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DOI: 10.1007/s11665-015-1404-6 1059-9495/$19.00

Friction Stir Processing of Al-TiB2 In Situ Composite:

Effect on Particle Distribution, Microstructure
and Properties
Devinder Yadav and Ranjit Bauri

(Submitted October 15, 2014; in revised form January 8, 2015)

Aluminum-based in situ composites suffer from the age-old issue of particle segregation along the grain
boundaries after casting. In the present study, friction stir processing (FSP) was employed as a secondary
process to improve the distribution of in situ formed TiB2 particles in Al-based composite. All the
agglomerates of TiB2 were broken, and uniform distribution of particles was achieved after double-pass
FSP. Also, FSP removed the casting defects and caused significant grain refinement of the Al matrix. The
microstructure was characterized by equiaxed fine grains with average size of 3 lm and narrow grain size
distribution. The microstructural refinements and homogenization after FSP not only enhanced the
strength but also improved the ductility of the as-cast composite.

Although the particles generated in situ are very fine and

Keywords aluminum, electron microscopy, metallic matrix com-
posites, thermomechanical processing stable, the main issue in these composites is the agglomeration
of the particles (Ref 7). The particles segregate along the grain
boundaries or the interdendritic regions during solidification,
leaving the grains devoid of particles. Such non-uniform
particle distribution degrades the mechanical properties and
1. Introduction the beneficial effect of the in situ particles is partially lost.
Moreover, the common casting defects such as porosity,
shrinking cavities, and dendritic grain structure also occur.
Metal matrix composites (MMCs) are important class of
Several secondary processes such as extrusion, rolling, mushy
structural materials which combine high ductility and high
state rolling and equal channel angular extrusion (ECAE)
toughness of metal with high strength and high modulus of the
have been employed to improve the particle distribution (Ref
ceramic reinforcement to get excellent combination of mechan-
7-10). However, once the particle clusters form, it is difficult
ical properties (Ref 1). The ceramic particles are either added
to remove them by these processes. There are no reports of
externally or are synthesized within the metal matrix in situ.
any other method or process to improve the particle distri-
The advantages of generating the reinforcing particles in situ,
bution in Al-TiB2 in situ composites. Therefore, there is an
than adding them externally are many such as a clean particle-
immediate need to develop secondary processes which can
matrix interface, good interfacial bonding, and fine particle size
improve the distribution of the particles in Al-based in situ
(Ref 2-4).
composites.
Among the aluminum-based in situ composites, Al-TiB2
Recently, friction stir processing (FSP) has been developed
composites are the most extensively studied due to their
as a generic tool for microstructure modification (Ref 11). The
excellent strength, good wear resistance and good high-
process is fairly simple and works on the principle of friction
temperature properties (Ref 4). A number of processing routes
stir welding. In this process, a specially designed tool, having
have been developed to fabricate these composites and these
a shoulder and a pin, is rotated at high speed and a downward
include self-propagating high-temperature synthesis (SHS),
force is applied to plunge the pin into the base plate till the
exothermic dispersion (XD Martin Marietta Laboratory, Balti-
shoulder touches the plate. The tool is then traversed at a
more, MD, USA), reactive hot pressing (RHP), flux-assisted
particular feed rate. Due to the large frictional heat generated
synthesis, and mechanical alloying. All these processes are
at the tool plate interface, the material becomes plastic and
derived either from conventional powder metallurgy or casting
flows around the pin and is consolidated by the shoulder. The
route. A comprehensive review of various fabrication routes of
side on which the tangential velocity of the tool is parallel to
in situ composites is given by Tjong and Ma (Ref 4). One of the
the tool traverse direction is called the advancing side and the
most widely adopted methods of processing them is by casting
anti-parallel one is called the retreating side. FSP has been
(liquid metallurgy) route where, salts rich in Ti and B are added
used to refine the grain size of various Al and Mg alloys,
into the Al melt and stirred continuously at high temperature to
eliminate casting defects and microstructure homogenization
synthesis TiB2 particles in situ (Ref 5, 6).
(Ref 12, 13).
The material mixing action and thermomechanical nature of
Devinder Yadav and Ranjit Bauri, Department of Metallurgical and FSP are utilised in incorporating both ceramic and metallic
Materials Engineering, Indian Institute of Technology Madras, particles into Al matrix to process composites, nanocomposites,
Chennai 600 036, India. Contact e-mail: deven3042@gmail.com. and in situ composites (Ref 14-20). The utility of FSP to

