Copyright 2012 by American Scientic Publishers

All rights reserved.

Printed in the United States of America

Science of Advanced Materials

Vol. 4, pp. 18, 2012
(www.aspbs.com/sam)

Wear Behavior of Spark Plasma Sintered Al2124

Aluminum Alloy Containing Carbon Nanotubes
A. M. Al-Qutub1 , A. Khalil1 , N. Saheb1 2 , Al-Aqeeli1 2 , and T. Laoui1 2
1

Department of Mechanical Engineering, King Fahd University of Petroleum and Minerals,

Dhahran-31261, Saudi Arabia
2
Center of Excellence in Nanotechnology, King Fahd University of Petroleum and Minerals,
Dhahran-31261, Saudi Arabia

ABSTRACT

1. INTRODUCTION
There has been signicant research on improving wear
resistance of aluminum and its alloys either by different types of heat treatments and coatings or by incorporating certain percentage of a different material to form
aluminum metal matrix composite (Al-MMC). The latter
approach has been more attractive and effective as the
former approach involves strengthening the material only
from the exterior which may not remain effective with the
passage of time. In contrast, the latter approach involves
strengthening the material as a whole on the continuum
level so that the properties remain unaffected. Several types
of ceramic particles such as SiC14 and alumina58 have
been tested as reinforcements for improving wear resistance of aluminum and its alloys. Due to higher hardness
and strength of the reinforcement phase, it has been commonly observed that wear resistance of aluminum alloys
increased with the increase of the volume fraction of the
reinforcement.

Author to whom correspondence should be addressed.

Email: nouari@kfupm.edu.sa
Received: xx Xxxx xxxx
Accepted: xx Xxxx xxxx

Sci. Adv. Mater. 2012, Vol. 4, No. xx

Recently, researchers used nanoparticles as reinforcing

agents to improve wear resistance of aluminum alloys.
One of the candidate nanoreinforcements for this purpose
was carbon nanotubes (CNTs)9 because of its exceptional
strength10 in addition to its light weight. However, little
work has been reported on the effect of CNTs addition
on wear behavior of aluminum alloys. Moreover, wear
mechanism and optimum CNT content have not been sufciently studied and the data available are contradictory.
Zhou et al.11 reported steady decrease in wear rate and
friction coefcient of aluminum up to 20 vol.% CNTs.
Kim et al.12 found that only 1 wt.% CNTs was an optimum content for best tribological characteristics of aluminum. Choi et al.13 reported that 4.5 vol.% CNTs was the
optimum content for lowest wear rate and friction coefcient of aluminum. The difference in optimum CNT content could be due to CNTs dispersion technique, composite
fabrication method, and type of wear test used. The aim
of this work is to investigate the inuence of CNTs addition on wear behavior of spark plasma sintered Al2124
alloy under dry sliding against a steel counterface at a constant sliding speed and different loads using pin-on-disk
conguration.

1947-2935/2012/4/001/008

doi:10.1166/sam.2012.1409

ARTICLE

In this work, the wear behavior of spark plasma sintered Al2124 alloy and its composite containing 1 wt.% carbon nanotubes (CNTs) was investigated at a constant sliding speed and different loads against AISI 4140 steel
counterface using pin-on-disk conguration. It was found that the addition of CNTs improved wear resistance
of Al2124 alloy under lower loads. At higher loads, remaining pores caused crack development and propagation and consequently severe delamination resulting in poor wear resistance of the composite as compared to
the monolithic alloy. Mixed modes of wear were observed for the monolithic alloy and the composite. Under
lower loads, the composite mainly displayed abrasion with some localized delamination whereas the monolithic
alloy showed signicant delamination. Under intermediate loads, adhesion was found to be dominant for the
composite as compared to microploughing observed for the monolithic alloy. Under the highest applied load
of 25 N, the composite displayed severe subsurface fracturing and delamination in the form of large akes as
compared to the monolithic alloy in which the delamination was less intense due to the formation of a stable
oxide layer.
KEYWORDS: Metal Matrix Nanocomposites, Powder Processing, Spark Plasma Sintering, Wear.

