Materials Science and Engineering A 528 (2011) 5741–5746

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Materials Science and Engineering A

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

Microstructural, mechanical and wear behavior of A390/graphite and A390/Al2 O3

surface composites fabricated using FSP
M. Raaft, T.S. Mahmoud ∗ , H.M. Zakaria, T.A. Khalifa
Mechanical Engineering Department, Faculty of Engineering, Benha University, Egypt

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

Article history: In the present investigation, A390/graphite and A390/Al2 O3 surface composite (SC) layers were fabricated
Received 4 November 2010 using friction stir processing (FSP). The effect of tool rotational and traverse speeds on the microstructural,
Received in revised form 4 March 2011 mechanical and wear characteristics of the surface layers was studied. The results revealed that increasing
Accepted 25 March 2011
the tool rotational speed increases the hardness of the composite layers. The traverse speed has less
Available online 19 April 2011
significant influence on the hardness of the composite layer than the tool rotational speed. The A390/Al2 O3
surface composites exhibited higher hardness than the A390/graphite surface composites. The surface
Keywords:
composites exhibited better wear resistance than the matrix alloy. The A390/Al2 O3 surface composites
Friction stir processing
Surface composites
exhibited lower wear rates than the A390/graphite surface composites. Increasing the tool rotational
Aluminum alloys reduces the wear rate of both A390/Al2 O3 and A390/graphite surface composites.
© 2011 Elsevier B.V. All rights reserved.

1. Introduction an effective mean of refining the structure of both aluminum and

Metal matrix composites (MMCs) reinforced with ceramic
phases exhibit high strength, high elastic modulus, improved
wear resistance, creep and fatigue than the unreinforced alloys.
Such characteristics make them promising structural materials for
aerospace and automobile industries [1,2]. However, MMCs suffer
from a great loss in ductility and toughness due to incorporation of
the hard ceramic reinforcements [2–4]. This limits their wide appli-
cations to a certain extent. For many applications, the useful life of
components often depends on their surface properties such as wear
resistance. In these situations, it is desirable that only the surface
layer of components is reinforced by ceramic phases while the bulk
of components retain the original composition and structure with
higher toughness.
Surface composites are produced by impregnating the particu-
lates in the surface only while keeping the core free from it. Surface
composites can be produced using several techniques including,
high-energy electron beam irradiation [5], powder metallurgy [6]
and friction stir processing (FSP) [7]. Using FSP, surface composites
with adequate strength and low cost were successfully produced
[8,9]. The increase in strength is due to a reduction in defects asso-
ciated with the presence of the hard phase, while the low cost is
a result of using a lesser amount of the hard phase. FSP is a solid
state processing technique that has attracted a great attention in
the last few years [10–17]. It has been demonstrated that FSP is
∗ Corresponding author. Fax: +20 2 26843737.
E-mail address: Tsamir@benha-univ.edu.eg (T.S. Mahmoud).
magnesium based alloys. In FSP, a specially designed rotating cylin-
drical tool, consists mainly of a pin and a shoulder, is plunged into
a metal plate. The tool is then traversed in the desired direction.
During FSP, the metal is exposed to a combination of intense plastic
deformation, mixing and thermal exposure, resulting in a modified
microstructure characterized by a fine and equiaxed grain struc-
ture.
Several investigations were conducted to evaluate the effect of
both the tool rotational and traverse speeds on the microstruc-
tural and mechanical characteristics of surface composites [8,9].
For example, Morisada et al. [9] used constant tool rotating rate of
1500 rpm and several travel speeds varied from 25 to 100 mm/min
to fabricate multi-walled carbon nanotubes (MWCNTs)/AZ31 sur-
face composites. The results revealed that the dispersion of the
MWCNTs is related to the travel speeds of the rotating tool. A good
dispersion of the MWCNTs, which are separated from each other,
is obtained for the sample friction stir processed (FSPed) at 25 and
1500 rpm. In another work carried out by Morisada et al. [8], the
fullerene/A5083 composites were successfully fabricated by the
FSP. FSP was conducted at constant travel speed of 50 mm/min and
the tool rotating rate was changed from 500 to 2000 rpm. They
showed that the fullerene was dispersed so as to form the onion
ring in the stir zone for the sample FSPed at 1000–2000 rpm. The
shape of the stir zone was changed from triangular to trapezoidal
by the increase in the rotating speed.
In the current investigation, surface composites were fabricated
using FSP. Several A390/graphite and A390/Al2 O3 aluminum sur-
face composite were fabricated using several tool rotational and
traverse speeds. The aim of the present work is to study the effect