Journal of Materials Engineering and Performance

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process surface composite was first shown by Mishra et al.
(Ref 14). Later on, the reinforcement particles were incorpo-
rated up to larger depths by carrying out FSP over grooves
filled with the reinforcement particles (Ref 15-17). The particles
were uniformly dispersed in the volume of the stir zone after
FSP. It was shown that by controlling the tool design and
groove depth, the particles can be incorporated to larger depths
in Al matrix (Ref 18). Hsu et al. (Ref 19) utilised the hot-
working nature of FSP to process Al-Al3Ti nanocomposites by
in situ reaction of elemental powders during FSP. The authors
showed that FSP provided severe deformation to promote
mixing at elevated temperature for in situ reaction and hot
consolidation to form a fully dense solid. Very recently, the
authors have shown the utility of FSP in improving the particle
distribution in Al-TiC in situ composites (Ref 20). All the
clusters of in situ formed TiC particles were broken down by
FSP and the microstructure homogenization thus achieved
along with the grain refinement led to improvements in both
strength and ductility.
The aim of the present investigation is to employ FSP as
secondary process to the as-cast Al-TiB2 in situ composite and
study its effect on particle distribution, microstructure, and
mechanical properties.
2. Experimental Details
The matrix material chosen in the present study was
commercially pure (99.5%) Al. The composite was synthesized
by the salt reaction method. Pure Al was melted in a graphite
crucible in a resistance-heated furnace. A salt mixture of
K2TiF6 and KBF4 (corresponding to 5 wt.% TiB2) was
wrapped in Al foil and made into small billets. The mixture
was pre-heated at 250 C for 1 h to remove the moisture
content. The pre-heated salt mixture was added to the Al melt
and it was held at 850 C for 1 h. The melt was continuously
stirred every 10 min. Finally, the slag was removed, the spent
salt was decanted, and the melt was poured into a pre-heated
cast iron mold in the form of a plate.
FSP was carried out on the as-cast composite plate using a
tool made of M2 steel having a shoulder diameter, pin diameter,
and pin length of 15, 5, and 4 mm, respectively. A rotational
speed of 1000 rpm and a traverse speed of 30 mm/min were
used. A second pass of FSP was also carried out over the first
pass (with complete overlap) with the same parameters.
X-ray diffraction was carried out in a Bruker D8 diffractom-
eter using Cu Ka radiation to evaluate the phases. Microstructure
of the composite was studied by scanning electron microscope
(SEM) and electron backscatter diffraction (EBSD). For SEM,
samples were metallographically polished and were observed in a
FEI Quanta FEG SEM, and energy-dispersive x-ray (EDX)
microanalysis was also performed. For EBSD studies, the
metallographically polished samples were electropolished in a
mixture of perchloric acid and methanol at 10 C and 10 V.
EBSD was carried out in a FEI Quanta FEG SEM equipped with
TSL-OIM software using a step size of 300 nm.
Tensile samples of gage length 5 mm and thickness 1 mm
were sliced entirely from the stir zone by electrical discharge
machining (EDM). Tensile tests were carried in an Admet
tensile tester at a strain rate of 10 3 s 1. Hardness was
measured with a Wolpert Wilson Vickers hardness tester using
a load of 100 g and a dwell time of 10 s.
3. Results and Discussion
3.1 As-Cast Composite
Figure 1 shows the XRD pattern of the as-cast composite.
Peaks corresponding to Al and TiB2 can be seen. The XRD
analysis did not show any sign of Al3Ti which is an undesirable
phase that forms at times in the salt reaction method when the
temperature is not controlled. Figure 2(a) is the SEM (BSE)
image of the as-cast composite. It can be seen from the contrast
difference that the in situ formed TiB2 particles are agglom-
erated along the grain boundaries. Particle-rich regions sur-
rounding the particle-free zones can also be seen. Figure 2(b)
shows one such agglomerate at high magnification where TiB2
particles with hexagonal and rectangular morphology can be
seen. Spot EDX on the particle clusters confirmed them to be
TiB2. The TiB2 particles were fine with size in the range of 0.5-
2 lm. The particle-matrix interface appeared clean as shown in
high-magnification SEM (BSE) image in Fig. 2(c). The SEM
investigation clearly shows that the as-cast microstructure is
heterogeneous in terms of particle distribution. Casting defects
such as porosity can also be seen in the as-cast composite
(Fig. 2a).
The particle distribution in MMCs depends on whether the
solidification front is pushing or engulfing the particles during
solidification, the former resulting in segregation in the
interdendritic regions and the latter in uniform distribution
(Ref 21). It has been also postulated that there is a critical
velocity of the solidification front below which the particles are
pushed and above which they are engulfed (Ref 22). Wang
et al. (Ref 23) suggested that the TiB2 particles are continuously
rejected by the solid-liquid interface and mechanically trapped
at the grain boundaries because of high interfacial energy
between TiB2 and aluminum. It has been also proposed that
aluminides formed on the basal plane of the particles can act as
glue between adjacent particles leading to clustering (Ref 15-
24). In the present case, similar clustering mechanisms seem to
have played a role in the segregation of particles along the grain
boundaries.
Fig. 1 XRD pattern of the as-cast Al-TiB2 in situ composite
Journal of Materials Engineering and Performance
Fig. 2 EM (BSE) images showing (a) as-cast composite (arrow shows a casting defect), (b) particle agglomerate, (c) particle-matrix interface at
high magnification

