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Influence of carbon nanotubes on the Article reuse guidelines:
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properties of friction composite materials DOI: 10.1177/0021998319891772
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Emad F EL-kashif1, Shaimaa A Esmail1, Omayma AM Elkady2,

BS Azzam3 and Ali A Khattab1

Abstract
Carbon nanotubes have a lot of applications in mechanical fields. This is because nanomaterials have many superior
mechanical properties such as very high strength-to-weight ratio, high modulus-to-weight ratio, high corrosion resist-
ance, and super intelligence properties, which make them as smart materials. One of these attractive applications is the
use of carbon nanotubes in vehicle brake friction material. Therefore, the fabrication and testing processes of these
nanomaterials should be performed carefully to evaluate their mechanical, tribological, and noise properties. In this
paper, friction material mixed with carbon nanotubes have been fabricated with different carbon nanotube contents and
the same fabrication parameters. The carbon nanotubes have been produced using the conventional submerged arc
discharge technique. The produced friction materials have been cut into pieces with standard sizes and then tested
mechanically and tribologically. The results of tests have illustrated that the addition of carbon nanotubes into the friction
materials could improve their mechanical properties (hardness, strength, and modulus) and also could enhance their
tribological properties (wear rate and friction coefficient). Moreover, the tests showed that the presence of carbon
nanotubes in friction materials could reduce the noise, vibration of the friction materials, and reduce the temperature
rise due to the effect of friction, which means that the carbon nanotubes could raise the thermal conductivity of friction
material, while the friction coefficient has stayed within the allowable standard limits (0.35–0.45). Surface morphology
shows that the presence of carbon nanotubes in the friction materials could help to avoid surface friction cracks or fins
within the normal operating conditions. The good combination of mechanical and tribological properties was obtained at
0.5% carbon nanotubes.

Keywords
Automotive brake, carbon nanotubes, hot dry mold, composite friction materials, coefficient of friction, specific
wear rate