0921-5093/$ – see front matter © 2011 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2011.03.097
5742 M. Raaft et al. / Materials Science and Engineering A 528 (2011) 5741–5746

Table 1 lates were added into a small amount of methanol and mixed, and
Chemical composition of A390 alloy.
then applied to surface of the plates in the groove to form a thin
Alloy Chemical compositions (wt.%) reinforced powder particle layer. The A390 aluminum plates with
preplaced reinforced powder particles layer were subjected to FSP
Si Fe Cu Mg Mn Ni Zn Ti Al
after drying in air. The FSP were conducted using vertical milling
A390 16.47 0.36 4.29 0.62 0.132 0.149 0.019 0.01 Bal.
machine using three different tool rotation speeds, typically, 1200,
1400 and 1600 rpm. Also, two traverse speeds (feed rates) were
adopted typically, 20 and 40 mm/min. In all experiments, the tool
angle was fixed to 3◦ and the tool down force was held constant
by keeping constant depth of the tool immersed in the A390 plate.
Fig. 2 shows a schematic illustration of surface composites fabrica-
tion using FSP as used in this research.
Specimens from the FSP plates were cross-sectioned perpen-
dicular to the processing direction and then ground, polished. The
microstructural characteristics of the surface composites plates
were investigated using an Olympus optical metallurgical micro-
scope. The metallographic specimens were grounded and polished
using standard metallographic techniques before the examination.
The volume fraction of the particulates inside the composites sur-
face layers was measured using standard quantitative methods via
a metallurgical image analyzer. The microstructural characteris-
tics of the fabricated surface composites plates were investigated
Fig. 1. A schematic drawing of the FSPed specimens (dimensions in mm). using a scanning electron microscope (SEM) equipped with energy
dispersive X-ray spectroscopy (EDS) analysis system. The micro-
hardness was measured on the cross-section perpendicular to the
of these speeds on the microstructural, mechanical and tribological processing direction at the centers of the stirred zone (SZ). The
characteristics of the developed surface composites. microhardness of surface composite layer and A390 aluminum
alloy substrate were measured using a microhardness tester with
2. Experimental procedures a 60 g load.
Dry sliding wear tests were conducted to evaluate the wear
In the present investigation, the A390 hypereutectic Al–Si cast resistance of the surface composite layers and compare it with the
alloy was adopted. Table 1 shows the chemical compositions of the wear resistance of the as-cast A390 matrix alloy. The wear tests
A390 alloy. Two ceramic particulates (reinforcements), typically, were conducted using K93500 Micro-Tribometerpin-on-disc wear
graphite (G) and Al2 O3 and were dispersed into the surface of the testing machine according to ASTM G99–95 standard. The coun-
A390 plates. The reinforcements having size range between 15 and terface disc was made from an EN24 steel of hardness 57HRC. The
60 ␮m. The alloy was received in the form of ingots and machined chemical composition of the steel disc in wt% is 0.45 C, 0.35 Si,
into plates with grooves. Fig. 1 shows a schematic drawing of the 0.70 Mn, 1.40 Cr, 0.35 Mo, 1.80 Ni, 0.05 S and 0.05 P. The arrange-
A390 FSPed specimens. ment were made to hold a specimen and also for application of
Surface composites were fabricated using FSP in a single pass the load on the specimen. The specimens have block form with
using a steel tool. The tool is made from H13 tool steel. The FSP 5 mm × 5 mm × 6 mm (height). Fig. 3 shows a schematic illustra-
tool consists of a cylindrical pin with 8 mm diameter and 1 mm tion of the wear test. The dry sliding wear tests were conducted
height and a shoulder of 18 mm diameter. The surface of A390 under constant sliding speed, load and time of 165 rpm, 0.4 bar
alloy plates was cleaned before processing. The ceramic particu- and 10 min, respectively. The wear track was kept constant also at

Fig. 2. A schematic illustration of surface composites fabrication process.

