)
with an initial strain rate of 5 × 10−4 s−1 was employed. Triplicate spec-
imens were examined for each conditions and materials, and the aver-
age values were reported. After fracturing, the cross-section was
observed by FE-SEM.
 F. Khodabakhshi et al. / Materials Characterization 108 (2015) 102–114
Fig. 7. A magnified view by FE-SEM images at large magnifications demonstrate the Al–Mg
matrix/Ti particles interface and formation of in situ Al3Ti nanoparticles. The white phase
is titanium, the light gray phase is Al3Ti, and the dark matrix is Al–Mg alloy.
3. Results
3.1. Materials flow and grain structure
The patterns of material flow for the processed Al–Mg alloy without
and in the presence of Ti particles are shown in Fig. 2a and b, respective-
ly. It is apparent that the processed zone of both samples exhibited an
onion ring flow structure, while the intensity and sharpness of the
banded structure is increased significantly when the Ti powder is
added. It is clear that the incorporation of Ti particles during FSP has dra-
matically influenced the material flow and geometry of the stir zone. It
seems that a homogenous distribution from Ti micro-particles through
SZ was achieved after employing of FSP for four passes. Figs. 3 and 4
show microstructural features of different zones (BM, HAZ, TMAZ, and
SZ) formed upon FSP of Al–Mg alloy without and with Ti particles, re-
spectively. The base metal consisted of a relatively coarse grain struc-
ture (~ 49 μm), while a relatively uniform microstructure with an
average size of ~ 20 μm were formed after FSP (Fig. 3a–c), indicating
that dynamic recrystallization (DRX) occurred during FSP. Microstruc-
tural studies revealed that the addition of secondary particles led to a
significant grain refinement. The average size of grains for the processed
alloy in the presence of Ti particles was about 1.5 μm, as demonstrated
in Figs. 4a–c and 5a–d. It should be noted that, the FE-SEM results in
Figs. 6–9 and STEM images of Fig. 10 should be considered supplemen-
tary microscopy in determining the mean size of SZ high angle grain
structure in the composite sample.
107
3.2. Analysis of secondary phases
Optical micrographs and FE-SEM images in Figs. 5 and 6 respectively,
show details of microstructural features in SZ for the FSPed Al–Mg alloy
in the presence of Ti particles. Fig. 7 shows the high magnification FE-
SEM images of the FSPed composite. Relatively coarse Ti particles
(white contrast particles in the FE-SEM images and brown contrast in
the optical micrographs) and round Al3Ti particles with a diameter
b100 nm were observed. The volume fraction of the Ti particles was ap-
proximately 2% based on quantitative microstructural analysis of FE-
SEM images in Figs. 6 and 7. Since, Al3Ti is the only reaction product be-
tween Al and Ti elements, the amount of in situ formed Al3Ti intermetal-
lic nanoparticles was calculated from the volume fraction of residual Ti
as 4 vol.% based on a mass balance calculation. Also, it should be noted
that the Al3Ti intermetallic phases were observed close to the Ti parti-
cle/matrix interfaces (Fig. 7a,b), supporting the occurrence of solid-
state chemical reactions between the aluminum matrix and titanium
particles. Fig. 8 shows FE-SEM images and the corresponding elemental
maps for the processed specimen. For this studied composite system, as
seen in Fig. 8a at low magnification, no Mg-rich particles were found,
and Mg was distributed into the Al matrix, however, the distribution
of Mg in the matrix was nonhomogeneous. Although in elemental
maps of Fig. 8b at high magnification, some weak intensities of ultra-
fine Mg rich particles were detected. Based on the previous research
on the Al–Mg–Ti complex system [63,64], these particles maybe FCC
structured Ti2Mg3Al18, however in the present work these are not Al
and Ti rich. Therefore, these nano-metric round phases are likely
Mg2Si particles which formed as a result of re-precipitation of some sol-
ute Mg atoms during FSP, since there is 0.147% Si in the base metal and
this would be comparable to the AA6000 series alloy which are mainly
strengthened by Mg2Si [18,65]. These nano-scaled Mg2Si precipitates
can contribute to secondary strengthening of the Al matrix around the
Al3Ti nanoparticles. Line-scan EDS analysis results from different size
particles combined with FE-SEM images in Fig. 9 are in agreement
with the obtained findings from elemental mappings analysis. Micro-
structural features including the sub-grains structure, dislocations ori-
entation, and twinning produced by severe plastic deformation of Al
matrix at SZ are shown in STEM and HR-TEM images of Fig. 10a–c.
High magnification STEM images from the in situ formed Al3Ti nanopar-
ticles in the Al matrix are displayed in Fig. 10d–f. An HR-TEM image
from the Al matrix/Al3Ti interface shown in Fig. 10g, indicating a good
crystallographic matching between the newly formed reinforcement
phase during processing and the metal matrix. Corresponding selected
area diffraction (SAD) spot patterns for the in situ Al3Ti phase and the
severely deformed Al matrix from [110] zone axis are shown in
Figs. 10h,i, respectively. By indexing the SAD pattern of Fig. 10h, it was
confirmed that those nano-metric Ti reach particles detected by FE-
SEM analysis are Al3Ti phase. Typical reported results of microstructural
analysis for the processed sample with TiO2 nanoparticles in the previ-
ous studies [58–60,62] were revealed the in situ formation of MgO
and Al3Ti phases, as the kinetics for Mg2Si precipitates formation were
restricted, attributed to a higher chemical affinity of magnesium to oxy-
gen than that of titanium.
3.3. Mechanical properties
Micro-hardness profiles across SZ for the Al–Mg alloy and Al–Mg–Ti
system are plotted in Fig. 11a. The mean Vickers hardness values for dif-
ferent zones of BM, HAZ, TMAZ, and SZ are reported in Table 2. The base
metal exhibited a uniform hardness across the cross section with an av-
erage value of ~51 HV. An increased (~16%) in the hardness of SZ was
attained after FSP without the addition of the secondary particles. How-
ever, the hardness was ramp up in SZ to ~131 HV (~156% increment)
when the titanium particles were introduced. The heterogeneous hard-
ness profile was attributed to the presence of distributed coarse Ti par-
ticles (Figs. 5 and 6). Fig. 11b shows the engineering stress-strain curves
108 F. Khodabakhshi et al. / Materials Characterization 108 (2015) 102–114