Introduction large volumes for the development of advanced

Current road safety regulations require the develop-
ment of new technical solutions for the main compo-
nents of the vehicle. Their technical performances
depend on the physical and mechanical characteristics
of the used materials which they were made from.1,2
Automotive brake friction materials have been devel-
oped to achieve safety regulations, such as stopping
distance under normal braking conditions and fade
resistance at high temperatures.3–5 In addition, various
experimental designs for commercial brake friction
materials have been also developed to improve the
wear resistance and to decrease the noise and vibration
raised during brake applications.6–12 During the last 10
years, carbon nanotubes (CNTs) have been produced in
friction materials. Small quantities of CNTs have sig-
nificant effects as it increases the nominal area of
contact, improves the mechanical properties, and
1
Department of Mechanical Design and Production, Faculty of
Engineering, Cairo University, Egypt
2
Powder Metallurgy Division, Manufacturing Department, Central
Metallurgical R&D Institute, Egypt
3
Department of Mechanical Engineering, College of Engineering, Taibah
University, Saudi Arabia
Corresponding author:
BS Azzam, Department of Mechanical Engineering, College of
Engineering, Taibah University, Madinah Monawarah, Saudi Arabia.
Email: Badr_azzam@yahoo.com
2 Journal of Composite Materials 0(0)
typically stabilizes the coefficient of friction and reduces
the wear rate.13
Lee et al.14 studied the effect of CNTs on the mech-
anical and tribological behavior of brake lining mater-
ials. Friction coefficient and wear behavior of the
samples, hardness, density, porosity were investigated.
They found that the open porosity of CNTs friction
specimens decreased with its content. Both the bulk
density and the hardness of CNTs containing brake
lining specimens increased with the CNTs content.
Apparent reduction in the wear rate and lower friction
coefficient were detected even though lower concentra-
tion of CNTs was adopted. Their scanning electron
microscopic (SEM) microstructure shows that increas-
ing the CNT content lead to smooth and adherent
lubricating film formation on the sliding surface
during wear tests, and accompanied with a lower m
and wear rate. Hwang et al.15 examined brake friction
materials containing multi-walled CNTs in amounts of
1.7, 4.7, and 8.5 wt%, to investigate their effect on the
braking performance. They found that the high tem-
perature friction stability increased with increasing the
amount of CNT added to the friction material. They
attributed this to the reinforcement of the composite by
CNTs and the larger strength at elevated temperatures
caused by CNTs. They added that increasing CNT con-
tent leads to lower coefficient of friction, which may be
due to the undispersed CNT bundles in the contact
surface. Finally they concluded that the damping cap-
acity of the friction material was improved by adding
CNTs due to the homogeneous distribution of CNT
bundles in the friction material, and CNTs increased
the wear resistance of the friction materials as a result
of the reinforcement effect.
The tribological, physical, and mechanical character-
istics have been chosen for differentiation and judgment
throughout the rationalized of the CNT percentage for
selecting the optimum composition and curing condi-
tions. The selection by sequential material addition has
been done on the light of the friction and wear tests.
Thus, a proposed composition and curing conditions to
produce a friction material can be nominated for auto-
motive disc brake applications.
Experimental procedures
The experimental work performed in this paper
includes the following stages: inspection and selection
of the chosen materials to formulate friction composite
samples with different ratios of CNTS, while the binder,
friction modifiers, reinforcing fibers, filling, and abra-
sive material ratios are kept constant; followed by siev-
ing of the powders to the required grain size and
hacking the fibers to definite length and mix them care-
fully; and finally fabrication of the formulated friction
composite samples using dry hot molding technique
and post baking processes at definite temperature and
limited period of time according to the material ingre-
dients and then the test processes of the proposed spe-
cimens have been tested according to known standards.
Four different samples have been prepared using
powder metallurgy technique with various filler mater-
ial (CNTs) percentages: 0.0, 0.5, 1 to 1.5 wt% partially
replaced the barium sulfate content, which was partially
5%. CNTs were produced by the electric arc-discharge
technique at about 60 A and 24 V. The resulted tube
average diameter was 7 nm with 90 nm length according
to SEM measurements. All samples were prepared
using powder metallurgy technique and its chemical
compositions are given in Table 1.
The resin includes 20% phenolic resin as reported by
many researchers.16,17 The fillers used are 25% calcium
carbonate (CaCO3) and 5% barium sulfate (BaSO4),
which were replaced partially by CNTs in amounts of