 M. Raaft et al. / Materials Science and Engineering A 528 (2011) 5741–5746
Fig. 3. A schematic illustration of the wear test.
70 mm. A standard test procedure was employed. A fresh disc was
used each time and before each test, the disc was cleaned with ace-
tone to remove any possible traces of oil, grease and other surface
contaminants. The specimen which was cleaned with ethanol was
weighed before and after the tests using an electronic balance accu-
rate to 0.0001 g. The dry sliding weight loss was computed using the
weight loss of the pin before and after the experiments. The data for
the wear tests was taken from the average of three measurements.
3. Results and discussion
3.1. Microstructural examinations
The microstructure of the as-cast A390 Al matrix alloy is shown
in Fig. 4. The microstructure of the alloy consists mainly of three
phases, the ␣- (light), eutectic (flake like) and coarse primary silicon
(dark) phases (see Fig. 4b). It has been found that the primary Si par-
ticulates distributes heterogeneously in the aluminum matrix. The
primary Si particulates have a size range between 10 and 100 ␮m.
The as cast A390 was found to suffer from porosity and large cav-
ities. The size of the cavities was found to vary from 20 to about
200 ␮m.
Fig. 5 shows example micrographs of the microstructure of the
developed surface composites layers. The actual volume faction of
the Al2 O3 and graphite particulates dispersed on the surface com-
posites layers was found to be 7 ± 1 vol.%. It has been observed that
the Al2 O3 and graphite particulates were dispersed in the A390 sur-
face. Agglomeration of such particulates was observed in the FSPed
layer. Moreover, it has been found that the Al2 O3 and graphite
particulates were broken into finer particulates. Some of these par-
ticulates were dispersed uniformly inside the A390 matrix while
others were agglomerated. Fig. 6 shows micrographs of the Al2 O3
and graphite broken particulates. It is assumed that the particulates
were broken due to the intensive stirring action during FSP. It is
clear that the morphology (shape and size) of the primary Si partic-
ulates in the surface composites layers is very different from that of
the as-cast A390 matrix. In such layers, the primary Si particulates
showed much more homogeneous microstructure as compared to
the A390 as-cast alloy. Both the large primary Si particulates and
the dendrite structure disappeared over the whole layers. This is
because the material during the FSP experienced intense stirring
and mixing, which resulted in the breakup of the coarse Si particles
and the dendritic structure and gave a homogeneous distribution
of more fine Si particulates throughout the A390 Al alloy matrix.
Moreover, the large cavities found near the surface of the as-cast
A390 alloy were completely disappeared in the FSPed layers.
The A390/graphite surface composites showed higher agglom-
eration percent of the ceramic particulates than the A390/Al2 O3
surface composites. However, it has been found that the percent
5743
Fig. 4. (a) Optical micrograph showing the general structure of the A390 Al alloy,
(b) SEM micrograph shows the coarse eutectic structure of the as-cast A390 alloy.
agglomeration depends significantly on both the tool rotational and
traverse speeds. Increasing the tool rotational speed improves the
distribution of the ceramic particulates inside the A390 matrix. For
instance, for the A390/graphite surface composites, increasing the
tool rotational speed from 1200 to 1400 rpm at constant traverse
speed of 1200 mm/min, reduced significantly the agglomeration of
the graphite particulates (compare Fig. 5b and d). Also, reducing the
tool traverse speed reduces the agglomeration of the particulates.
3.2. Micro-hardness measurements
Fig. 7 shows the variation of the hardness of the surface com-
posites with the tool rotational speed at 20 and 40 mm/min
traverse speeds. The matrix A390 alloy exhibited hardness of
120 VHN. The surface composite layers exhibited higher hard-
ness when compared with the A390 matrix alloy. It has been
found that the hardness of the surface composite layer depends
on the FSP processing parameters, typically, the tool rotational and
welding speeds. Increasing the tool rotational speed increases sig-
nificantly the hardness of the surface composites. For example,
for A390/Al2 O3 surface composites FSPed at 20 mm/min traverse
speed increasing the tool rotational speed from 1200 to 1800
increased that hardness from 123 to 224 VHN. It is found that
the traverse speed has less significant influence on the hardness
of the surface composites than the tool rotational speed. At con-
stant tool rotational speed, increasing the tool traverse speed from
20 to 40 mm/min slightly increased the hardness of the surface
composites.
The A390/Al2 O3 surface composites exhibited higher hardness
when compared with the A390/graphite surface composites. For
5744 M. Raaft et al. / Materials Science and Engineering A 528 (2011) 5741–5746

Fig. 5. Optical micrographs of (a, b) A390/graphite and (c, d) A390/Al2 O3 and surface composites layers FSPed at (a, c) 1200 rpm and 20 mm/min and (b, d) 1800 rpm and
20 mm/min.

