Research article

Received: 14 March 2014

Revised: 28 September 2014

Accepted: 29 September 2014

Published online in Wiley Online Library

(wileyonlinelibrary.com) DOI 10.1002/sia.5694

Fabrication of Al/AlN nano-composite layers by

friction stir processing of 6061 Al-T6 substrate
Seyed Farshid Kashani-Bozorg,a* Maryam Samieeb
and Abbas Honarbakhsh-Raoufb
Friction stir processing was employed for the production of Al/AlN nano-composite layers on a 6061 Al-T6 substrate. Nano-sized
AlN powder was inserted in a groove in the middle length of the substrate. Defect-free layers were achieved using tool rotation
and substrate advancing speeds in the range of 9001400 rpm and 63310 mm/s, respectively. Subsequent passes were conducted to break-up AlN clusters that formed in a non-uniform fashion after initial pass. The grain size of aluminum matrix was
found to decrease by the introduction of AlN powder. A nano-composite layer with near uniform dispersion of nano-sized AlN reinforcements with a ~9.6% volume fraction was achieved in a matrix of fine dynamically restorated Al grains with a mean size of
~2.5 m after three subsequent passes. This layer showed an average micro hardness value of ~164 HV (much greater than
~103 HV of the underlying substrate). In addition, the nano-composite layer exhibited superior dry sliding wear performance
against hardened steel compared to that of 6061-T6 substrate. Increasing tool rotation and substrate advancing speeds were
found to decrease the AlN content of the processed layer possibly due to increasing in powder scattering by the pin tool. This
was associated with a decrease and increase in hardness values and wear-loss data, respectively. Copyright 2014 John Wiley
& Sons, Ltd.
Keywords: nano-composite; friction stir processing; Al; AlN; surface properties

Introduction
AlN is an attractive reinforcement for aluminum due to its excellent
properties such as low density, high thermal conductivity, and low
coefficient of thermal expansion.[1] It offers appropriate adhesive
interfaces similar to SiC and a relatively higher wettability to
aluminum matrix than Al2O3.[1] Al/AlN composite was previously
fabricated using squeeze casting[2] and solid state powder
techniques.[3] Dispersion of AlN was found to be a problem in casting. On the other hand, solid state powder method is involved with
several steps that take lengthy times. Surface techniques were also
employed for the fabrication of Al/AlN composite layers. Ion implantation was used[4]; achieving a hard surface took a treatment
of more than 2 h. In another approach, magnetron sputtering was
employed[5]; the deposition rate was found to be limited to
50 nm/min. Matsumoto et al.[6] used high velocity oxy fuel technique to spray AlAlN powder mixture on a 6061 Al alloy; powder
agglomeration and porosities due to weak bonding of Al2O3AlN
were observed.
Friction stir processing (FSP) is a solid state technique for producing composite surface layers.[7] By introduction of ceramic particles
to the stir zone, the plasticized surface material is mixed with
ceramic particles. Aluminum composite surface layers have been
fabricated with uniform dispersion of reinforcements such as
SiC,[7] Al2O3,[8] B4C,[9] and Si3N4[10] using FSP.
Mechanical properties of composite materials can be enhanced by
decreasing the size of reinforcements. However, it is difficult to distribute nano-sized particles in a metallic matrix to fabricate nanocomposite, as nano-sized particles suffer from agglomeration.[11]
In the present investigation, FSP is employed for the fabrication
of novel Al/AlN nano-composite surface layer on a 6061-T6 Al substrate. In order to achieve sound layers with uniform dispersion of

Surf. Interface Anal. (2014)

nano-sized AlN reinforcements, process parameters such as tool rotation and substrate advancing speeds and number of passes were
altered. In addition, subsequent passes were carried out. The microstructures of the surface layers were characterized, and their hardness and wear properties were evaluated.

Experimental
As-received materials
A 10-mm-thick rolled plate of 6061-T6 aluminum alloy was used as
substrate material; the nominal chemical composition was listed in
Table 1. Rectangular work pieces with a width and length of 50 and
100 mm, respectively, were prepared from the plate. Nano-sized
AlN (purity of >95%) powder (supplied by Plasma Chem) with a
particle size of 5200 nm and a mean diameter of ~45 nm was used
as matrix reinforcement. To introduce nano-sized AlN powder, a
groove was made on the surface of each work piece; the depth
and width of the groove were 3 and 1 mm, respectively. Before
FSP experiment, the groove was filled with nano-sized AlN powder.