3.2 Effect of FSP on Particle Distribution and Microstructure was carried out to improve the particle distribution by Mervin
et al. (Ref 7). However, alligatoring type failure occurred under
FSP was carried out on the as-cast plate to improve the
certain conditions and one of the reasons attributed was the
particle distribution in the composite. Figure 3(a) and (b) shows
presence of TiB2 particles at the grain boundaries. Even
the SEM (BSE) image of the composite on the advancing side
secondary process such as extrusion does not break the clusters
and cross section of the stir zone. A clear demarcation is seen
and leads to alignment of TiB2 clusters along the extrusion
between the as-cast region and the friction stir-processed
direction (Ref 8, 25). ECAE of the Al-5% TiB2 in situ
(FSPed) zone. Particle agglomerates and casting defects can be
composite only led to decrease in the size of particle-free zone
seen in the as-cast base material, whereas a homogeneous
from 50-100 to 20-30 lm (Ref 9). Rolling of the in situ
microstructure can be seen in the FSPed region (stir zone).
composite also did not break all the agglomerates and small
Figure 3(c) shows that the distribution of TiB2 particles is
clusters were still observed (Ref 10). A single pass of FSP was
uniform on the surface of the stir zone. Some small agglom-
sufficient in the present case to break the agglomerates and
erates in the range of 5-6 lm and few casting defects were left
distribute the particles inside the grains (Fig. 3). This can be
behind in the stir zone after first FSP pass. Second pass led to
attributed to the intense material flow during FSP. The material
the breaking of the smaller agglomerates and a homogeneous
flow during FSP is not well understood but it is generally
particle distribution was achieved as shown in Fig. 3(d). The
accepted that it flows from the retreating to the advancing side
left over casting defects were also eliminated completely after
several times around the pin in a complex way. This intense
the second pass.
mixing of the plasticized material breaks the agglomerates and
It should be noted here that several strategies have been
distributes the TiB2 particles uniformly in the matrix. The
applied to improve the particle distribution in the in situ
volume of the material undergoing refinement depends on the
composites. Watson (Ref 25) found that the cluster size
tool dimensions and geometry. The shoulder width decides the
decreased from 50 to 10 lm when the composite melt was
width of the stir zone, and the pin length decides the depth. FSP
held at 700 C for 73 h prior to casting. Mushy state rolling

Journal of Materials Engineering and Performance

Fig. 3 SEM (BSE) images of the interface between cast and FSPed region on (a) surface, (b) cross section, (c) FSPed region (stir zone) show-
ing uniform distribution of particles and (d) particle distribution after double pass

does not change the shape of the component and can be carried
out locally on a cast component. At the same time, large areas
can also be covered by multiple parallel passes of FSP.
FSP is a thermomechanical process during which the
material deforms at elevated temperature with the strain rate in
the range of 10-100 s 1 (Ref 26). Therefore, occurrence of
dynamic recrystallization is expected during the process.
EBSD was carried out on the composite to further study the
microstructure developed in FSP. Figure 4 shows the EBSD
(IPF + grain boundary) map of the as-cast composite. The
TiB2 particles were too fine and could not be indexed. Some
of the TiB2 particles came out during electropolishing thereby
leaving pits behind. The poorly indexed points (with confi-
dence index < 0.1), shown in black color, were excluded from
the image, and no image cleaning was carried out. The
average grain size of the as-cast composite was found to be
around 50 lm. It is well known that TiB2 particles act as
good grain refiners by acting as heterogeneous nucleation sites
and also by restricting the grain growth during solidification
(Ref 22, 27).
The EBSD (IPF + grain boundary) maps of the single-pass
and double-pass FSPed composite are shown in Fig. 5(a) and
(b), respectively. Fine and equiaxed grains can be observed Fig. 4 EBSD (IPF + grain boundary) map of the as-cast composite