Fig. 6. Fractured Al2 O3 (a) and graphite (b) particulates during FSP of the surface composites. The composites were FSP at 1800 rpm and 20 mm/min.

(a) 300 (b) 300

250
Hardness (VHN)

Hardness (VHN)

200 200

150

100 100
20 mm/min 20 mm/min
50
40 mm/min 40 mm/min
0 0
1000 1200 1400 1600 1800 2000 1000 1200 1400 1600 1800 2000
Tool Rotational Speed (rpm) Tool Rotational Speed (rpm)

Fig. 7. Variation of the hardness of the surface composites with the tool rotational speed at 20 and 40 mm/min traverse speeds for (a) A390/Al2 O3 and (b) A390/graphite
surface composites.
 M. Raaft et al. / Materials Science and Engineering A 528 (2011) 5741–5746 5745

(a) 12 (b) 12
20 mm/min

Wear Rate (10-6 g/sec)

Wear Rate (10-6 g/sec)

10 10
40 mm/min

8 8

6 6

4 4 20 mm/min
40 mm/min
2 2
1000 1200 1400 1600 1800 2000 1000 1200 1400 1600 1800 2000
Tool Rotational Speed (rpm) Tool Rotational Speed (rpm)

Fig. 8. Variation of the wear rate of the surface composites with the tool rotational speed at 20 and 40 mm/min traverse speeds for (a) A390/Al2 O3 and (b) A390/graphite
surface composites.

example, the A390/graphite and A390/Al2 O3 /graphite surface com-
posites FSPed at 1200 rpm and 20 mm/min exhibited hardness of
121 and 112 VHN, respectively. The maximum hardness (224 VHN)
was observed for A390/Al2 O3 surface composites FSPed at tool
rotational and traverse speeds of 1800 rpm and 20 mm/min. This
represents an increase of about 86% of the hardness compared with
the hardness A390 matrix alloy.
The increase of the hardness of the FSPed monolithic alloys and
also surface composites layers produced and/or modified by FSP
was reported by many workers [8,9,18]. For example, in the work
carried out by Morisada et al. [18], the SiC particles were dispersed
into AZ31 in order to reveal the effect of the FSP with the SiC par-
ticles on the microstructure and hardness of the magnesium alloy.
The results revealed that the microhardness for the as-received
AZ31, the FSPed AZ31, and the FSPed AZ31 with SiC particles were
about 48.1, 60.0, and 69.3 VHN, respectively. It is considered that
these values were reflected by not only the grain refinement using
the SiC particles, but also the high hardness of the SiC particles.
3.3. Wear resistance
Fig. 8 shows the variation of the wear rate of the surface compos-
ites with the tool rotational speed at 20 and 40 mm/min traverse
speeds. It has been found that, for A390/Al2 O3 and A390/graphite
surface composites, increasing the tool rotational reduces the wear
rate of such surface composites. For example, A390/Al2 O3 surface
composites FSP at traverse speed of 20 mm/min, and tool rotational
speeds of 1200 and 1800 rpm exhibited wear rates of 7.3 × 10−6 and
4.5 × 10−6 g/s, respectively. While at 40 mm/min, the wear rates
were about 7.5 × 10−6 and 5.6 × 10−6 g/s, respectively. It is impor-
tant to mention that the as-cast (un-FSPed) A390 alloy exhibited a
wear rate of about 9.7 × 10−6 g/s which is higher than of the inves-
tigated composites. The A390/Al2 O3 surface composites exhibited
better wear resistance than the A390/graphite surface composites.
The main reasons for increasing the wear resistance of the sur-
face composites compared with the as-cast (un-FSPed) matrix alloy
are: (1) the presence of the hard ceramic particles at the surface