* Correspondence to: S. Farshid Kashani-Bozorg, Center of Excellence for Surface

Engineering and Corrosion Protection of Industries, School of Metallurgy and
Materials, Engineering, College of Engineering, University of Tehran, P.O.
Box 11155-4563, Tehran, Iran.
E-mail: fkashani@ut.ac.ir
a School of Metallurgy and Materials Engineering, College of Engineering, University
of Tehran, P.O. Box 11155-4563, Tehran, Iran
b Department of Materials, Faculty of Engineering, University of Semnan, Semnan,
Iran

Copyright 2014 John Wiley & Sons, Ltd.

S. F. Kashani-Bozorg, M. Samiee and A. Honarbakhsh-Raoof

Table 1. Nominal chemical composition (wt. %) of 6061-T6 Al substrate

Hardness and wear evaluations

Mg

Si

Fe

Cu

Cr

Mn

Zn

Ti

Al

1.05

0.63

0.41

0.32

0.05

0.07

0.12

0.01

Balance

The micro hardness profiles were obtained on the cross sections of

the fabricated layers along the width (on a line parallel to its surface
in a depth of ~0.5 mm) and depth using a Vickers indenter under a
200 gf load for 10 s.
Wear tests of the as-received 6061-T6 Al and FSPed substrate
(without introduction of AlN powder) and fabricated Al/AlN nanocomposite surface layers were performed on their 5-mm-diameter
cylindrical pin specimens using a pin-on-disc device under a load
of 16.5 N for a sliding distance of 2000 m. The as-prepared and
worn-out pins were cleaned in acetone and weighed to an accuracy

A non-consumable rotating tool was fabricated from high carbon

steel (hardened H-13 tool steel); the diameters of shoulder and pin
were 16 and 5 mm, respectively. The pin length was 4 mm as well.

Friction stir processing setup

FSP experiments were conducted using a vertical milling machine.
A 3 forward tilt angle was applied on the tool. Work pieces were
subjected to various tool rotation and substrate advancing speeds
in the ranges of 8001800 rpm and 50350 mm/min, respectively.
Before FSP, each work piece was fixed and held tightly by a fixture.
In order to achieve uniform processed layers, additional passes
were applied; the direction of each subsequent pass was changed,
i.e. advancing and retreating sides were reversed after each subsequent pass. A schematic view of FSP experiment is shown in Fig. 1.
Another set of FSP experiments was conducted without
introduction of AlN powder. Specimens were taken from the fabricated layers and named as Fx, y, where x and y represent values of
rotation (rpm) and advancing (mm/min) speeds, respectively. For
instance, F900, 63 represents the layer produced after four FSP passes
using tool rotation and advancing speeds of 900 rpm and
63 mm/min, respectively.

Figure 2. A typical top view of sound friction stir processed layer; F900, 63.

Table 2. The status of the fabricated layers as a function of tool rotation

and substrate advancing speeds
Rotational speed, rpm

800

900

1000

1120

1400

1800

T
T
T
L
L

N
N

N
N
N
N
N

Microstructural characterization
Several specimens were prepared from the cross section of the fabricated layers. Specimens were then polished on their top surfaces
and cross sections using different grades of abrasive papers. Final
polishing was done using a 1-m-size diamond paste. In order to
get optical micrographs, specimens were etched by 0.5%HF reagent. The microstructure of the fabricated layers was examined
on top surfaces and cross sections by optical and scanning electron
microscopy. The latter was linked to an energy dispersive spectrometry device for the determination of chemical composition. Mean
matrix grain size was measured by linear intercept method. Volume
fraction of AlN particulates was determined using image processing. X-ray diffraction was used for the determination of crystal
structures.

Figure 1. A schematic view of FSP experiment.

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Advancing speed, mm/min.

35
63
125
310
350

L, = lack of fill; T, = tunneling defective layer; , = sound layer; N, = nonuniform surface layer with flash.

Figure 3. Top view of a layer with lack of fill defect; F800, 310.

Copyright 2014 John Wiley & Sons, Ltd.

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Al/AlN nano-composite layers

of 0.1 mg before and after the test. The counterpart discs
were made of AISI 52100 steel with a hardness value of ~60 HRC.
All wear specimens and their counterpart discs were polished with
a 1200- SiC grit prior to wear testing. Finally, scanning electron
microscopy was employed for the study of worn-out specimens.