0.5, 1, and 1.5 wt%; the barite and CaCO3 were used in
such content as Handa and Kato18 recommended
because barite decreases the fade resistance but when
it is eliminated completely from the composite, the wear
rate increases. The friction modifiers (graphite, iron,
and rubber) were limited to 5% as recommended by
Cai et al.19 to achieve the optimization between mech-
anical and tribological properties. The abrasive mater-
ials (5% SiC and 5% Al2O3) were kept constant for all
samples according to Cai et al.19 who investigated the
effect of mullite (3Al2O3–2SiO2) content on the mech-
anical and tribological properties of friction materials
and they found that 10% mullite showed the best com-
pressive strength and good wear resistance compared to
other samples with either lower or higher content of
mullite. Reinforcement (rockwool fiber (RWF) and
steel fiber (25%)) was kept constant as well among all
samples according to Takamya et al.20 who recom-
mended the steel fibers to be in the range of 25–30%
as larger content of steel fibers increase the wear rate of
the disk.
Raw materials were blended together in a mixer for
10 min to get homogenous distribution of the ingredi-
ents.21 Molding of friction composite materials to pro-
duce friction composite samples of four different
chemical compositions; molding pressure, molding tem-
perature, and molding time were selected as manufac-
turing parameters where they have been kept fixed for
all samples to eliminate their effects on the physical,
mechanical, and tribological properties of friction
materials. The ingredients have been pressed in a hot
dry mold at 16 MPa on a compression testing machine
(Model WDW-300 universal testing machine). A hot
dry mold was fabricated from steel, and heated by
gas torch up to 150 C curing temperature. The tem-
perature has been measured by an infrared heat gun
EL-kashif et al.
Table 1. Chemical composition of friction samples, wt%.
Materials Base sample
Carbon nanotubes (wt%) 0 0.5
Binder (phenolic resin) (%) 20
Reinforcement ‘‘RWF’’ and ‘‘steel fiber’’ (%) 25
Fillers (%) 30
Friction modifiers (%) 15
Abrasive1 (SiC) (%) 5 5
Abrasive2 (Al2O3) (%) 5 5
for the time duration of 1 min per each mm thickness of
the proposed specimens.22 The manufactured speci-
mens have been cut into specimens of square cross sec-
tion of 40 mm  40 mm and 10 mm thickness, as shown
in Figure 1. Post curing was then carried out in an oven
at 150 C for 60 min to relieve the residual stress induced
in the samples due to the curing process and to com-
plete the chemical reactions in the friction material
specimens.
Characterizations
Density of brake pad materials
The density or specific gravity has been measured using
a specific gravity meter, which depends upon the ingre-
dients of the brake material formulation. The true dens-
ity of the specimen was determined by weighing the
specimen on a digital electronic balance. The measured
volume of the sample was 40 mm  40 mm  10 mm.
The specific gravity has been determined as follows
mass, ðmÞ
Specific gravity or density :  ¼ g=cm3 ð1Þ
volume, ðvÞ
Mechanical properties
Surface hardness measurement. Surface hardness of the
specimen has been measured using a Rockwell hardness
tester model HBRVU-187.5. The hardness measure-
ments were performed on uniformly surface of the spe-
cimen. These measurements include three different
positions of each specimen and the average was taken
as the HRc scale.
Compression strength. A compression test procedure has
been applied on the composite friction material samples
where the cross section of the samples was
10 mm  10 mm.
3
Sample #1 Sample #2 Sample #3
1 1.5
20 20 20
25 25 25
29.5 29 28.5
15 15 15
5 5
5 5
Figure 1. Fabricated friction specimen.
Test procedures for tribological evaluation
Tribological test to get the friction coefficient and spe-
cific wear rate of the friction samples has been per-
formed on the ‘‘pin-on-disk’’ tester machine according
to standard test SAE-J661.23,24 The machine frictional
disc is a typical automobile brake disc (made of alloyed
grey cast iron). Figure 2 shows a scheme for pin-on-disc
testing machine with its diagnostic instrumentation
system to detect the specimen friction force and disc
rotation speed, bulk temperature of the disc rotor,
and system friction noise level. A sound level meter
(SLM) model 2240 of impulsive detection type has
been located in the near-field region to detect the fric-
tion system noise.
Coefficient of friction. The friction coefficient of the pro-
posed friction materials is related to the testing time
and testing conditions, which has been performed at
50 N friction force and 7 m/s sliding speed of the disc.
Specific wear rate measurements. Specific wear rate ‘‘aver-
age’’ test was carried out on the ‘‘pin-on-disk’’ machine
to determine the loss in sample mass as a measure of
wear over time depending on the whole tribological
system. Tribo-systems always consist of the following
components: the sample composite material, a counter-
part, a medium in between rubbing as lubricant or
abrasive, the environment, and also normal pressure
4 Journal of Composite Materials 0(0)