Fig. 8. FE-SEM images combined with the elemental mapping analysis results.

Fig. 9. Line scan analysis from reinforcement particles with three different sizes.
 F. Khodabakhshi et al. / Materials Characterization 108 (2015) 102–114 109

Fig. 10. (a) Bright-, (b) dark-field STEM, and (c) HR-TEM images from the hot severely deformed structure of SZ showing dislocations, twin boundaries, sub-grains, and the other
microstructural features. (d–f) High magnification STEM images from the in situ formed Al3Ti nanoparticles, and (g) HR-TEM image from the Al–Mg matrix/Al3Ti interface. The SAD
spot patterns for (h) the in situ Al3Ti phase and (i) the deformed Al matrix.

for the examined materials. The main mechanical characteristics obtain-
ed from these graphs are summarized in Table 2. The annealed Al–Mg
alloy exhibited relatively low yield stress (YS, ~ 68 MPa) and ultimate
tensile strength (UTS, ~ 180 MPa) with high elongation (~ 29.5%). A
slight enhancement in the strength and elongation was achieved after
FSP of the Al–Mg alloy due to grain structural refinement because of op-
erating DRX mechanism occurred in the SZ during the processing. The
addition of Ti particles enhanced the longitudinal tensile strength to
values of 151 MPa (yield) and 246 MPa (ultimate) with a decrease in
the tensile elongation to 22%, which are more significant are much im-
provements than the measured values in previous works [58–60,62]
for the FSPed Al–Mg–TiO2 system. By incorporating the ex situ Ti
micro-particles and subsequently forming new in situ Al3Ti nano-
particles during FSP process, dislocation density around the reinforcing
particles is increased significantly while simultaneously refining the
grains due to elastic mismatch and particle stimulated nucleation mech-
anisms, respectively [46,47,54,66]. As a result, the hardness and tensile
strength of the processed nanocomposite was enhanced and the elon-
gation reduced as compared to the initial and processed Al–Mg alloys.
However, it can be noted that the magnitude of elongation is
remarkable. Much lower mechanical properties were measured upon
transverse tensile testing as the specimens were fractured from the
SZ/TMAZ interface.
3.4. Fracture behavior
The fracture surface of the tensile tested specimens was observed by
FE-SEM to study the failure mechanisms. Fig. 12 shows typical micro-
graphs of the fracture surfaces. The annealed Al–Mg alloy exhibited a
ductile rupture behavior with characteristics of gray fibrous surface
with dimples and the presence of shear zones (Fig. 12a–c). As shown
in the related stress–strain graph of Fig. 11b, significant deformation
and considerable amount of necking was observed in this sample. No
major difference was observed for the FSPed Al–Mg alloy except finer
dimple sizes (Fig. 12d–f), which could be related to its finder grain
structure [60]. The presence of a gray fibrous surface with dimples in
these non-reinforced samples demonstrates the fracture mode was a
shear ductile rupture. Deep and elongated dimples are the results of nu-
cleation of micro voids, their growth and finally coalescence of dimples
which are affected by shear stress [67]. It was found that the presence of
110 F. Khodabakhshi et al. / Materials Characterization 108 (2015) 102–114