Results and discussion

Fabrication of sound surface layers
Figure 2 exhibits a typical top view of the fabricated sound surface
layer (F900, 63). FSP experiments showed that the production of
sound surface layers was possible using ranges of tool rotation
and substrate advancing speeds according to Table 2. All fabricated

Figure 4. Cross section of a fabricated layer exhibiting cavity defect at a

depth of the advancing side (F800, 125).

layers were initially inspected by eye examination. Sound status

was confirmed after revealing a defect-free microstructure at track
cross section; this was carried out using optical and scanning electron microscopy. A surface layer with incomplete filling defects was
resulted using a relatively low tool rotation and high advancing
speeds of 800 rpm and 350 mm/min., respectively (Fig. 3). By increasing tool rotation and decreasing advancing speeds, surface
layers were formed with sound top views. However, cross sections
of few layers showed either tunneling or cavity defects (e.g. Fig. 4).
Cavity defects were mainly found at the advancing side close to the
pin; this is believed to be due to incomplete flow at a column close
to advancing side. Here, two main modes of material flow regimes
are involved namely pin driven flow and shoulder driven flow;
these merge together to form a defect-free processed layer[12]; material flows towards the advancing side near the shoulder as the
tool shoulder and base material interaction increases (i.e. shoulder
driven flow), when the shoulder-driven material does not reach
the advancing side, a groove like (tunnel) defect is produced. By increasing tool rotation speed, shoulder driven flow enhances; thus,
the top of the surface layer is filled by the plasticized material. However, material flow below certain depth is not affected by increasing
shoulder/surface material interaction. Thus, a cavity can be formed
close to the pin at the advancing side due to incomplete material
flow (Fig. 4).

a
Advancing side

Retreating side

Figure 6. The microstructures of the as-received 6061-T6 Al substrate

exhibiting elongated grains, typical of a rolled plate.

Figure 5. Cross section of a sound layer (F900, 63); an overview (a) and flow
pattern features (b and c).

Surf. Interface Anal. (2014)

Figure 7. The microstructure of the FSPed layer (with no AlN powder) after
four FSP passes (F900, 63).

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S. F. Kashani-Bozorg, M. Samiee and A. Honarbakhsh-Raoof

In order to achieve defect-free layers, relatively higher tool rotation and lower substrate advancing speeds were employed. This
strategy increases heat input and in turn enhances material flow.
Sound processed layers (e.g. Fig. 5a) exhibited vortices-like pattern
in stir zone (Figs 5b and 5c). It was indicated that when the shoulder
interaction increases both pin and shoulder-driven material merge
with each other and the differentially etched bands join
together.[12] Thus, a vortices-like pattern (onion ring pattern) forms
when the shoulder-driven and pin-driven material flows merge together (Fig. 5c). Further increasing the heat input, either by decreasing advancing speed or increasing tool rotation, resulted in the
formation of non-uniform surface layers with swelling and flashes.

Figure 8. The as-received AlN powder with a mean particle size of ~45 nm.

Substrate and fabricated layer microstructures

The microstructure of the as-received 6061-T6 Al substrate consists
of elongated grains, typical of a hot rolled structure (Fig. 6); mean
grain length was found to be ~105 m.
In the case of FSPed layer (without introduction of AlN powder), the
stir zone exhibited relatively fine grains (e.g. F900, 63 specimen in Fig. 7).
Stir zone material is under severe-plastic deformation at temperature
close to melting point during FSP. Thus, the plasticized material is hot
deformed; the production of fine equiaxed grains (Fig. 6) is indicative
of the occurrence of a dynamic restoration process. In this case, the
mean grain size of the stir zone was found to be ~11 m, which is remarkably smaller than that of its underlying Al substrate (~105 m).
By introduction of nano-sized AlN powder (Fig. 8) into the stir
zone, clusters of AlN powder were found in the stir zone microstructure in a non-uniform fashion as bands (Fig. 9a). Relatively high
cohesion energy is associated with fine nano-sized particles
that increase their tendency to clump together forming clusters
(e.g., Fig. 9b).[11] Surface material moves from advancing side to
the retreating side where it is extruded in a helical path into a plasticized zone surrounding the pin tool.[13] Different motions of material were reported; these include circumventing motion of surface
material around the tool shoulder, torsional motion due to rotational motion of surface material within the interaction layer under
the tool shoulder, and vortex motion associated with the flow of
thickness material due to the action of the tool pin.[14] AlN clusters
were found within the bands. We believe that their locations after
the first pass depend on the main processing parameters (tool rotation and substrate advancing speeds). Initially, powder is taken

Figure 9. The microstructure of Al/AlN composite layer (F900, 63) produced by a single pass exhibiting non-uniform dispersion of AlN powder (a), formation of
AlN clusters (b), and energy dispersive spectrum of b (c).