1
2

8
3

4
10 7
6

1. Test rig frame 2.Electric motor 3. Brake disc

4. Friction specimen 5. Press arm 6.Forcetransducer
7. Oscilloscope 8. PC 9. Sound level meter
10. Digital tachometer

Figure 2. Arrangement of the pin-on-disc tester and its diagnostic instrumentation system.

and sliding speed over a certain period of time. Specific

wear rate could be determined from equation (2) as Table 2. Testing conditions of friction coefficient, wear rate,
follows and sound level.

Background noise 77 dB Test duration 18 min

W
Specific wear rate ðSWRÞ ¼ cm3 =N  m
  V  T  Ff Sliding speed 7 m/s Ambient 20 C
ð2Þ temperature
Friction pressure 0.5 MPa Microphone 200 mm
where W is the weight difference (g), Ff is the friction distance
force (N), T is the test duration (s), r is the density Sample area 10 mm  10 mm Sound filter A
(g/cm3), and V is the sliding speed (m/s).
The applied load (50 N) was constant over all the
tests done, and no various loads were used. The friction
coefficient, the specific wear rate, and sound level test- Table 3. Chemical composition of the cast iron disc.
ing conditions are given in Table 2. Sound filter A was
C% Mn % Si % S% Ni % Cr % Mo %
used to permit the broad band sound level only and
cause attenuation for the other levels. 3.3–3.5 0.6–0.9 1.8–2.1 0.12 0.6–0.7 0.15–0.25 0.2–0.3
Low wear rates indicate high wear resistance of the
material and the small values of ‘‘wear rate’’ are desir-
able for the manufacturing operation. The tribological and detection environment conditions, respectively.
tests have been, generally, used for the quick evaluation The sound level meter should be calibrated after each
of automotive brake friction materials according to ES. test using its build in calibrating system. The measured
No 2006/1981. noise level is broad band level.
The chemical composition of the used friction disc is The friction system exposed noise level has been dis-
given in Table 3 and it was made from alloyed grey cast crete carried out for full test period of 18 continuous
iron to simulate the actual operating conditions of most minutes of the pin-on-disc tester operation. The brake
vehicles. frictional dynamic behavior and its generated noise
levels are used to evaluate the brake frictional materials
Friction noise evaluation. The resolution of sound waves performance quality and their response variations due
has been resolute according to Filter A, while the gen- to defects of long period usage or inventory for auto-
eral microphone type on the used sound level meter lays motive applications.
200 mm far away from the friction contact area for
near-field measurements to avoid any effective interfer- Composite friction material surface morphology. The surface
ence of other external sound sources. Figure 2 and morphology of the friction composite material samples
Table 3 illustrate the sound meter microphone location was analyzed using optical microscope and SEM was
EL-kashif et al.
Table 4. Physical, mechanical, and tribological characteristics of the tested friction composite materials.
Materials Base sample
Carbon nanotubes (wt%) 0 0.5%
Density (g/cm3) 2.384
Compressive strength,  comp (MPa) 72.14
Averaged stiffness (kN/mm) 27.4
Hardness, HRc 32.5
Min. friction coefficient 0.38
Max. friction coefficient 0.47
Specific wear rate, SWR (cm3/Nm) 3.44E-8
Average level sound response (dB(A)) 81.1
performed with a JXA-840A JEOL electron probe
micro analyzer type. The sample surfaces for SEM
observations were coated with gold to facilitate the
characterization of the friction layer.
Results and discussion
Effect of carbon nanotubes on properties of friction
material
Overview of the comparison test results. The test results of
all composites brake pads samples are shown in
Table 4. Test results were taken as the average of
four tested samples. The samples are named according
to the CNTs content; base sample has 0% CNTs, while
sample #1, sample #2, and sample #3 have 0.5, 1, and
1.5% CNTs, respectively.
Composite material density. Density of the tested friction
specimens is given in Figure 3.The density results
showed that it increases slightly by increasing CNTs
content and sample #3 (1.5% CNTs) shows the highest
density of 2.437 g/cm3, which may be due the increased
nominal area of contact and as result the porosity is
decreased and this result are in good agreement with
other results obtained by other researchers.13–15 To cal-
culate the theoretical density, the samples have to be a
close-packed system without any holes or pores; how-
ever, the samples of this study have many porosity that
