RAMKUMAR R.: DRY SLIDING WEAR BEHAVIOUR OF CARBON NANOTUBE/ALUMINA/EPOXY HYBRID NANOCOMPOSITES
277–283
DRY SLIDING WEAR BEHAVIOUR OF CARBON
NANOTUBE/ALUMINA/EPOXY HYBRID NANOCOMPOSITES
DRSNA OBRABA HIBRIDNIH NANOKOMPOZITOV,
SESTAVLJENIH IZ OGLJIKOVIH NANOCEVK, ALUMINIJEVEGA
OKSIDA IN EPOKSIDNE SMOLE
Ramkumar R.
1
, Sabarinathan C.
2*
, Rajeswaran M.
3
, Prathap P.
3
,
Sankar Ganesh R.
4
1
Department of Mechanical Engineering, St Xaviers Polytechnic College, Sivgangai, Tamil Nadu 630302, India
2
Department of Automobile Engineering, Hindusthan College of Engineering and Technology, Coimbatore, Tamil Nadu 641032, India
3
Department of Mechanical Engineering, Sri Krishna College of Technology, Coimbatore, Tamil Nadu 641042, India
4
Department of Automobile Engineering, Hindusthan College of Engineering and Technology, Coimbatore, Tamil Nadu 641032, India
Prejem rokopisa – received: 2023-12-07; sprejem za objavo – accepted for publication: 2024-03-13
doi:10.17222/mit.2023.1068
In the field of materials science, polymer composites have been extensively used in various industries such as marine, automo-
tive, aerospace, sports and other industries due to their good dimensional stability and excellent structural properties. In this
present research investigation, epoxy served as the polymer material, while multi-walled carbon nanotubes (MWCNTs) and alu-
mina nanofillers were employed for reinforcing the matrix through hybridization. The wear characteristics of the composite ma-
terial were examined under dry sliding conditions, employing a pin-on-disc machine with a track diameter of 50 mm. The load
on the specimen was varied between low (20 N), medium (40 N) and high (60 N), while the weight fraction of the hybrid
nanofillers underwent variations in a range of 0.1–0.5 w/% with an increment of 0.1 w/%. The results showed that the reinforce-
ment of hybrid nanofillers significantly reduces the wear phenomena of the composite material. Hybrid nanocomposites with
(0.1, 0.2 and 0.3) w/% of MWCNTs-Al2O3 exhibit noteworthy advancements in the wear resistance. Particularly the 0.3 w/%
MWCNTs-Al2O3 hybrid nanocomposite demonstrates exceptional wear resistance compared to pure epoxy. The incorporation of
0.3 w/% of MWCNTs-Al2O3 results in a significantly improved wear resistance, with enhancements of (83, 81 and 80) % ob-
served during low (20 N), moderate (40 N) and high (60 N) loading conditions, respectively, compared to pure epoxy. Similarly,
deformation, delamination and filler plugging were observed with medium and high load. The surface morphology of the worn
specimens was assessed through the application of field emission scanning electron microscopy.
Keywords: wear, epoxy, MWCNTs, alumina, morphology analysis
Nova spoznanja o kompozitnih materialih na osnovi polimerne matrice so prispevala k njihovi intenzivniuporabi na razli~nih
industrijskih podro~jih kot so ladjedelni{tvo, proizvodnja avtomobilov, letalska industrija, industrija izdelave {portne opreme in
{e na mnogo drugih.Te vrste kompozitov imajo dobro dimenzionalno stabilnost in odli~ne strukturne lastnosti. V tem ~lanku
avtorji opisujejo raziskavo obrabe hibridnega kompozita s polimerno matrico in oja~itveno fazo iz ve~stenskih ogljikovih
nanocevk in delcev aluminijevega oksida. Drsno obrabo kompozitnega nateriala so dolo~ili z napravo, ki ima vrtljivi disk in trn,
ki pod izbranim tlakom drsi po preizku{ancu (angl.: pin-on-disc machine)s premerom sledi 50 mm. Izbrali so naslednje
obremenitve na trnu: nizko (20 N), srednjo (40 N) in visoko (60 N), medtem ko se je dele` hibridnega polnila v kompozitu gibal
med med 0,1 w/% in 0,5 w/% v korakih po 0,1 w/%. Rezultati preizkusov so pokazali, da dodatek polnila oziroma oja~itvenih
faz znatno zmanj{a drsno obrabo hibridnega kompozita. Hibridni nanokompozitiz 0,1 w/%, 0,2 w/% in 0,3 w/% polnila so imeli
ob~utno bolj{o odpornost proti drsni obrabi.Hibridni kompozit z 0,3 w/% polnila pa je imel {e posebej dobro odpornost proti
obrabi in sicer: kompozit z 0,3 w/% polnila je imel za 83 % manj{o obrabo pri obremenitvi 20 N, za 81 % manj{o obrabo pri
obremenitvi 40 N in za 80 % manj{o obrabo pri obremenitvi 60 N v primerjavi s ~istim epoksijem. Opazovali so tudi
deformacijo, cepljenje (delaminacija) in utrditev nanodelcev v hibridnih kompozitih v odvisnosti od masne vsebnosti polnila.