Wear Behavior of Spark Plasma Sintered Al2124 Aluminum Alloy Containing Carbon Nanotubes

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2. MATERIALS AND EXPERIMENTAL

PROCEDURES
Al2124 prealloyed powder, supplied by Aluminium Powder Co. Ltd., UK and 95 percent pure multi-walled carbon
nanotubes (MWCNTs) were used in this work. Al2124
alloy powders containing 0.5, 0.75, 1 and 2 wt.% CNTs
were sonicated in a probe sonicator for 30 minutes using
ethanol. The sonicated mixture was charged into cylindrical stainless steel vials together with stainless steels
balls. A ball to powder weight ratio of 10:1 was used
and wet milling was carried out at room temperature
for 1 hour at 200 rpm in argon atmosphere to prevent
the oxidation of the powders. After drying, the powders
were further dry milled for 15 minutes to breakdown the
agglomerates. The powders were consolidated using spark
plasma sintering (SPS) process. Sintering was carried out
at 450  C for 20 minutes under a pressure of 35 MPa.
More details on the effect of processing on the dispersion of CNTs and spark plasma sintering were reported
elsewhere.1416 The density of sintered samples was measured using Alfa Mirage electronic densimeter (model
MD-300s) having accuracy of 0.001 g/cm3 and quantied
according to Archimedes principle. Vickers microhardness
of spark plasma sintered samples was measured using a
digital microhardness tester (Buehler, USA) using a load
of 100 gf and dwell time of 12 seconds. The reported hardness values represent the average of 10 readings taken at
different locations across the specimen.
Cylindrical pins having diameter of 6 mm and length
of 12 mm were prepared from sintered monolithic alloy
and the composite containing 1 wt.% CNTs. The at surface of the pin was carefully ground with 600 grit size
abrasive paper and then polished using a 9 micron diamond polishing suspension. AISI 4140 steel disk with a
hardness of 24 HRC was used as counterface. An average Ra value of 0.3 microns was maintained for the disk
through grinding it with alumina abrasive wheel. The surfaces of the pin and disk were cleaned with ethanol before
running the tests. Pin-on-disk wear tests were conducted
at room temperature using a pin-on-disk tribometer satisfying ASTM G99 standard. The tests were carried out
under dry sliding conditions at constant sliding speed of
0.5 m/s and applied loads ranging from 5 to 25 N. For
all the tests, the sliding distance was kept constant at
500 m for which steady state conditions prevailed. Each
unique test was conducted three times. A Tescan Lyra-3
Field Emission Scanning Electron Microscope (FESEM)
with integrated Energy Dispersive X-Ray Spectroscopy
(EDS) facility was used for analyzing the worn specimens and the carefully collected debris to understand
the wear mechanisms. The worn specimens were washed
with ethanol via sonication for 5 minutes prior to SEM
and EDS analysis. Microscopic examination of counterface disk was also carried out to support the obtained
results.
2

Al-Qutub et al.