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Al/AlN nano-composite layers

from the advancing side to retreating side. If the plastic flow is
weak, then the clusters are mainly found in the retreating side. A
strong flow can take the powder further to the advancing side; this
can be done by increasing tool rotation. Another issue is the advancing speed that introduces a vertical flow. Thus, a suitable ratio
of tool rotation to advancing speed provides quite uniform dispersion. Break-up of clusters is gradually done by further passes.
EDS analysis of the stir zone was indicative of the presence of
nitrogen (Fig. 9c); this is related to AlN reinforcements. In addition,
substantial Fe and Cr were detected; these were found to be
greater than those of the substrate. Thus, it can be deduced that
extra Fe and Cr values resulted due to tool wear during FSP.
Additional FSP passes activate stirring of material.[8,15] Thus, all
processed layers were subjected to three additional passes.
Sequential breaking-up of these clusters to smaller ones occurred
after subsequent FSP passes. Plasticized material is squeezed
around the pin. The squeezed material is affected by circular flow
imposed by the shape of the tool. Tool rotation led to circular
movement of material in the same direction, which resulted in
intensive mixing of constituents as shown in Fig. 10.
Table 3 summarized the chemical composition of three areas
from the top, middle, and bottom of a fabricated layer (F900, 63) after
three extra passes; aluminum, magnesium, silicon, nitrogen, oxygen, and iron elements were detected. Aluminum, magnesium,
and silicon are the main components of the as-received substrate.
The relatively high concentration of nitrogen goes to AlN particulates since no crystal structure other than Al and AlN were detected
by X-ray diffraction. Negligible variation of nitrogen concentrations

Table 3. Chemical composition (at. %) of the fabricated Al/AlN nano-composite surface layer (F900, 63)
at three different regions; top, middle, and bottom
of the stir zone after three additional passes
Element
Al

Mg

Si

Fe

At. %
Top
Middle
Bottom
Top
Middle
Bottom
Top
Middle
Bottom
Top
Middle
Bottom
Top
Middle
Bottom
Top
Middle
Bottom

66.4
64.5
63.2
23.4
23.9
25.5
0.5
0.4
0.4
0.2
0.1
0.2
9.4
10.9
9.6
0.3
0.2
0.3

in the three areas indicates near uniform dispersion of AlN reinforcements in the fabricated layer.

Figure 10. Dispersion of AlN powder in the fabricated layers after three additional passes using various tool rotation and substrate advancing speeds; F900, 63
(a),F900, 125 (b), and F1120, 125 (c).

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S. F. Kashani-Bozorg, M. Samiee and A. Honarbakhsh-Raoof

Main process parameters such as tool rotation and substrate advancing speeds, tool dimensions, and design have their own contributions to AlN content of the fabricated composite layer. Thus, their
variations affect dispersion of AlN powder in the stir zone. A relatively low substrate advancing speed resulted in more AlN content
of the fabricated nano-composite layer (e.g. Fig. 10a vs. Fig. 10b)
possibly due to less powder scattering during FSP. Powder is placed
in front of the pin. As the tool advancing speed increases, more
powder is pushed out of the groove by the advancing and rotating
pin. A decrease in AlN content was detected as the advancing
speed increased from 63 to 125 mm/min; AlN volume fraction
was calculated to be ~9.6 and 6.5% for F900, 63 and F900, 125 nanocomposite layers, respectively. What should be taken into account
is the ratio of tool rotation speed/advancing speed; this, in the case
of F900,63 is going to be nearly twice that of F900,125. Similar effect
with a relatively lower impact was observed considering variation
in tool rotation speed; an increase in tool rotation speed from 900
(F900, 125 in Fig. 10b) to 1120 rpm (F1120, 125 in Fig. 10c) using a fix advancing speed of 125 mm/min. slightly decreases AlN content; AlN
volume fraction was found to decrease from ~6.5 to ~5.7%. This indicates that powder scattering due to an increase in tool rotation is
lower than that of same increase in advancing speed. In the latter
case, powder scattering is somewhat limited by the groove wall;
this does not happen upon advancing.
There is another issue related to Fig. 10. The particles of Fig. 10a
correspond well to the mean mesh size (the mean particle size of
the as-received AlN powder was ~45 nm). On the other hand, the
particles of Fig. 10b and c are bigger. Bearing in mind that the asreceived AlN powder had a range of particle size (5200 nm), it is
believed that the smaller particles (i.e., lighter particles) scattered
more by increasing advancing speed (Fig. 10b) and also scattered
more by increasing tool rotation and advancing speeds (Fig. 10c).
By introduction of nano-sized AlN powder into the stir zone, a relatively finer microstructure was resulted compared to that of the
FSPed one (without introduction of nano-sized powder) using similar process parameters (e.g. Fig. 11; F900, 63, F900, 125, and F1120,125
nano-composite layers exhibited a dynamically restorated grains
with mean sizes of ~2.5, 4, and 5 m, respectively). Grain/sub-grain
boundaries were found to be pinned by nano-sized ceramic powders. The effect of second-phase particles on grain boundaries
was initially studied by Zener.[16] Dispersion of second-phase particles exerts a retarding force or pressure, named Zener drag, on the
low and high-angle grain boundaries; this significantly affects the
recovery, recrystallization, and grain growth of deformed structures.
Zener proposed a quantitative theoretical expression for the grain
size as a function of the average volume fraction of the uniformly
dispersed particles (Eqn (1)):
dz 4r=3Vf