Journal of Materials Engineering and Performance

Fig. 5 EBSD (IPF + grain boundary) map of (a) single pass, (b) double-pass FSPed composite, (c) grain size distribution and (d) grain bound-
ary map (arrows show the mixed character boundaries)
Fig. 6 Tensile stress-strain curves of as-cast and FSPed Al-TiB2
in situ composites
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both after first and second pass with a narrow grain size
distribution. The average grain size was found to be 3 lm after
first pass with more than 60% of the boundaries being high
angle (>15 misorientation). Hence, FSP not only dispersed
the TiB2 particles uniformly but also caused grain refinement of
the matrix. The amount of grain refinement is significant as it is
achieved in one step. Most of the grain-refining processes
involve several steps or several passes to achieve good amount
of grain refinement (Ref 28). The homogeneity of the
microstructure can be attributed to the temperature of defor-
mation during FSP. It is generally found that the deformation
becomes more homogeneous as the temperature of deformation
increases (Ref 29). The grain size distribution after first and
second pass is shown in Fig. 5(c). From the EBSD study, it can
be seen that the second pass does not refine the grain size
further. This indicates that the final grain size of the composite
depends on the process parameters and not on the initial grain
size. Similar results were obtained in the case of double-pass
FSP of pure aluminum (Ref 30).
Table 1 Mechanical properties of Al-5TiB2 in situ composite
Material Hardness, Hv
Pure Al 28
Al-5TiB2 as-cast 38 ± 7
FSP single pass 51 ± 2
FSP double pass 52 ± 2
Al-5vol.% TiB2 (Ref 32) … 96
Al-11.6% Al2O3 (Ref 33) … 86
Al-22% SiC (Ref 34) … …
The fine grains during FSP are formed by dynamic
recrystallization process (Ref 12). Dislocations are generated
due to the plastic flow during FSP. Large numbers of
geometrically necessary dislocations are also generated at the
particle matrix interface due to the large difference in the
coefficient of thermal expansion between Al (24 9 10 6/C)
and TiB2 (8.1 9 10 6/C). Hence, the particle-matrix interfaces
are additional source of dislocations. The dislocations get
arranged into subgrain boundaries due to high rate of dynamic
recovery which arises due to high-stacking fault energy
(166 mJ/m2) of Al. It was shown that these subgrain boundaries
turn into low-angle and then high-angle grain boundaries by a
continuous type recrystallization (CDRX) process thereby
giving rise to a fine and equiaxed grain microstructure (Ref
31). In the grain boundary map in Fig. 5(d), several boundaries
were seen with mixed character (mixed color), with a part of the
boundary having low angle (5-15 misorientation, green) and
part with high angle (>15 misorientation, blue) character.
This mixed nature of grain boundaries is an indication of
occurrence of CDRX. At this point, it can be argued that the
uniform distribution of TiB2 particles will accelerate the
recrystallization kinetics compared to unreinforced Al by
generating more dislocations at the particle-matrix interfaces.
3.3 Mechanical Properties
Figure 6 shows the tensile stress-strain curves of the as-cast,
single-pass (FSP-SP) and double-pass (FSP-DP) FSPed com-
posites. The results are summarized in Table 1. The composite
exhibited a yield strength (0.2% off set) of 124 MPa after a
single pass of FSP compared to 83 MPa of the as-cast
composite, which is an improvement by a factor of 1.5. Ulti-
mate tensile strength (UTS) also increased substantially from
103 MPa in as-cast to 154 MPa in FSPed condition (single
pass). It should be noted that pure Al is a low-strength metal
(YS of 35 MPa and UTS of 70 MPa). Therefore, the increase in
the strength by FSP is quite significant. More importantly, the
ductility improved from 11% in the as-cast condition to 19%
after FSP. This is also a significant achievement given the fact
that most MMCs suffer from low ductility (Ref 35-37). The
study can be extended to Al alloys and the improvement in the
mechanical properties can be compared with the unreinforced
alloys.
The mechanical properties of a composite depend on the
homogeneity of particle distribution. Segregation or agglomer-
ation of particles at the grain boundaries or any other region
reduces the ductility. Segregation of particles can also have a
negative effect on the strength of the composite (Ref 37). In the
present study, FSP improved the homogeneity of particle
distribution. The beneficial effect of homogeneous particle
distribution was also evident in the further improvement in
0.2% proof stress, MPa UTS, MPa % elongation
35 70 40
80 103 11
124 154 20
153 172 19
124 9.2
165 8
110 8
strength properties after the second FSP pass (Table 1). There
was no significant grain refinement after the second pass.
However, the smaller particle agglomerates left behind after
the first pass were broken completely and distributed during
the second pass thereby creating more number of particle-
matrix interfaces for effective load transfer. Moreover, the left
over smaller casting defects were eliminated after the second
pass. The strength enhancement thus can be attributed to
OrowanÕs dispersion strengthening mechanism due to uniform
distribution of the TiB2 particles (Ref 38). The grain
refinement also contributed to the strength enhancement
according to Hall-Petch relationship (Ref 39). The homoge-
neous particle distribution and development of a well-defined
grain structure during FSP improved the ductility significantly.
Elimination of the casting defects also helped improving the
ductility.
The hardness also improved after FSP. The FSPed compos-
ite exhibited an average hardness of 51 Hv after the first pass
and 52 Hv after the second pass compared to 38 Hv of the as-
cast composite. The hardness exhibited a similar trend as the
grain size with respect to the number of passes.
The fracture surface of the as-cast composite is shown in
Fig. 7(a). The as-cast composite exhibited failure along the
dendritic boundaries as they became brittle due to the
segregation of TiB2 particles along them. The high-magnifica-
tion image in Fig. 7(b) shows the agglomerated TiB2 particles
inside the dimples. The FSPed composite (single pass) showed
well defined and deep dimples indicating ductile failure as
shown in Fig. 7(c). Individual TiB2 particles sitting in the
dimples can be seen in Fig. 7(d) indicating uniform distribution
and good bonding with the matrix that helps in effective load
transfer. Several small dimples, whose size matched with the
grain size of the FSPed composite, were also observed beside
many of the big dimples as shown in Fig. 7(c). It indicates that
either the smaller dimples coalesce to form the bigger ones or a
plausible secondary failure mechanism might be occurring at
the final stages of the tensile test after the bigger dimples are
formed. The microstructural features on the fracture surface of
the double-pass FSPed composite were similar to single-pass
FSPed composite.
3.4 Morphology of TiB2 Particles
It should be noted that particle morphology does play a role
in the mechanical properties of MMCs (Ref 40). Hence,
capturing the actual 3D morphology of the in situ TiB2 particles
is important. However, the reported morphology of TiB2 par-
ticles in the literature is based on SEM images which present
only a 2D view of the particles since the particles get cut along
certain faces during the metallographic polishing. Hence, the
actual morphology of the particles is missed and not much
Journal of Materials Engineering and Performance
Fig. 7 SEM images of fracture surfaces. (a) as-cast composite, (b) particle agglomerate in dimples in the as-cast composite, (c) FSPed compos-
ite and (d) individual particles sitting in the dimples