3. RESULTS AND DISCUSSION

3.1. Microstructure and Hardness
Figure 1(a) shows a pore free microstructure of spark
plasma sintered Al2124 monolithic alloy. A relative density of 99.17% and a hardness of 116 HV were achieved.
Addition of 0.5, 0.75, and 1 wt.% CNTs led to lower
densication compared to the monolithic alloy as a result
of some remaining pores and agglomeration of CNTs.
However, it increased the hardness to a maximum value
of 121 HV at 1 wt.% CNTs. Typical microstructure
of Al2124 alloy containing 1 wt.% CNTs is shown in
Figures 1(b) and (c). A relative density of 98.36% was
achieved. A further increase of CNTs content to 2 wt.%
resulted in poor densication and sharp decrease in hardness; this is due to poor densication, presence of pores,
and excessive CNT agglomeration. Poor densication and
mechanical properties of aluminum reinforced with higher
CNT content were reported in many studies due to excessive CNT clustering.12 13 1721 The composite containing
1 wt.% CNTs had the highest hardness and was selected
for wear analysis along with the monolithic alloy.
3.2. Wear Rate
The wear rate with standard deviation for the Al2124
monolithic alloy and the composite as a function of load is
presented in Figure 2. For both materials, the wear rate was
found to increase with increasing load. Under lower loads
of 5 N and 10 N, the composite displayed better wear resistance as compared to Al2124 monolithic alloy whereas for
loads of 15, 20, and 25 N, the Al2124 monolithic alloy displayed better wear resistance compared to the composite.
The wear rate of the composite almost doubled as the load
increased from 10 N to 15 N, but no such drastic increase
was observed for the Al2124 monolith alloy up to a load
of 20 N. However, at a load of 25 N, signicant increase
in wear rate was observed. Also, the composite displayed
very high wear rate with very large standard deviation as
compared to the monolithic alloy for loads of 15, 20, and
25 N. These results show that addition of 1 wt.% CNTs
improves the wear resistance of Al2124 alloy under lower
loads (mild conditions). At higher loads (sever conditions),
the pores in the composite and CNT agglomerates serve as
source of crack nucleation and growth causing excessive
subsurface fracturing and delamination leading to higher
wear rate. Also, weak adhesion of CNTs with the matrix
can be another reason for the observed trend. It has been
shown1 that wear rate of materials fabricated through powder metallurgy is very sensitive to its percent porosity
because the pores serve as a source of crack nucleation
which causes severe subsurface fracturing. The observed
trend could also be due to the difference in wear mechanisms of the two materials as discussed below.
The better wear resistance of the composite compared
to the monolithic alloy at lower loads is in agreement with
Sci. Adv. Mater., 4, 18, 2012

Al-Qutub et al.

Wear Behavior of Spark Plasma Sintered Al2124 Aluminum Alloy Containing Carbon Nanotubes

(a)

20 m
(b)
Fig. 2. Wear rate as a function of load for the Al2124 alloy and
composite.

(c)

5 m
Fig. 1. SEM micrographs of specimens sintered at 450  C (a) Al2124,
(b) composite, and (c) magnied part indicated by arrow in (b).

other studies which reported that aluminum metal matrix

composites display better wear resistance at low loads and
there exists a critical load after which the reinforcement
has negative effect on the wear resistance of the matrix.
Wang et al.22 studied the effect of adding 15 vol.% Ni3 Al
on the wear resistance of Al6092 alloy and found that up
to a load of 91 N, the composite displayed better wear
resistance, however as the load was increased to 140 N,
the trend reversed. Korkut23 also reported a similar trend
for Al2024\SiFe\Alumina composite prepared by powder
metallurgy. He found that as the conditions switch from
Sci. Adv. Mater., 4, 18, 2012

3.3. Analysis of Worn Surfaces

Figure 3 shows SEM micrographs of worn surfaces of
Al2124 monolithic alloy and the composite under different
3