(1)

In this expression, r and Vf are the radius and volume fraction of

second phase particles, respectively.[16] Using Zener expression, the
critical grain size due to grain boundary pinning by dispersed
second-phase particles or Zener limiting grain size can be predicted. However, the calculated critical Al matrix grain of the fabricated Al/AlN nano-composite layer with AlN volume fraction of
9.6 was found to be less than one micron using Zener approach;
this is not in agreement with the experimental one (~2.5 m in
Fig. 11a). It should be considered that FSP is associated with sever
plastic deformation. Dynamic grain growth under high temperature
and strain rate provide rapid boundary mobility. Plastic deformation changes the geometry of grain structures, and this perturbs

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Figure 11. Fine dynamically restorated grains of Al/AlN nano-composite

layers; F900, 63 (a), F900, 125 (b), and F1120, 125 (c).

the local equilibrium of structure associated with the Zener limit.[17]

This effect is increased when there is inhomogeneous deformation
as a result of intergranular plastic anisotropy. In addition, a steep
strains and strain rate gradients are associated with FSP that provides inhomogeneous deformation. These are likely to make a significant contribution to the grain growth observed in practice and
affect grain growth in Zener pinned systems by perturbing the
grain structure geometry. Moreover, a new relationship for the calculation of the Zener drag pressure was described in which the
effect of the size distribution of nano-scale dispersed particles is
taken into account in addition to particle radius and volume fraction, which have been incorporated in the existing relationships.[18]
Mathematical investigations showed that the ratio of the Zener
drag pressure from the new equation to that from the existing

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Al/AlN nano-composite layers

equation is maximized when the number densities of all particles
with different sizes are equal. The size distribution of nano-scale
dispersed particles gives rise to a larger Zener drag pressure than
that having a narrow size distribution of nano-scale dispersed
particles.[18]
It can be concluded that severe hot deformation in the presence
of nano-sized AlN reinforcements affected grain growth. Thus,
grains were resulted with a mean size well beyond Zener prediction.
Micro hardness measurement
Figure 12a represents the micro-hardness profile on the cross section of the fabricated layers; measurements were carried out along
the width on a line parallel to its surface in a depth of ~0.5 mm for
F900, 63, F900, 125, and F1120, 125 nano-composite layers and F900, 63
layer (without introduction of AlN powder). Generally, the micro
hardness values of the nano-composite layers were found to be
greater than that of the as-received 6061-T6 Al substrate. Surface
material experiences sever plastic deformation at relatively high
temperature in FSP. Thus, finer matrix grains are resulted due to
the occurrence of dynamically restoration phenomena. According
to HallPetch relationship, decreasing grain size results in hardness
enhancement. All fabricated Al/AlN nano-composite layers exhibited much greater micro hardness values than that of the FSPed
layer (without introduction of AlN powder). AlN is a material with
hardness value greater than 18 GPa.[19] Having AlN reinforcements,
composite layers offer relatively great hardness values. A maximum
micro hardness value of ~164 HV was achieved for F900, 63 nanocomposite layer; this is much greater than ~103 HV of the