Povr{insko morfologijo obrabljenih preizku{ancev so opazovali s pomo~jo vrsti~nega elektronskega mikroskopa na emisijo pol-
ja elektronov.
Klju~ne besede: obraba, epoksi, ve~stenske ogljikove nanocevke, aluminijev oksid, morfolo{ka analiza
1 INTRODUCTION
Epoxy resins are extensively utilized in scientific and
technological applications, covering the marine, automo-
tive, aerospace and sports industries, due to their remark-
able mechanical properties.
1,2
However, the wear phe-
nomena and coefficient of friction exhibited by pure
epoxy are substantial.
3
Thus, hybrid nanocomposites
have emerged as a novel category of materials, augment-
ing the performance of composite materials by unlocking
novel characteristics and facilitating distinctive interac-
tions among materials. Numerous studies indicate that
hybrid nanocomposites exhibit elevated mechanical and
thermal properties in comparison to traditional compos-
ites.
4–7
Due to their increased aspect ratio and noteworthy
mechanical characteristics, fitting physical, thermal and
electrical properties, carbon nanotubes (CNTs) are pres-
ently acknowledged as a pivotal category of nano-
material for the synthesis of polymer-infused nanocom-
posites. Carbon nanotubes (CNTs) have the capability to
Materiali in tehnologije / Materials and technology 58 (2024) 3, 277–283 277
UDK 539.375.6:54-311 ISSN 1580-2949
Original scientific article/Izvirni znanstveni ~lanek MTAEC9, 58(3)277(2024)
*Corresponding author's e-mail:
c.sabarinathan@gmail.com (Sabarinathan C.)

reinforce a polymeric matrix, enhance its toughness, and
retard the propagation of cracks by establishing a bridg-
ing mechanism that binds crack surfaces.
8,9
Hence, re-
searchers in polymer science are actively seeking alter-
native strategies for the dispersion of CNTs within
polymer matrices. In recent times, the integration of
CNTs with inorganic additives has been observed to sub-
stantially enhance mechanical properties when compared
with individual filler systems. In recent advancements,
alumina (Al
2
O
3
) has emerged as an integral hybrid ele-
ment within the composition of CNT hybrid compounds,
playing a role as the filler in polymer composite sys-
tems.
10
The widespread adoption of Al
2
O
3
in hybridiza-
tions alongside CNTs can be attributed to their elevated
hardness, refractoriness, exceptional dielectric and fa-
vourable thermal properties.
11
In this study, the hybrid compound of CNT-Al
2
O
3
was synthesized through the CNTs on alumina particles,
employing a catalyst precursor. High-density polyethyl-
ene exhibits admirable tensile and flexural properties,
however, its proneness to tribological behaviour limits its
use in minimum-load industrial application components.
Furthermore, the incorporation of 0.1 w/% graphite
nanoplatelets and graphene oxide demonstrated a lower
contact pressure coupled with an increase in the wear re-
sistance.
13
Experiments conducted on multi-filler rein-
forced epoxy composites revealed enhancements in the
tensile strength, tensile modulus, elongation at break,
and wear resistance. These improvements were attributed
to the reinforcement of multiple fillers and their compati-
bility with the epoxy matrix.