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20 m

mild to severe, the composite starts displaying higher wear

rates as compared to the monolithic alloy. The authors of
the above studies attributed this behavior to the brittle fracture and fragmentation of reinforcement at higher loads.
Sudarshan et al.24 also reported similar trend while studying wear behavior of A356 aluminum alloy reinforced with
y ash particles. They found that the composite containing lower proportion of y ash particles displayed better
wear resistance as compared to monolithic alloy at lower
loads only. It was proposed that at higher loads, the interface between the matrix and the y ash particle provides
preferential path for the growth of subsurface cracks.
Also, it can be noted that even under lower loads, the
improvement in wear resistance of Al2124 alloy upon
CNT addition was not signicant. At loads of 5 and
10 N, the average wear rate of the composite decreased by
0.5 mm3 /km and 0.65 mm3 /km, respectively, as compared
to the monolithic alloy. The same trend was observed by
Zhou et al.11 who reported marginal improvement in wear
resistance of aluminum-CNT composites; where a wear
rate of 0.0135 mg/m for monolithic aluminum was reduced
to a minimum value of around 0.01 mg/m for aluminum
reinforced with 20 vol.% CNTs. Kim et al.12 also reported
only slight decrease in wear rate for aluminum-CNT composites. In their investigation, the wear rate of monolithic
aluminum was found to be around 11.5 mg which reduced
to a minimum value of about 9.5 mg for 1 wt.% CNTs. It is
worth mentioning here that in the present work and other
works,11 12 a pin-on-disk conguration was used. Whereas
Choi et al.13 used ball-on-disk conguration and reported
decrease in wear rate from 75 mg to 35 mg upon 4.5 vol.%
CNT addition in aluminum.

M AG NI F I C AT I O N

Al-Qutub et al.

LOAD

5N

15 N

25 N

50 m

50 m

50 m

20 m

20 m

20 m

50 m

50 m

50 m

20 m

20 m

20 m

Fig. 3.

X500
X1000

Al2124 + 1 wt .% C NT s

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X1000

Al2124

X500

M AT E R I AL

Wear Behavior of Spark Plasma Sintered Al2124 Aluminum Alloy Containing Carbon Nanotubes

SEM micrographs of worn surfaces of monolithic alloy and composite.

loads and at different magnications. At 5 N, the monolithic alloy is characterized by abrasion in addition to
noticeable amount of delamination. Also at higher magnication, tiny cracks can be observed in the delaminated regions. On the other hand, at 5 N, the composite
is mainly characterized by abrasion with some localized
delamination at few locations and subsurface cracking can
be hardly observed. This shows the strengthening effect
of CNTs and explains why the wear rate of composite
is lower as compared to the monolithic alloy at lower
load. At 15 N, the monolithic alloy is characterized by
ploughing wear. The long scars represent subsurface plastic deformation caused mainly due to ploughing. In contrast, at 15 N, this ploughing effect is not evident in case
of composite. The composite is mainly characterized by
localized pits representing adhesion of material from the
specimen to the counterface. Also, as can be seen at higher
4

magnication, the surface has tiny white particles possibly due to the transfer of iron from the counterface. Some
tiny cracks can be observed, especially around the adhered
regions showing the onset of delamination. The switching
of wear mechanism from localized delamination to adhesion explains the sharp increase in wear rate from 10 N to
15 N in case of composite. At the maximum applied load
of 25 N, in addition to abrasion caused by microdebris, the
monolithic alloy is characterized by deep grooves showing
delamination due to the removal of thicker akes. Also,
at higher magnication, some cohesion of particles can
be observed inside the deep groove which may be representing some oxide formation. In contrast, the morphology
of composite at 25 N is completely different. The surface is characterized by severe damage due to large scale
delamination. The tiny cracks developed in composite at
a lower load propagated freely at a higher load. The long
Sci. Adv. Mater., 4, 18, 2012

Al-Qutub et al.

Wear Behavior of Spark Plasma Sintered Al2124 Aluminum Alloy Containing Carbon Nanotubes

(a)

1 mm

(b)