as-received 6061-T6 Al substrate. AlN volume fraction of this layer

was found to be ~9.6%. Lii et al. used squeeze casting to produce
Al/AlN composite layer with AlN volume fraction of 51 to 70%.[2]
The measured micro hardness value was found to be 93 to
145 HV.[2] It is clear that at a relatively lower AlN volume fraction,
quite high micro hardness value was achieved by introduction of
nano-sized powder into the stir zone. Abdoli et al. found that
addition of AlN powder with a volume fraction of 10% increases micro hardness value of mechanically milled aluminum by further
~50 HV.[20] It is interesting that dispersion of AlN reinforcements
was carried out by FSP at a relatively lower time; this increased micro hardness value of the as-received 6061-T6 Al substrate by further ~61 HV. Relatively, greater micro hardness value is expected
for mechanically milled product due to uniform dispersion of reinforcements in a nano-structured powder. However, a dense bulk
composite could hardly be achieved by subsequent cold pressing
of the nano-structured milled product.[20] On the other hand,
porosity-free microstructure can be achieved by FSP due to stirring
and forging actions imposed by the tool.
Comparison of micro hardness values of the three reported
Al/AlN nano-composite surface layers reflects that decreasing the
advancing speed and increasing the rotation speed lead to relatively harder Al/AlN nano-composite layer with relatively lower variation in regional micro hardness value. It is clear that both
strategies (i.e. decreasing the advancing speed and increasing the
rotation speed) are associated with increasing heat input, which
promotes matrix grain growth. Thus, such scenario is not in agreement with a greater hardness. It should be noted that AlN powder
volume fraction and its mean size and dispersion are important issues here. A relatively low substrate advancing speed resulted in
more AlN powder in the nano-composite layer (Figs 10a and 10b)
and in turn less powder scattering during FSP. Powder is placed
in front of pin tool. As the tool advancing speed increases, more
powder is pushed out of the groove by the advancing and rotating
pin. Fig. 10 shows that by increasing tool rotation and substrate advancing speeds, smaller particles are lost. On the other hand, by decreasing advancing speed, AlN volume fraction of the fabricated
layers increases (Figs 10a and 10b); this in turn increases mean micro hardness value. As the tool rotational speed increases, the velocity of material flow (which is complex in FSP due to motion at
various directions) increases. These motions break-up AlN clusters
0.004

0.0038

1:6061-T6 Al substrate
2:FSPed substrate
3:Al/AlN - F900,63
4:Al/AlN - F900,125
5:Al/AlN- F1120,125

0.0036

0.0035

0.003

0.002

0.0025

Wear Rate,
mg/m

0.0023
0.0018

0.002
0.0015
0.001
0.0005

Figure 12. The micro-hardness profiles of the fabricated Al/AlN nanocomposite layers using various process parameters and FSPed substrate
(without addition of AlN powder) employing a tool rotation and substrate
advancing speeds of 900 rpm and 63 mm/s, respectively, after three more
passes on their cross sections along the width (a) and depth (b).

Surf. Interface Anal. (2014)

0
1

Figure 13. Wear rates of the as-received and FSPed Al substrates, and
Al/AlN nano-composite surface layers (F900, 63, F900, 125, and F1120, 125).

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S. F. Kashani-Bozorg, M. Samiee and A. Honarbakhsh-Raoof

and disperse them uniformly in the aluminum matrix, which in turn
minimize variation in micro hardness values.
Moreover, it should be taken into account that in the case of
Al/AlN nano-composite layers, the enhancement of hardness was
caused not only by dispersion of hard AlN reinforcements and dynamic restoration phenomena associated with FSP but also the pinning effect of nano-sized AlN reinforcements that restricts matrix
grain growth (Fig. 11a vs. Figs 11b and 11c). As finer AlN particles
were dispersed more uniformly in a layer (Fig. 9a), finer mean matrix

grain size resulted (Fig. 11a). Furthermore, uniform dispersion of

fine nano-sized AlN reinforcements provides less scattering in
micro-hardness values.
It is interesting that FSPed substrate (without introduction of AlN
powder) offers lower micro hardness value than the as-received
6061-T6 substrate. Such behavior was reported earlier on friction
stir processing/welding of heat treatable 6063Al alloys[21]; using
transmission electron microscopy, it was shown that the hardness
profile depends greatly on the precipitate distribution and only

Figure 14. Friction coefficient as a function of wear distance for the as-received substrate (a) and fabricated Al/AlN nano-composite surface layers of F900, 63
(b), F900, 125 (c), and F1120, 125 (d).