14
The study aimed to evalu-
ate the influence of MXene@Ag hybrids on the thermal,
mechanical, and tribological properties of epoxy resin.
The findings indicated a substantial reduction in the
tribological properties, namely wear phenomena and
friction characteristics of the composites when compared
to the values observed for epoxy resin.
15
Carbon nano-
tubes (CNTs) were synthesized and dispersed within the
matrix of magnesium (Mg) with the aid of alumina as a
‘vehicle.’ This approach resulted in notable enhance-
ments in the mechanical properties. Optimizing both me-
chanical and electrical characteristics necessitates a stra-
tegic improvement in the distribution of the hybrid filler
within the epoxy matrix. An increased weight percentage
of the filler will increase the mechanical properties and
heat conductivity of ZrB2 and decrease the smoothening
of the hybrid composites due to the heat accumulation
due to friction with a significant heat transfer. This phe-
nomenon contributes to the reduction in the wear and ad-
hesive wear of epoxy hybrid composites.
16
Numerous research endeavours are dedicated to ad-
vancing polymer materials through the incorporation of
nanofillers, with a specific emphasis on hybrid compos-
ites. This pursuit aims to not only enhance tribological
properties but also to achieve multifunctional materials.
Recent publications extensively delved into elucidating
advancements in the mechanical and thermal properties
achieved by incorporating MWCNTs-Al
2
O
3
hybrids into
a polymer matrix. However, there have been limited in-
vestigations on the prediction of tribological perfor-
mance and determining the optimum weight of hybrid
composites. Consequently, the potential advantages of
MWCNTs-Al
2
O
3
hybrid particles have been harnessed to
enhance the tribological properties of pure epoxy, and
discussions have ensued regarding the optimal weight of
MWCNTs-Al
2
O
3
hybrid composites.
2 EXPERIMENTAL PART
2.1 Pure epoxy
In this study, the epoxy matrix used was Bisphenol
A. The initial constituent is denoted as the epoxy resin,
while the subsequent element is a curing agent, also
known as a hardener. The solidification process, facili-
tated by the curing agent, enables the formation of a
multidimensional cross-linked network within the epoxy
resin. The supplier of the epoxy was BottomUp Technol-
ogies, Bangalore, India. The density of the epoxy was
1300 kg/cm
3
. The tensile (70 MPa), flexural (110 MPa)
and compressive (380 MPa) strength of the epoxy were
used in this study. The glass transition temperature of the
epoxy was found to be 110 °C. Moreover, the water ab-
sorption of the epoxy was recorded to be 0.5 w/%.
2.2 Synthesis of CNT-alumina hybrid nanofillers
The synthesis of CNT-alumina hybrid nanofillers was
achieved through the chemical vapour deposition (CVD)
method. Utilizing Co(NO
3
)
2
·6H
2
O as the catalyst precur-
sor, carbon nanotubes (CNTs) were directly grown on
alumina nanoparticles. First, alumina nanoparticles with
an average size of 100–300 nm according to the manu-
facturer’s data, shown in Figure 1a, was cleaned and
prepared by treating it with a solution of HCl and rinsing
it with deionized water. A solution of Co(NO
3
)
2
·6H
2
O
was then deposited onto the alumina substrate. This is
typically done by dipping the substrate into the solution
and then drying it in air. The catalyst solution was for-
mulated by blending Co(NO
3
)
2
·6H
2
O and alumina in eth-
anol, subsequently subjecting it to sonication for a dura-
tion of 30 min. The resultant mixture was kept in an oven
at 100 °C for 12 h for drying. Then, the CVD process
was performed in a reaction chamber with the gas flow
consisting of a mixture of acetylene (C
2
H
2
), hydrogen
(H
2
) and argon (Ar), with a ratio of 2:5:8 and a flow rate
of about 1000 sccm. To facilitate the CNT growth, a dis-
tilled water bubbler was used. The reaction was per-
formed at 900 °C for a duration of 30 min. Composites
containing Co/alumina were synthesized, and the Co
content was varied from 1.0 to 5.0 w/% with increments
of 1.0 %.
The hybrid nanofillers synthesized from 1.0 w/% of
Co/alumina displayed a limited quantity of grown CNTs,
and these were uniformly distributed within the matrix.