Fig. 11. (a) Micro-hardness profiles across thickness section of annealed Al–Mg alloy be-
fore and after FSP, and FSPed Al–Mg–Ti composite. (b) Engineering stress-strain curves
display transverse and longitudinal tensile flow behaviors of FSPed Al–Mg–Ti composite
in comparison to the annealed Al–Mg alloy before and after FSP.
reinforcement particles have a significant influence on the fracture sur-
face features. As shown in Fig. 12g–i, the fracture surface of the Al–Mg
alloy with the addition of Ti particles showed a ductile–brittle failure
mechanism. Fine dimples without significant shear tearing were ob-
served. Some cracked particles were found on the fracture surface of
composite sample (gray arrows in Fig. 12g–i). Particles were seen in
the core of most dimples, supporting the role of particle-matrix inter-
face on the rupturing [68]. EDS analysis determined that those particles
were mostly Al3Ti and un-reacted Ti particles, as the results are present-
ed in Fig. 13. The related regions for these EDS analysis are indicated on
the FE-SEM fractographs of different samples in Fig. 12c,f,i.
4. Discussion
4.1. Effect of secondary particles on the grain structure
As shown in Fig. 3, the initial annealed Al–Mg base metal posses coarse
grain structure with an average size ~49 μm, and this microstructure was
refined to equiaxed grains with size of ~20.3 μm after employing FSP for
four passes without introducing the reinforcement particles. It is sug-
gested that once a given volume of plastically deformed material was
located the outside the deformation zone of the rotating tool pin, it
has coarsened very quickly under the influence of heat [69]. For both
processed samples, a sharp transition in grain size can be noted moving
from the BM toward the SZ grain structure, with drastic refinement
clearly visible. In the Al–Mg alloy with an initial solution-treated condi-
tion, discontinuous dynamic recrystallization (DDRX) can occur during
the hot deformation conditions involved during FSP, and the tendency
for DDRX to occur can be attribute to the moderate to low stacking
fault energy in this alloy [58,60]. In DDRX, new, dislocation-free grains
form at sites such as prior grain boundaries, deformation band inter-
faces or boundaries of newly recrystallized grains when a critical dislo-
cation density is achieved within the grains [70]. The driving force for
initiation of recrystallization is the strain-induced build up of stored
strain energy in the form of fine dislocation cells and a high density of
mobile dislocations [71]. After FSP of the Al–Mg–Ti composite system,
as a result of the in situ reactions promoting intermetallic phase forma-
tion, the average grain size of SZ was reduced significantly down to
~1.5 μm, as shown in Figs. 5 and 8a. Insoluble nanoparticles can provide
suitable sites to enhance the nucleation rate of new grains at the begin-
ning of DDRX by particulate stimulated nucleation (PSN) [72], and sub-
sequently the rate of grain boundary migration would have been
hindered by Zener–Holloman pinning (ZHP) mechanism also contribut-
ed by the fractured Ti powder particles and other fine nucleated parti-
cles which will be discussed shortly [73]. Both of these PSZ and ZHP
mechanisms operate in concert and lead to enhanced grain refinement
during FSP. Hence, multiple microstructural and phase transformational
phenomena are operating during FSP of Al–Mg–Ti composite, which led
to a grain structure in the SZ which seems to be bimodal in size
distribution.
4.2. Formation mechanisms of intermetallic phases
As revealed in previous works for FSPed Al–Mg–TiO2 system [59,62],
the in situ solid-state reactions during FSP is controlled by diffusion of
Mg in the Al matrix/TiO2 nanoparticles interface and as a result, the
MgO phase is formed according to deformation-assisted interfacial
chemical reaction mechanism. As the reaction proceeds, titanium
atoms will dissolute in the aluminum matrix to form Al3Ti at the parti-
cles–matrix interface by deformation-assisted solution–precipitation
mechanism. However, different mechanisms of in situ phase formation
are observed in this study for the FSPed Al–Mg–Ti intermetallic system.
High magnification FE-SEM images in Fig. 7 provide some indication of
the mechanism for reactive diffusion between Al and Ti. At first, Al3Ti
phase formed at the outer layer of the initial Ti micro-particles and a
structure like core-shell produced. The difference in the diffusion coeffi-
cients between Ti in Al during the Al–Ti inter-diffusion would create va-
cancies in the Al as a result of Kirkendall's effect, thereby causing a
volume expansion in Ti [47,66]. Furthermore, the density of Al3Ti is
lower than that of Ti, hence the formation of Al3Ti would cause a consid-
erable volume expansion. The volume expansion would produce tensile
stresses in the outer layer of the particles and compressive stress in the
core of the particles, and this resulted in the initiation of some micro-