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Al/AlN nano-composite layers

slightly on the grain size. The softened region is characterized by
dissolution and growth of the precipitates during thermal cycle of
friction stir welding.[22]
The micro-hardness profiles were also obtained on the cross section of the fabricated nano-composite layers (F900, 63, F900, 125, and
F1120, 125) along the depth (Fig. 12b); the hardness value of the
nano-composite layers decreased to the hardness of the underlying
substrate at a distance of ~33.5 mm from the top surface. These
profiles support uniform dispersion of AlN reinforcements in the
depth of the stir zone. Thorough material mixing is achieved by
multiple passes and adjusting tool rotation and substrate advancing speeds parameters.
Wear properties
Figure 13 show the wear rates (weight-loss divided by sliding distance) of the as-received and FSPed 6061 Al substrates and fabricated Al/AlN nano-composites (F900, 63, F900, 125, and F1120, 125
specimens). In general, addition of nano-sized reinforcements was
found to be advantageous to wear properties; the wear rates of
all Al/AlN nano-composite surface layers were lower than that of
the as-received substrate under a load of 16 N. The improved wear
resistance may be attributed to their greater hardness values; this
could decrease adhesion between the pin material and sliding disc.
Comparison of wear-loss data of the three reported Al/AlN nanocomposite layers reflects that a decrease in the advancing speed

and increase in the rotation speed lead to a Al/AlN nano-composite

layer with higher resistance to wear, e.g. F900, 63 layer exhibited
greatest AlN volume fraction (Fig. 10a), highest micro hardness
value (Fig. 12), and lowest weight-loss data (Fig. 13). Nearly uniform
dispersion of hard nano-sized AlN particles in a fine grained matrix
strengthened the layer against sliding wear. In other words, the direct load between the matrix surface and the disk reduced effectively as a result of AlN reinforcements.
Figure 14 shows friction coefficient values of the as-received substrate and Al/AlN nano-composites surface layers (F900, 63, F900, 125,
and F1120, 125) as a function of sliding distance. General fluctuations
in friction coefficient values are related to periodical accumulation
and elimination of wear debris on the worn specimen. The largest
and smallest fluctuations correspond to the as-received substrate,
0.72, and Al/AlN nano-composite layer (F900, 63), 0.30, having the
largest AlN volume fraction (9.6%). In general, large fluctuation in
friction coefficient values is in agreement with the domination of
adhesive wear mechanism (Fig. 14a). Contrary to this, Al/AlN
nano-composite layers reinforced by nano-sized AlN powder,
because of hardness enhancement, exhibited relatively less fluctuation in friction coefficient values (Figs 14b, 14c, and 14d).
Increasing the substrate advancing speed and tool rotation
speed resulted in surface layer with relatively larger friction coefficient values (Fig. 14). According to the microstructure of nanocomposite layers (Fig. 10), it can be deduced that the greater the
volume fraction of nano-sized AlN powder (Fig. 10a), the smaller

Figure 15. Worn-out surface of the as-received 6061-T6 Al substrate exhibiting relatively wide and deep deformed regions in the direction of sliding (a),
abrasive grooves, de-lamination of material (b), crack formation (c), and wear debris (d).

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S. F. Kashani-Bozorg, M. Samiee and A. Honarbakhsh-Raoof

the friction coefficient value (Fig. 14b). Nano-sized particles reinforced the material and decreased the direct load on aluminum matrix. All curves show an initial increase in friction coefficient values
(Fig. 14). The relative motion during dry sliding wear leads to material transfer from one surface to another; this could happen through
solid-state cold welding and localized bonding between the
contacting solid surfaces.[22] Thus, after a specific sliding distance,
the surface asperities were worn down, and the contact stress decreased owing to an increase in contact area for the same load; this
increased the friction coefficient.
Figure 15 exhibits worn-out surface of the as-received aluminum
substrate. Relatively wide and deep deformed regions with boundaries parallel to sliding direction were observed using a low magnification on scanning electron microscope (Fig. 15a). Complete local
surface matching between disc/specimen is associated with substantial increase in temperature; this increases friction coefficient
value and makes local welding. However, continuous sliding breaks
down local welded regions from the softer aluminum side. Thus,
plastically deformed regions were resulted with deformation morphology (Fig. 15b). This scenario is in agreement with relatively high
friction coefficient value of the as-received substrate (Fig. 14a). Adjacent to plastically deformed regions, abrasive grooves were observed (Fig. 15b); these are due to abrasive nature of hardened
steel against soft aluminum substrate, i.e. the as-received substrate
was continuously plowed during wear test.
Addition to these, surface delamination was found (Fig. 15b). This
was attributed to the large hydrostatic pressure acting near the asperity contact. Employing higher magnifications, micro cracks were
detected in abrasive grooves and deformed regions (Fig. 15c). During sliding wear, owing to imposed plastic deformation, dislocations were introduced in the sub-surface of the worn material.
The generated dislocations led to eventual formation of cracks or
voids in the sub-surface regions. It is likely that these cracks formed
at the particle/matrix interface. Fragmentation of particles could
also lead to de-cohesion of particle/matrix interface, generating
voids.
The cracks and resultant voids coalesced with eventual delamination of material and production of wear debris (Figs 15b
and 15d).
Chemical analysis and morphology of the worn-out surface and
its associated debris can help to figure out the wear behavior with