will give large deviation between the theoretical and
actual densities and that is the reason for not calculat-
ing the theoretical densities.
Material hardness. The results obtained of surface hard-
ness shown in Figure 4 illustrates that the hardness of
friction materials increased by the addition of CNTs
gradually, where the large hardness is preferred for
the manufacturing operation and for better wear resist-
ance. Sample #3 (1.5% CNTs) has the largest hardness
50.1 HRC, while the base sample show lower hardness
5
Sample #1 Sample #2 Sample #3
1% 1.5%
2.385 2.387 2.437
169.37 115.61 94.51
48.58 28.58 32.7
42.8 48.3 50.1
0.41 0.35 0.36
0.46 0.43 0.43
1.25E-8 1.19E-8 1.1E-8
78.12 79.8 81.1
32.5HRC and as a result the hardness is directly pro-
portional to CNT content, which may be due the
reinforcement and meshing action induced by CNTs.
Stiffness of the material. The stress–strain relationship is
given in Figure 5, which can help in determining the
specimen material stiffness and compressive strength.
The results of stress–strain for the tested specimens
show the following: sample #2 with 1 wt% CNTs regis-
tered an effective strain of about 32% to reach its max-
imum stress of about 115.6 MPa and achieved the
lowest stiffness compared to the other samples; while
sample #1 with 0.5 wt% CNTs registered the largest
stiffness and the highest compressive strength relative
to others. This imply that 0.5 wt% CNTs sample gives
the optimum strength and stiffness, which is corres-
ponding to the optimum CNTs lubricant layers
formed at the surface and inside the composite as fur-
ther increase in the CNT content has an adverse effect
on strength and stiffness. This imply that (0.5% CNTs)
is the optimum CNT content for the compressive
strength and stiffness and further increase in the CNT
content shows a decrease in both strength and stiffness.
Compression strength. Compression strength results of
the tested specimens are given in Figure 6. Analysis of
these results show the following.
The compressive properties of the friction materials
have increased for the first specimen of 0.5 wt% CNTs
and then have decreased with increasing CNT ratios.
Sample #3 (1.5 wt% CNTs) shows the minimum com-
pressive strength, but higher than the base sample due
to the lubricant layers in case of CNT addition.
Lee et al.14 studied the effect of CNTs on the mech-
anical and tribological behavior of brake lining mater-
ials and they found that both the bulk density and the
hardness of specimens increased with the CNTs con-
tent. Apparent reduction in the wear rate and the m
was detected even though low concentration of CNTs
was adopted. As the concentration of catalyst
6 Journal of Composite Materials 0(0)
Figure 3. Variation of material densities for different CNTs ratios.
Figure 4. The surface hardness measurements of friction specimens.
increased, CNTs containing brake lining specimens
exhibited the lower wear rate and m. They added that
SEM microstructure indicated smooth and adherent
lubricating film formation on the sliding surface
during wear tests and the film thickness increases by
increasing CNTs content, and accompanied with a
lower m and wear rate.
Hwang et al.15 examined brake friction materials
containing multi-walled CNTs in amounts of 1.7, 4.7,
and 8.5 wt% and investigated their effect on the braking
performance. They found that the high temperature
friction stability increased with increasing the CNT
content and they attributed that to the reinforcement
of the composite by CNTs and the larger strength at
elevated temperatures caused by CNTs; increasing
CNT content leads to lower friction coefficient, which
may be due to the undispersed CNT bundles in contact
surface; the damping capacity of the friction material
was improved by adding CNTs due to the homoge-
neous distribution of CNT bundles in the friction
material; CNTs increased the wear resistance of the
friction materials as a result of the reinforcement effect.
Tribological properties
Specific wear rate. Evaluation of the test specimen’s fric-
tion wear rates is presented in Figure 7.
The specific wear rates for all samples show that
samples 2 and 3 have minimum wear rates. This is
because both samples illustrate high surface hardness.
The wear rate decrease as the CNT ratio increases. This
may be because CNTs act as a solid lubricant, which
decreases the wear rate of samples. The specific wear
rate results during test period are within the allowable
standard value limits (2E-8 to 8E-7 cm3/Nm).25,26 This
means that these samples may possess long life service,
EL-kashif et al. 7