RAMKUMAR R.: DRY SLIDING WEAR BEHAVIOUR OF CARBON NANOTUBE/ALUMINA/EPOXY HYBRID NANOCOMPOSITES
278 Materiali in tehnologije / Materials and technology 58 (2024) 3, 277–283

An increase in the Co/alumina ratio from 2.0 w/% to
3.0 w/% resulted in a significant growth of CNTs in the
alumina, which were also uniformly distributed in the
matrix. However, a ratio of 4.0 w/% to 5.0 w/% demon-
strated excessive growth of CNTs, forming bundles in
the alumina. The CNTs were wrapped around the alu-
mina particles due to the large quantity of CNTs grown
as a result of the increase in the Co/alumina ratio. The
grown CNTs had a diameter of about 50–100 nm and a
length of about 10–20 μm. The results suggest that a
higher concentration of the cobalt catalyst led to an in-
creased yield of carbon nanotubes as shown in Fig-
ure 1b.
2.3 Fabrication of epoxy-CNT-alumina hybrid nano-
composites
The CNT-alumina hybrid nanofillers were dispersed
into a solution of ethanol and water with a ratio of 5:3,
along with a dispersant agent of 1.5 % sodium hexa-
metaphosphate. The solution was then stirred using an
ultrasonicator at a frequency of 75 kHz for 30 min, after
which the sonication process was continued. Pure epoxy
was introduced into the solution, and a vigorous
sonication process was continued for another 20 min to
enhance the blending between the pure epoxy and
CNT-alumina hybrid nanofillers. Utilizing an ultra-
sonicator at a specific frequency during the dispersion
process can potentially enhance the homogeneity and
uniform distribution of CNT-alumina hybrid nanofillers
within the matrix. The curing agent was then added into
the solution with a ratio of 10:2, and the sonication pro-
cess was continued with uniform mixing of the curing
agent. The resultant solution was poured into an acrylic
mould measuring 10 mm in diameter and 60 mm in
length, as illustrated in Figure 2. Subsequently, the
mould was kept in a vacuum oven for2htoev acuate air
bubbles from the mixture, followed by maintaining it at
80 °C for 12 h. The mould was then cooled to room tem-
perature, and hybrid nanocomposite samples were
obtained. The weight ratio of the filler in the cured sam-
ples varied from 0.1 w/% to 0.5 w/% with an increment
of 0.1 %. Five samples with each weight ratio were pre-
pared.
2.4 Wear test
A pin-on-disc machine was employed to carry out a
dry-sliding wear test, using a Ducom TR20, following
the guidelines outlined in the ASTM standard G99. Low
(20 N), medium (40 N) and high (60 N) sliding loads
were applied, and the counterpart disc speed was set to
200 min
–1
. The experiment ran for a total of 30 min with
a sliding distance of 1000 m.
17
A wear test sample with a
pin sample size of 10 mm in diameter and 30 mm in
height was used. A 100Cr6 steel disc was used as the
counter-part material and, to ensure a uniform contact, a
fine emery sheet was employed to meticulously polish
the surface of the pin. The diameter of the wear track
RAMKUMAR R.: DRY SLIDING WEAR BEHAVIOUR OF CARBON NANOTUBE/ALUMINA/EPOXY HYBRID NANOCOMPOSITES
Materiali in tehnologije / Materials and technology 58 (2024) 3, 277–283 279
Figure 2: Wear specimens of: a) pure epoxy, b) 0.1, c) 0.2, d) 0.3,
e) 0.4, f) 0.5 weight fraction of MWCNTs-Al
2
O
3
hybrid nano-
composites
Figure 1: FESEM images of: a) alumina powder and b) CNT-alumina used in this experiment

was 50 mm. The software and hardware components of
the machine were utilized to configure the parameters re-
quired for the initialization, such as the disc speed, speci-
men load and duration of the experiment. The software
module supported the recording of the wear and friction
values. Prior to loading them into the machine, the sam-
ples were weighed using an electronic balance with a
precision of 0.1 mg. The wear loss was calculated based
on the initial and final weight of the samples; before and
after the test, acetone soaked soft paper was used to
clean the counterpart. The surface morphology of both
pure epoxy and hybrid nanocomposite worn surface were
scrutinized using a field emission microscope, providing
a deeper understanding of the wear phenomena.