more details. EDS analyses on wear debris of the worn-out surface

of the as-received Al substrate showed substantial concentration
of O (e.g. Fig. 16); this is indicative of surface oxidation due to
increased surface temperature, which occurred during pin/
specimen contact.
It can be deduced that adhesive mechanism is the dominant
wear mechanism for the unreinforced Al substrate. It should be
noted that abrasive mechanism is also active when local matching
was not achieved during wear.
In addition, the worn surface of the FSPed substrate exhibited severe deformed regions (Fig. 17). Similar features were found close
to those of the as-received substrate.
Figure 18 exhibits worn-out surfaces of Al/AlN nano-composites;
F900, 63 (Fig. 18a), F900, 125 (Fig. 18b), and F1120, 125 (Fig. 18c). Again,
plastically deformed regions were observed in the direction parallel
to sliding in all composite layers. However, these regions were
found to be relatively narrower and shallower than those of the
as-received substrate. In addition, finer and limited plastically

Figure 17. Worn-out surface of the FSPed substrate (with no AlN addition)
showing heavily deformed regions in the direction of sliding.

Figure 16. Energy dispersive spectrum of wear debris on the worn-out surface of the as-received 6061-T6 Al substrate showed substantial concentration of O.

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Surf. Interface Anal. (2014)

Al/AlN nano-composite layers

Figure 18. Worn-out surfaces of AlN/Al nano-composite layers; F1120, 125 (a), F900, 125 (b), and F900, 63 (c), deformed regions and pits or regions of removed
material (d), fine abrasive grooves (e).

damaged regions were observed as the volume fraction of AlN

reinforcements increased (Figs 18c and 18d). Moreover, narrower
grooves than those of the untreated substrate were detected
using higher magnification (Fig. 18e). Al/AlN nano-composite layer
(F900, 63) showed the least damaged surface; this is attributed to its
relatively high micro hardness value (achieved by AlN volume fraction of 9.6%).
EDS analyses on wear debris of the worn-out Al/AlN nanocomposite specimen (F900, 63) showed substantial concentrations
of Fe and O (e.g., Fig. 19). In addition, new elements such as C, Cr,
and Cu were found; these elements were originated from disc
material and transferred from disc to pin (specimen) surface during
the wear process. Hard AlN reinforcements could penetrate and cut
steel disc, causing Fe-based debris. In addition, owing to an
increase in surface temperature, oxidation of debris is inevitable.
In general, relatively shallow and narrow abrasion grooves and
small deformed regions are associated with relatively low rate of

wear. Thus, in the case of Al/AlN nano-composite specimens abrasive and adhesive wear are both active. They showed better resistance to deformation during wear tests due to their relatively
high hardness values. In this case, adhesive wear is limited and wear
proceeds mainly by the domination of abrasive mechanism with
relatively lower surface weight losses.

Conclusions
In the present investigation, nano-sized AlN powder was introduced into the stir zone of 6061-T6 Al alloy work pieces using friction stir processing. The results are summarized as below:
1. Sound layers were formed on 6061-T6 Al work pieces using
tool rotation and substrate advancing speeds in the range
of 9001400 rpm and 63310 mm/s, respectively.
2. The FSPed (without introduction of AlN powder) stir zone
showed a microstructure of fine dynamically restorated
equiaxed grains with a mean size of ~11 m.
3. Clusters of AlN powder were formed in a non-uniform fashion
(as band regions) after the first pass. Break-up of clusters and
near uniform dispersion were achieved after three additional
passes.
4. The addition of nano-sized AlN reinforcements was found to
be advantageous in surface hardening; the fabricated nanocomposite layer with an AlN volume fraction of ~9.6% exhibited a micro hardness value of ~164 HV; this is much higher
than that of the underlying substrate (~103 HV). In addition,
the nano-composite layer showed a wear rate of about one
half of that of the FSPed (without introduction of AlN powder)
and untreated substrates.

Acknowledgements
Figure 19. Energy dispersive spectrum of wear debris on the worn-out
surface of Al/AlN nano-composite specimen (F900, 63) showed substantial
concentrations of Fe and O (F900, 63).

Surf. Interface Anal. (2014)

Financial supports from the University of Tehran and Iran Nanotechnology Initiative are gratefully acknowledged.

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S. F. Kashani-Bozorg, M. Samiee and A. Honarbakhsh-Raoof

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