Fig. 9. SEM micrographs of the worn surfaces (a) and (b) A390/Al2 O3 surface composites FSPed at 1200 rpm (a) and 1800 rpm (b) and 20 and 20 mm/min, respectively; (c)
and (d) A390/graphite surface composites FSPed at 1200 rpm (c) and 1800 rpm (d) and 20 and 20 mm/min, respectively.
5746 M. Raaft et al. / Materials Science and Engineering A 528 (2011) 5741–5746
layer, (2) the presence of the fine primary Si particulates, and (3)
the reduction of surface defects such as porosity and cavity due to
FSP. During the wear test cavities reduce the contact area which
increases the actual pressure on the surface of the specimen and
hence increasing the wear rate. The reduction of the wear rate of
the surface composites with increasing the tool rotational speed is
attributed to the increase of the hardness of the surface composite
layer with increasing the tool rotational speed.
Fig. 9 shows SEM micrographs of the worn surfaces of the sur-
face composites after the dry sliding wear testing. Generally, the
surface composites exhibited classical features of the dry sliding
wear. It can be seen that the worn surfaces under dry sliding appear
to have slight plough and scratch marks. The SEM micrographs
show that abrasive wear is the main wear mechanism. Such mech-
anism essentially results of hard ceramic particles exposed on the
worn surface and the loose fragments between two surfaces, dom-
inates in surface composites layers. The relatively low wear rates
exist, indicating the regime of mild wear. However, the in the case
of surface composites FSPed at 1200 rpm the number of scratches
were increased, i.e. the surface composites FSPed at 1800 exhibited
smoother worn surface. For A390/graphite surface composites, it is
noticed that graphite lubricant films were formed on the worn sur-
face of the composite alloy (see Fig. 9c and d). It is suggested that the
formation of the graphite film at the surfaces of the composites can
avoid direct contact between the specimens and the counterpart,
thus reducing the shear stress transferred to the sliding surface, and
decreasing both the friction coefficient and wear rate.
The A390/graphite surface composites worn surfaces were cov-
ered in a thick layer (tribolayer) that was predominantly oxide. The
layer was extensively cracked and had delaminated in places. The
oxide layers at the contact surfaces were formed as a result of the
iron transferred from the counterface. During sliding metal–metal
wear tests of Al based composites, the iron oxide layer formed on
the contact surfaces acted as a solid lubricant and improved wear
resistant. The formation of the tribolayers increased the surface
hardness significantly and played an important role in delaying
the mild-to-severe wear transition in Al matrix composites. The
presence of graphite served as a safeguard by generating a hard
compacted tribolayer with smooth surface and sufficient thick-
ness to protect the material underneath from excessive subsurface
damage.
The dry wear characteristics of Al/graphite surface composites
may have been explained by two competing factors; first, the ben-
eficial effect of the graphite particulates addition in reducing the
wear and friction of the composites due to formation of a thin
lubricating graphite rich film on the tribosurface and secondly, the
adverse effects of the graphite addition in formation of porosity and
cracks as well as the deterioration of mechanical properties result-
ing in enhanced delamination. Apart from the graphite content, the
efficiency of solid lubrication by graphite in Al/graphite composites
depends on a number of factors such as wear testing conditions and
especially the applied pressure and also the morphology, shape,
size, and the distribution of graphite particles as well as the nature
of the particle matrix interfacial bonding together with the matrix
microstructure.
4. Conclusions
Based on the results obtained from the current investigations
the following conclusions can be made:
1. The microstructure of the A390/graphite and A390/Al2 O3 sur-
face composites depends significantly on both the tool rotational
and traverse speeds. Increasing the tool rotational and/or reduc-
ing the traverse speeds improves the distribution of the ceramic
particulates inside the A390 matrix. The A390/graphite surface
composites showed higher agglomeration percent of the ceramic
particulates than the A390/Al2 O3 surface composites.
2. The hardness of the surface composite layer depends on the FSP
processing parameters, typically, the tool rotational and welding
speeds. At constant traverse speed, increasing the tool rota-
tional speed increases hardness of the surface composites. The
traverse speed has less significant influence on the hardness
of the surface composites than the tool rotational speed. The
A390/Al2 O3 surface composites exhibited higher hardness than
the A390/graphite surface composites.
3. The surface composites exhibited higher wear resistance than
the as-cast A390 alloy. Increasing the tool rotational speed
reduces the wear rate of the surface composites. The A390/Al2 O3
surface composites exhibited better wear resistance than the
A390/graphite surface composites.
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