Table 2
Tensile and indentation properties for different zones (BM, HAZ, TMAZ, and SZ) of the friction stir processed Al–Mg alloy and Al–Mg–Ti composite: Elastic modulus (E, MPa); Yield stress
(YS, MPa); Ultimate tensile strength (UTS, MPa); Elongation (e, %); Fracture stress (FS, MPa); Micro-hardness (HV, Vickers).

Properties Tensile properties Vickers hardness

Sample Condition Orientation E YS UTS e FS BM HAZ TMAZ SZ

Al–Mg Annealed Longitudinal 70 68 180 29.5 159 51.1 ± 0.6 – – –

Al–Mg FSP Longitudinal 71 65.3 194.4 33.2 158.8 51.1 ± 0.6 51.1 ± 0.6 51.6 ± 0.8 59.5 ± 2.0
Al–Mg–Ti FSP Transverse 72 92.5 195.0 14.0 183.4 51.1 ± 0.6 51.1 ± 0.6 57.8 ± 8.7 130.6 ± 20.6
Al–Mg–Ti FSP Longitudinal 76 151.5 246.2 22.2 209 – – – –
 F. Khodabakhshi et al. / Materials Characterization 108 (2015) 102–114
Fig. 12. FE-SEM images show the fracture surfaces of (a–c) initial Al–Mg alloy, (d–f) FSPed Al–Mg alloy, and (g–i) FSPed Al–Mg–Ti composite at (a, d, g) 200×, (b, e, h) 1000×, (c, f, i) and
2000× magnifications.
cracks in the Al3Ti as the reaction proceeded during multi-pass FSP
(STEM images of Fig. 10d–f). The number of micro-cracks would be in-
crease with the volume expansion increases. The large brittle Al3Ti
blocks can be easily broken into smaller particles with sizes b100 nm
due to the existence of these micro-cracks and imposed intense plastic
deformation during continuation of FSP process. According to the result
of elemental maps (Fig. 8) and EDS analysis (Fig. 9), no Mg-containing
intermetallics were formed in the FSPed Al–Mg–Ti sample and Mg dis-
solved into the Al matrix, although its distribution was non-uniform
due to formation of nano-metric Mg2Si precipitates. The presence of sol-
ute Mg would facilitate the Al–Ti inter-diffusion at the Al–Ti interface to
form Al3Ti particles as a result of the Al–Ti reaction. The severe plastic
deformation during FSP, would promote a thermo-mechanically acti-
vated condition which removed the Al3Ti particles from the Al–Ti inter-
face and distributed them into the Al–Mg metal matrix uniformly.
4.3. Modeling of mechanical properties
4.3.1. Elastic modulus
With the incorporation of titanium particles through Al–Mg metal
matrix during FSP, the Young's modulus of prepared in situ intermetallic
reinforced nanocomposite was increased noticeably in comparison to
Al–Mg base metal or FSPed Al–Mg alloy without pre-placed particles
as shown in Table 2, which can be attributed to the high elastic modulus
of Al3Ti phase. The Young's modulus of particulate-reinforced compos-
ites can be predicted from the Halpin–Tsai equation as follows [74]:


Em Ep ð1 þ ηV Þ þ ηEm ð1−V Þ
Ec ¼
Ep ð1−V Þ þ Em ðη þ V Þ
111
where Ec, Em, and Ep are the elastic modulus of the composite, metal ma-
trix, and reinforcing particles, respectively, η is an adjustable parameter,
and V is the volume fraction of the particles. For the prepared Al–Mg–
Al3Ti nanocomposite, Em = 70 GPa and Ep = 216 GPa [75]. By taking
η = 1, the calculated Young's modulus of FSPed in situ intermetallic
nanocomposite with 4% volume fraction of Al3Ti nanoparticles is report-
ed in Table. 3. As seen, the Measured Young's modulus of Al–Mg–Al3Ti
nanocomposite agrees well with the prediction of the Halpin–Tsai equa-
tion. This suggests that there is good bonding strength between Al3Ti
nanoparticles and the Al matrix so that in situ formed Al3Ti nanoparti-
cles can contribute effectively to load sharing in the nanocomposite.
4.3.2. Yield strength and strengthening mechanisms
Four possible strengthening micro-mechanisms which may operate
in particulate-reinforced metal matrix nanocomposites are [76]; (i)
grain and substructure strengthening, (ii) Orowan strengthening, (iii)
quench hardening resulting from the dislocations generated to accom-
modate the differential thermal contraction between the reinforcing
nanoparticles and the metal matrix, and (iv) work hardening due to
the strain misfit or elastic modulus mismatch between the elastic rein-
forcing particles and the plastic matrix. Due to the low aspect ratio of re-
inforcing phases in particulate nanocomposites, the contribution of load
transferring mechanism is negligible. By considering the superimposed
effects of Hall–Petch strengthening (σH − P), Orowan strengthening
(σOR), coefficient of thermal expansion (σCTE) and elastic modulus mis-
match (σEM), the strength of the matrix can be expressed as [77]:
σ c ¼ σ m þ σ H−P þ σ OR þ σ CTE þ σ EM ð2Þ
where σm is the strength of the unreinforced metal matrix (~50 MPa for
ð1Þ
the examined Al–Mg alloy). The grain size has a strong influence on
112 F. Khodabakhshi et al. / Materials Characterization 108 (2015) 102–114

where D is the grain size, k is the strengthening proportional constant

(~ 70 MPa.μm−0.5), M is the Taylor factor (~ 3 for face-centered cubic
polycrystals), τOR is the shear strength associated with reinforcing parti-
cles, β is a constant, G is the matrix shear modulus (~26.2 GPa), b is the
Burgers vector (~0.286 nm), ρCTE and ρEM are geometrical necessary dis-
locations density due to CTE and EM respectively, ν is Poisson's ration
(~0.345), dp is the diameter of Al3Ti nanoparticles (~100 nm), r0 is the
dislocation core radius (=4 b), A is a geometric constant, Δα is the dif-
ference in CTE, ΔT is the difference between test and processing temper-
atures, and ε is the strain in EM [78]. To estimate the contribution of
Orowan strengthening by Al3Ti nanoparticles, it is assumed that these
particles are spherical and uniformly distributed. The interparticle spac-
ing, λ, of Al3Ti nanoparticles with diameter of dp and volume fraction of
Vp can be calculated from the following equation [79].

" sffiffiffiffiffiffi! # rffiffiffi!