3 RESULTS AND DISCUSSION
3.1 Tribological properties
The investigation into the tribological properties of
epoxy and hybrid nanocomposites, specifically multi-
walled carbon nanotubes (MWCNTs)/alumina, reinforc-
ing the epoxy, was conducted employing a pin-on-disc
machine. The pure epoxy exhibited average wear rates of
(0.06, 0.10 and 0.15) mm
3
/Nm under the low, medium
and high load, respectively. However, the additions of
0.1 w/% and 0.2 w/% of hybrid nanofillers into the epoxy
matrix considerably reduced the wear rate to (0.05, 0.07,
0.12 and 0.03, 0.05, 0.08) mm
3
/Nm, respectively, in low,
medium and high load conditions. Furthermore, the sig-
nificant reduction in the wear rate was observed to be
linked with the hybrid nanofiller content of 0.3 w/% in
the epoxy matrix and the wear values were (0.01, 0.02,
0.03) mm
3
/Nm under different loading conditions. This
result showed that the wear resistance was improved by
(83, 81 and 80) % in comparison with pure epoxy under
different loading conditions. Similarly, the addition of
0.4 w/% caused the wear rate to be lower than that of
pure epoxy and higher than that of 0.3 w/% hybrid
nanofiller composite. Furthermore, the increase in the
hybrid nanofiller content to 0.5 w/% caused the wear rate
to be the same as that of pure epoxy. The spatial network
structure within the epoxy resin, formed by MWCNT-
alumina, effectively dispersed the frictional heat gener-
ated at the interface, promptly hindering resin degrada-
tion and softening. Additionally, the optimized propor-
tion of hybrid nanofillers guaranteed a uniform and
efficient distribution within the pure epoxy. The optimal
weight percentage of the hybrid nanofillers played a sig-
nificant role in the formation of a high-quality friction
film, facilitating the transfer of friction. Furthermore, the
worn surface of the 0.3 w/% hybrid nanocomposite ex-
hibited punctate protrusions, suggesting an enhancement
in the shear strength of the pure epoxy and an effective
protection against material peeling during the friction
process, resulting in a reduction of the wear rate. An ex-
cessive incorporation of hybrid nanofillers into the epoxy
resulted in the formation of voids, compromising the ma-
terial’s structural integrity, mechanical properties and
overall performance within the host matrix, attributable
to the non-uniform distribution of the filler materials. In
Figures 3a to 3c, the specific wear rates of pure epoxy
and different weight fractions of the hybrid nanocom-
posites under the low, medium and high loads are graphi-
cally represented.
3.2 Morphology analysis of epoxy and hybrid nano-
composites
The surface morphology and internal wear mecha-
nism of pure epoxy and epoxy/MWCNTs-alumina hy-
brid nanocomposites were investigated (Figures 4 to 6).