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distance crack propagation caused severe subsurface fracturing and delamination and hence extremely high wear
rate for the composite. Figure 4 shows the overall morphology of worn surfaces of the monolithic and the composite at an applied load of 25 N. From Figure 4(a), it is
evident that the monolithic alloy underwent plastic deformation due to ploughing effect. As seen in Figure 4(c), the
corners of the monolithic alloy specimen are characterized
by plastic deformation and thermal softening representing
ductile nature of the monolithic alloy. In contrast, as evident from Figure 4(b), the composite is characterized by
severe subsurface fracturing and delamination, especially
at the corners, Figure 4(d), representing the brittle nature
of the composite. EDS analysis of worn surfaces at different loads are presented in Figure 5. There is no signicant difference in the composition of the monolithic alloy
and the composite at 5 N. However, at higher loads, the
amount of oxygen is much higher in the monolithic alloy
as compared to the composite which shows the formation of stable oxide layer on the monolithic alloy surface.
This oxide layer might served as a protective layer causing
lower wear rate of the monolithic alloy as compared to
the composite. Also, at higher loads, the composites surface is mainly comprised of aluminum, especially at 25 N
where almost 90 percent of the surface is comprised of
aluminum with negligible proportion of iron. This shows
that due to excessive fracturing and delamination in the
composite at higher load, stable iron oxide layer failed to
form and if some oxide layer formed or some iron adhered
from the counterface, it failed to survive because of the
frequent fracturing and delamination of material from the
specimens surface.

1 mm

(c)

3.4. Analysis of Debris

Figure 6 shows the morphology of debris formed at different loads in case of monolithic alloy and composite.
At 10 N, the debris of monolithic alloy is mainly characterized by larger akes, Figure 6(a), whereas the debris
of composite is characterized by smaller akes in addition to tiny particles, Figure 6(b). This is agreement with
the SEM analysis of worn surfaces where delamination
was more pronounced in case of monolithic alloy at lower
loads. At 20 N, the opposite trend is observed. While the
monolithic alloy debris is mainly composed of delaminated
akes, Figure 6(c); the composites debris is characterized
by very large akes due to excessive subsurface damage
of the specimen, Figure 6(d). This is also in agreement
with the SEM analysis of worn surfaces where at higher
loads, the composite displayed excessive fracturing and
delamination due to long distance crack propagation.
The composition of debris shown in Figure 6 was analyzed through EDS and shown in Figure 7. These results
are in good agreement with those shown in Figure 5. The
monolithic alloy debris contains signicant proportion of
iron and oxygen. This shows the formation of thick iron
Sci. Adv. Mater., 4, 18, 2012

200 m

(d)

200 m

Fig. 4. SEM micrographs of worn specimens at a load of 25 N of

(a) Al2124 alloy and (b) composite, (c) and (d) edges of specimens shown
in (a) and (b), respectively.

Wear Behavior of Spark Plasma Sintered Al2124 Aluminum Alloy Containing Carbon Nanotubes

Al-Qutub et al.

(a)

200 m

ARTICLE

(b)

Fig. 5. EDS analysis of worn surfaces of (a) Al2124 alloy and (b) composite pins under different loads.

oxide layer on the specimen during steady state wear process. As the test continued, the oxide layer is removed
from the surface due to weak adhesion with the specimen
and hence became part of the debris. On the other hand,
there is only slight formation of iron oxide layer in case
of composite and this layer is not stable at all due to frequent fracturing and delamination of composites surface
at higher loads. Also, the proportion of aluminum in composites debris is much higher as compared to monolithic
alloy which represents frequent delamination of aluminum
in the form of large akes. This may be attributed from
one side to the cracks developed due to CNT agglomerates
and from other side to the weak adhesion between CNTs
and the matrix at some locations in the composite.

200 m

(c)

200 m

(d)

3.5. Analysis of Counterface

The microscopic analysis of counterface at an applied
load of 10 N and 20 N is shown in Figure 8. While the
counterface is mainly characterized by abrasion in case of
monolithic alloy, Figures 8(a) and (c), the counterface in
case of composite is also characterized by adhered lumps
from the specimen, marked with arrows in Figures 8(b)
and (d). Also it can be seen that the size of the adhered
lumps increased with the increase of the load. This is in
agreement with the SEM results of worn surfaces where
signs of adhesion in case of composite were very clear.
This shows that adhesive wear is also prominent in the
composite.
6

200 m
Fig. 6. SEM micrographs of debris formed in case of monolithic alloy
(left) and composite (right) at an applied load of 10 N (a) and (b) and
20 N (c) and (d).
Sci. Adv. Mater., 4, 18, 2012

Al-Qutub et al.