Fig. 8 SEM image of fracture surface showing (a) morphology of the TiB2 particle and (b) top view of the particle

information is available on this aspect of the in situ TiB2 par- attached to the dimples and provide views of multiple faces
ticles. Therefore, an attempt was made in this study to capture unlike in the polished surfaces where they are embedded in the
the actual morphology of the particles. Analyzing the fracture matrix. The TiB2 particles were observed carefully at high
surface could be ideal for such a study as the particles are partly magnification in the fracture surface. As seen from Fig. 8(a)

Journal of Materials Engineering and Performance

and (b), the visible faces are actually the pyramidal faces of a
hexagon truncated on either side. From the SEM images in
Fig. 2(b) and (c), what we see is the cross-sectional view of the
particles cut along certain planes during metallographic pol-
ishing or the 2D view of the particles. Depending on the plane
of observations, the particles might appear as rectangular,
cubic, or quadrilateral. In the present case, the rectangular
particles seen in the SEM images are essentially the pyramidal
planes of the hexagonal particles. Hence, the actual particle
morphology appears to be hexagonal pyramidal and not the
other shapes presented by the SEM images of polished
surfaces.
4. Conclusions
Al-based in situ composites suffer from the agglomeration
of the reinforcing particles at the grain boundaries. The particle
agglomeration degrades the mechanical properties of the
composite. In this study, FSP was successfully employed as a
secondary process to improve the particle distribution in
Al-5TiB2 in situ composite. The following conclusions can
be drawn from the present study.
1. FSP of the as-cast composite broke down the particle
agglomerates and distributed the TiB2 particles uniformly
in the Al matrix.
2. FSP also eliminated the casting defects and caused signif-
icant grain refinement in the Al matrix. The microstruc-
ture after FSP is characterized by narrow grain size
distribution with more than 60% of the boundaries being
high angle.
3. The microstructure homogenization led to significant
improvement in the mechanical properties. The most
important aspect was that not only the strength was en-
hanced by 1.5 times but the ductility of the composite
also improved from 11 to 19% after FSP.
Acknowledgments
The authors would like to thank the faculty at Materials Joining
Laboratory, Dept. of Metallurgical and Materials Engineering, IIT
Madras, for providing access to NRB supported FSP facility.
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