1 π 2
λ¼ −2 dp ð5Þ
2 Vp 3

Based on the microstructural details explained before, the contribu-

Fig. 13. EDS chemical analysis correspond to the fracture surfaces of (a) initial Al–Mg alloy,
(b) FSPed Al–Mg alloy, and (c) FSPed Al–Mg–Ti composite. These analyses's performed
from the indicated regions in FE-SEM fractographs of Fig. 12c, f, and i, respectively.
metal strength since the grain boundaries can hinder the dislocation
movement. This is due to the different orientation of adjacent grains
and to the high lattice disorder characteristic of these regions, which
prevent the dislocations from moving in a continuous slip plane [76].
The so-called Orowan mechanism consists in the interaction of nano-
particles with dislocations. The non-shearable ceramic reinforcement
particles pin the crossing dislocations and promote dislocations bowing
around the particles (Orowan loops) under external load [77]. The mis-
match in coefficient of thermal expansion (CTE) and in elastic modulus
(EM) between the reinforcements and the metal matrix is accommo-
dated during material cooling and straining by the formation of geomet-
rically necessary dislocations [77]. Therefore, the final strength of the
composite can be evaluated by summing the above contributions relat-
ed to the single strengthening effects as indicated below [76]:
pffiffiffi qffiffiffiffiffiffiffiffiffiffi pffiffiffiffiffiffiffiffiffi
k state chemical reactions between Al and Ti to form Al3Ti particles. The
σ c ¼ σ 0 þ pffiffiffiffi þ Mτ OR þ 3βGb ρCTE þ ρEM
D size of the hard inclusions was smaller than 100 nm with an approxi-
rffiffiffi ! (sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi sffiffiffiffiffiffiffiffiffiffiffiffiffiffi)
k 0:81GbM 2 dp pffiffiffi AΔαΔTV p 6V p
σ c ¼ σ 0 þ pffiffiffiffi þ ln þ 3βGb  þ
D 2πð1−νÞ1=2 λ 3 r0 bdp 1−V p πdp
tions of different strengthening mechanisms for FSPed Al–Mg alloy and
Al–Mg–Al3Ti nanocomposite were calculated and presented in Table 3.
Moreover, the total yield strengths of these processed materials were
predicted and compared by the estimated values from experimental
measurements. As shown, the high strength of in situ intermetallic
nanocomposite prepared by FSP can be mainly attributed to the grain
size strengthening which results from fine grain size of Al–Mg metal
matrix, and the Orowan strengthening which is due to high volume
fraction of nano-metric sized Al3Ti particles. As explained in the men-
tioned modeling procedure floc-shaped particles were ignored and as-
sumed that all of nano-particles homogeneously distributed, but as
revealed by microstructural studies the fraction of floc-shaped particles
in the fabricated nanocomposites is considerable. Therefore, some dif-
ferences between expected strength through modeling and experimen-
tally measured strength as presented in Table 3 can be reasonable.
5. Conclusions
An Al–Mg/Al3Ti (b100 nm, 4 vol%) nanocomposite was fabricated by
friction stir processing of an Al–Mg alloy (AA5052) with pre-placed Ti
particles. The formation mechanism of intermetallic particles during
FSP, microstructural evolutions and mechanical properties of the nano-
composites were studied and compared with the un-reinforced alumi-
num alloy. Microstructural studies determined that the average grain
size of the Al–Mg alloy decreased from ~49 µm down to 20 µm by
employing FSP. Pre-placing of titanium particles accelerated the grain
refinement, so that a fine-grained metal matrix was attained. The aver-
age grain size of the composite was about 1.5 µm but the size distribu-
tion was broad with a sign of bimodal distribution. The large plastic
strain and high temperature introduced by FSP also facilitated solid-
ð3Þ
mate volume fraction of 4%. Ultra-fine Mg2Si particles were also detect-
ed in the microstructure. Due to the presence of hard inclusions, the
3
ε mechanical strength of the nanocomposite was considerably increased
compared to the unreinforced alloy with the material still exhibited rea-
ð4Þ sonably high tensile elongation (~22%). Model analysis revealed the

Table 3
Predicted Young's modulus and contribution of different strengthening mechanisms to the yield strength of friction stir processed Al–Mg alloy and Al–Mg–Ti intermetallic composite sys-
tem: Ec,p, Predicted Young's modulus; Ec,m, Measured Young's modulus; σyc,p, Predicted tensile yield strength; σyc,m, Measured tensile yield strength.

Properties Elastic modulus Yield strength

Sample Ec,p(GPa) Ec,m(GPa) σ0(MPa) σH − P(MPa) σOR(MPa) σCTE(MPa) σEM(MPa) σyc,p(MPa) σyc,m(MPa)

FSPed Al–Mg alloy 70 71 50 15.5 – – – 65.5 65.3

FSPed Al–Mg–Ti composite 75 76 50 57.2 54.6 30.4 5.2 197.4 151.5
 F. Khodabakhshi et al. / Materials Characterization 108 (2015) 102–114
importance of grain refinement and distributing nano-metric hard in-
clusions on the mechanical properties of Al–Mg/Al3Ti (b100 nm,
4 vol%) nanocomposite. Fractographic studies also showed a combined
ductile–brittle fracture mode for the nanocomposite compared to the
fully ductile rupture of the annealed Al–Mg alloy as well as the FSPed
Al–Mg alloy without pre-placing titanium particles.
Acknowledgments
Financial support from the Iranian National Elite's Foundation is
greatly appreciated.
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