Wear Behavior of Spark Plasma Sintered Al2124 Aluminum Alloy Containing Carbon Nanotubes

(a)

(b)

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Fig. 7. EDS analysis of debris of (a) Al2124 alloy and (b) composite
under different loads.

In order to verify that these lumps represent adhesion

from the specimen to the counterface, the lumps were
mechanically peeled off from the counterface and their
composition was analyzed through EDS and the results
are shown in Figure 9. As evident, the lumps are mainly
composed of aluminum and this conrms that the adhesion actively occurred from the pin to the counterface in
case of composite. Signicant proportion of oxygen was
also found in the lump which shows formation of aluminum oxide. The continuous abrasion of the specimens
by these adhered lumps having signicant amount of hard
aluminum oxide could be another reason for higher wear
rate of composite at higher loads.
The wear mechanisms observed for the Al2124-CNT
composite in the present work can be compared to those
observed by Zhou et al.,11 Kim et al.12 and Choi et al.13
for Al-CNT composites. Zhou et al. found oxidation as the
main wear mechanism for Al-CNT composite. They proposed the formation of alumina layer on the composite and
its subsequent delamination causing abrasion between the
specimen and the counterface. This single specic wear
mechanism may be due to the fact that all tests were performed under a constant load and sliding speed with varying CNT content. On the other hand, Kim et al. observed
mixed abrasive and adhesive wear for Al-CNT composites with varying CNT content at a xed load and sliding speed. They also reported minimal oxidation wear
for the composite containing 1 wt.% CNTs. Choi et al.
reported microploughing and delamination as the dominant
Sci. Adv. Mater., 4, 18, 2012

(c)

(d)

Fig. 8. Microscopic images (X20) of worn track on counterface in case

of monolithic alloy (left) and composite (right) at an applied load of 10 N
(a) and (b) and 20 N (c) and (d).

Wear Behavior of Spark Plasma Sintered Al2124 Aluminum Alloy Containing Carbon Nanotubes

Al-Qutub et al.

consequently severe delamination resulting in poor wear

resistance of the composite as compared to the monolithic alloy. Mixed modes of wear were observed for the
monolithic alloy and the composite. Under lower loads,
the composite mainly displayed abrasion with some localized delamination whereas the monolithic alloy showed
signicant delamination. Under intermediate loads, adhesion was found to be dominant for composite as compared to microploughing observed for the monolithic alloy.
Under the highest applied load of 25 N, the composite
displayed severe subsurface fracturing and delamination in
the form of large akes as compared to the monolithic
alloy in which the delamination was less intense due to
the formation of a stable oxide layer.

ARTICLE

Acknowledgment: The authors would like to acknowledge the nancial support for this work provided by King
Abdul Aziz City for Science and Technology (KACST)
through research project number ARP-28-122.

References and Notes

Fig. 9. EDS analysis of peeled off lumps from the counterface in case
of composite specimens.

1.
2.
3.
4.
5.

wear modes for Al-CNT composites. At higher loads,

they observed more delamination which is in agreement
with the present work where excessive delamination was
observed for composite at the maximum applied load of
25 N. The different modes of wear of Al-CNT composites
reported in literature may be due to different CNT contents, composite fabrication method, and wear test parameters (speed and load). However, the present work claries
that the wear behavior of Al-CNT composites is largely
inuenced by the applied load and there exist a critical
load at which the pores inside the composite become active
resulting in long distance crack propagation and subsequent delamination of the material. As a consequence,
CNTs could have a negative inuence on wear resistance
of aluminum and its alloys under severe conditions.

6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
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18.

4. CONCLUSION
Pin on disk wear tests at a constant sliding speed of
0.5 m/s and varying loads from 5 to 25 N against
AISI 4140 steel counterface showed that CNTs is candidate reinforcement for improving wear resistance of
Al2124 alloy under lower loads. At higher loads, remaining pores caused crack development and propagation and

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