The worn surface of pure epoxy exhibited hyperbolic
marking, pull-outs, deep grooves and fractures, indicat-
ing poor wear resistance and brittleness in low (20 N),
medium (40 N) and high (60 N) load conditions. The in-
troduction of 0.1 w/% to 0.5 w/% of MWCNTs-alumina
hybrid nanofillers into the epoxy considerably improved
the wear resistance of the host matrix. In low, medium
and high load conditions, a specimen’s worn surface ex-
hibited a petal surface, grooves, plastic deformation,
RAMKUMAR R.: DRY SLIDING WEAR BEHAVIOUR OF CARBON NANOTUBE/ALUMINA/EPOXY HYBRID NANOCOMPOSITES
280 Materiali in tehnologije / Materials and technology 58 (2024) 3, 277–283
Figure 3: Specific wear rate of pure epoxy and hybrid nanocom-
posites at: a) low-load (20 N) conditions, b) medium-load (40 N) con-
ditions, c) high-load (60 N) conditions

RAMKUMAR R.: DRY SLIDING WEAR BEHAVIOUR OF CARBON NANOTUBE/ALUMINA/EPOXY HYBRID NANOCOMPOSITES
Materiali in tehnologije / Materials and technology 58 (2024) 3, 277–283 281
Figure 4: Morphology analysis of a) pure epoxy, b) 0.1, c) 0.2, d) 0.3, e) 0.4, and f) 0.5 weight fraction of MWCNTs- alumina hybrid
nanocomposites during low (20 N) loading
Figure 5: Morphology analysis of a) pure epoxy, b) 0.1, c) 0.2, d) 0.3, e) 0.4, and f) 0.5 weight fraction of MWCNTs-alumina hybrid
nanocomposites during low (40 N) loading

delamination, matrix plugging and microcracks, respec-
tively. Plastic distortion on a worn surface indicates that
the sample is brittle in nature, thus easily subjected to
plastic deformation. Further addition of 0.3 w/% of hy-
brid nanofillers to pure epoxy significantly improved the
wear resistance, resulting in a worn surface with
microcracks, smoothness, tinny wear debris, and adhe-
sion delamination. A smooth surface was identified on
the sample, which was attributed to the large frictional
force developed on the worn surface due to the tangential
displacement due to continuous initiation and propaga-
tion of cracks that finally evolved into fatigue phenom-
ena. These were due to the accumulation of continuous
stress and destress of the worn surface, leading to the
brittleness of the material. Furthermore, it was observed
that the debris rolled between the worn surface and the
counterpart were pulverised into fine particles. The fine
particle occupied the microcracks on a worn surface,
providing long-run stability. Similarly, further additions
of 0.4w/% and 0.5w/% of hybrid nanofillers to pure ep-
oxy caused deep grooves, petal-surface layer deforma-
tion, wave-like fracture, the pit and cluster formation on
the surface.
4 CONCLUSIONS
In this research study, MWCNTs-alumina nanocom-
posites were fabricated using chemical vapour deposition
where carbon nanotubes were grown directly on alumina
particles. The hybrid nanofiller amount ranged from
0.1 w/% to 0.5 w/% with an increment of 0.1 w/%. The
primary accomplishments of this investigation can be
listed as follows:
• MWCNTs-Al
2
O
3
hybrid nanocomposites with (0.1,
0.2 and 0.3)w/% exhibit noteworthy advancements in
wear resistance. Particularly, the 0.3 w/%
MWCNTs-Al
2
O
3
hybrid nanocomposite demon-
strates exceptional wear resistance compared to pure
epoxy.
• The introduction of a low amount of the MWCNTs-
Al
2
O
3
hybrid nanocomposite results in a substantial
enhancement of the tribological performance of the
pure epoxy matrix.
• The incorporation of 0.3 w/% of MWCNTs-Al
2
O
3
hybrid nanocomposite results in significantly im-
proved wear resistance, with enhancements by (83,
81 and 80) % observed during low (20 N), moderate
(40 N) and high (60 N) loading, respectively, com-
pared to pure epoxy.
• The addition of 0.3 w/% of hybrid nanofillers into
pure epoxy significantly improves the wear resis-
tance, as evidenced by the presence of microcracks,
RAMKUMAR R.: DRY SLIDING WEAR BEHAVIOUR OF CARBON NANOTUBE/ALUMINA/EPOXY HYBRID NANOCOMPOSITES
282 Materiali in tehnologije / Materials and technology 58 (2024) 3, 277–283
Figure 6: Morphology analysis of a) pure epoxy, b) 0.1, c) 0.2, d) 0.3, e) 0.4, and f) 0.5 weight fraction of MWCNTs-alumina hybrid
nanocomposites during low (60 N) loading

smooth surface, tiny wear debris and adhesion
delamination on the worn surface, indicating en-
hanced material integrity and performance.
• The presence of deep grooves, petal-surface layer de-
formation, wave-like fractures, pits, and cluster for-
mations on the worn surfaces of epoxy composites
with 0.4 w/% and 0.5 w/% hybrid nanofillers indi-
cates increased wear and potential degradation, high-
lighting the importance of optimizing the nanofiller
amount for maintaining the material performance and
integrity under high load conditions.
• The presence of plastic deformation, delamination,
matrix plugging and microcracks on a worn surface
under various load conditions indicates a transition
from a brittle to a more plastic nature of the sample,
suggesting enhanced ductility and resistance to wear.
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