180
Base Sample
160 0.5 CNT
1 CNT
140
1.5 CNT
120

Stress / MPa
100

80

60

40

20

0
0 10 20 30 40 50
Strain / %

Figure 5. Stress–strain curves for test specimens.

Figure 6. Compressive strength for all samples.

Figure 7. Effect of CNTs ratios on the specific wear rates of the tested specimens.
8 Journal of Composite Materials 0(0)
Figure 8. Variation of friction coefficient with test duration.
Figure 9. Friction temperature gain for tested specimens.
whereas the base sample with 0 wt% CNTs showed the
maximum wear rate, which imply that base sample may
fail in shorter service life.
Friction coefficient variations. From the results of friction
coefficient shown in Figure 8, it can be shown that the
friction coefficient has a nearly stable level for all the
tested specimens and all samples reach to friction coef-
ficient m ¼ 0.44 after about 6 min from the test begin-
ning. This period represents the running-in-period of
the friction couple surfaces and evaporation of mois-
ture content. Sample #1 with 0.5 wt% CNT has the
most stable friction coefficient ranging from 0.41 to
0.46 during the period of test. This may due to that
the CNTs can enhance the mechanical meshing
force,13 thus improving the friction coefficient, where
all samples set in an allowable standard coefficient
value in the automotive (0.35–0.45).25,26 All friction
tests have been finished without any fading signal
response of the samples.
Friction temperature gain. The recorded friction specimen
mass temperature has been presented in Figure 9 for all
tested samples. Analysis of the obtained results show
that the maximum temperature gained due to friction in
the time domain is achieved for base sample, while the
lowest temperature gain is presented for sample #3
(1.5 wt% CNTs). Sample #1 with 0.5 wt% CNTs and
sample #2 with 1 wt% CNTs show good heat dissipa-
tion and low temperature gain during the test. In brake
lining materials, the increase in CNTs shows lower tem-
perature gain due to the low thermal conductivity of
CNTs and due to the modification of the friction layers,
which improves the high temperature friction
stability.14
Friction noise level. The generated levels of the tested spe-
cimens’ noise are given in Figure 10. The resolutions of
the obtained noise levels indicate that the highest dur-
able noise level was obtained for sample #3 (1.5 wt%
CNTs), which showed the maximum hardness level.
While the lowest and the most stable sound level was
observed for sample #1 (0.5 wt% CNTs), which has a
EL-kashif et al. 9

Figure 10. Response of friction noise level for tested samples.

Figure 11. Surface morphology of sample #3 after friction test.

Figure 12. Optical microstructure for all samples.

10
relative lower hardness. On the other hand, sample #2
showed a decreasing sound level with time after 4 min
of test period.
Surface morphology of the friction specimens. The surface
morphology of the friction composite material samples
has been observed using SEM for sample #3 with
1.5 wt% CNTs after friction test, as shown in
Figure 11. These worn surfaces were obtained after
pin-on-disk test and different features are shown as fric-
tion layer and CNTs bundles.
The given general scope of the surface morphology
shows that the surface continues without cracks to
ensure that the resin ratio is enough with no specific
material accumulations, which ensures homogenous
mixing of the composite material in the sample. It can
be shown that there are no large particles in the com-
posite surface to concentrate the friction stress and heat
dramatically. Moreover, there are separated material
layers with carbon area, which can be seen dark black
of the CNTs. As a final conclusion, the surface
morphology gives a good sight on composite materials
mixing quality.
The optical microstructure showed a homogenous
distribution of different material constituents, which
are pointed by arrows and there is no agglomeration
of certain constituent as shown in Figure 12.
Conclusions
The mechanical, friction, and wear properties of a pro-
posed friction material reinforced by different ratios of
CNTs were examined in this study, and the following
conclusions can be drawn:
1. The coefficient of friction decreased with increasing
CNT content due to the undispersed CNT bundles
on the contact surface.
2. The noise raised from the material decreased and its
damping capacity increased with larger content of
CNTs.
3. CNTs improved the wear resistance of the friction
material.
4. The addition of CNTs improved the density, hard-
ness, and stiffness of the friction material.
5. The surface morphology has been enhanced by
adding CNTs into it where CNTs could help to
avoid surface friction cracks or fins within the
normal operating conditions.
6. The sound level of the friction operation has
decreased by increasing the CNTs where CNTs
could increase the damping capacity of friction
materials.
7. Moreover, the friction specimens with up to 1.5 wt%
CNT ratio showed a stable friction coefficient
Journal of Composite Materials 0(0)
between 0.35 and 0.45 for surface hardness more
than 50 HRc at low level of material specific wear
rate. This helps to prolong the service life of friction
materials.
Declaration of Conflicting Interests
The author(s) declared no potential conflicts of interest with
respect to the research, authorship, and/or publication of this
article.
Funding
The author(s) received no financial support for the research,
authorship, and/or publication of this article.
ORCID iD
BS Azzam https://orcid.org/0000-0001-8964-351X
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