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Lubricating and physico-chemical properties of CI- 4 plus engine oil

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DOI: 10.1080/17515831.2018.1452847

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 Tribology - Materials, Surfaces & Interfaces

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Lubricating and physico-chemical properties of CI-

4 plus engine oil dispersed with surface modified
multi-walled carbon nanotubes

V. Srinivas, Ch. Kodanda Rama Rao & N. Mohan Rao

To cite this article: V. Srinivas, Ch. Kodanda Rama Rao & N. Mohan Rao (2018):
Lubricating and physico-chemical properties of CI- 4 plus engine oil dispersed with surface
modified multi-walled carbon nanotubes, Tribology - Materials, Surfaces & Interfaces, DOI:
10.1080/17515831.2018.1452847

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Tribology – Materials, Surfaces & Interfaces, 2018
https://doi.org/10.1080/17515831.2018.1452847

Lubricating and physico-chemical properties of CI- 4 plus engine oil dispersed

with surface modified multi-walled carbon nanotubes
V. Srinivasa, Ch. Kodanda Rama Raoa and N. Mohan Raob
a
Department of Mechanical Engineering, GITAM, Visakhapatnam, India; bDepartment of Mechanical Engineering, University College of
Engineering, JNTU, Kakinada, India

ABSTRACT ARTICLE HISTORY

This paper studies the effect of surface modification of multiwall carbon nanotubes (MWCNTs) Received 15 April 2017
prior to dispersion in engine oil to improve the tribological properties. The MWCNTs are stabilised Accepted 10 March 2018
in the lubricant with two different surfactants cetrimonium bromide (CTAB) and sorbitan
KEYWORDS
monooleate (SPAN 80) and the effect of surfactants on the tribological properties has been Multi walled carbon
studied. Pristine and surface modified MWCNTs in weight per cent range of 0·5% are dispersed in nanotubes; surface
CI4 plus diesel engine oil. The foaming tendency and other physico-chemical properties of test modification; wear scar;
lubricant have been studied to investigate the effect of nano materials and surfactants. The anti- friction coefficient; extreme
wear and anti-friction properties are tested on a four ball wear tester and the comparison is made pressure tests; weld load
to assess the relative performance of pristine MWCNTs over surface modified MWCNTs. A strong
influence of the surface modification technique is found on lubricating and physico-chemical
properties. Both CTAB and SPAN 80 could keep the MWCNTs stable in the lubricant without
compromising the foaming tendency of lubricant and other physico-chemical properties. The
friction and wear characteristics of lubricants have improved with the  dispersion of surface
modified MWCNTs while there is no improvement in the properties of lubricant dispersed with
pristine MWCNTs.

Introduction density and the electron mobility. Lubricants dispersed

with allotropes of carbon are being extensively studied
Diesel engine oils used in industries and automotive
[8–13,15–21] for their self-lubricating properties and
engines are often subjected to heavy loads due to which
lower friction coefficients thereby improving anti-wear
they experience high temperatures and pressures caus-
properties. It is also reported in the literature that the
ing higher friction and surface damage leading to failure
carbon allotropes need to be surface modified to pre-
of the system. To prevent failure, conventional lubricat-
vent agglomeration and settling down in the lubricant
ing oils are dispersed with extreme pressure (EP) and
medium. This paper aims at investigating improvement
anti-wear (AW) additives that react chemically with
in anti-wear, anti-friction and extreme pressure proper-
the metal surfaces, forming easily sheared layers and
ties of formulated CI 4 grade engine oil dispersed with
thereby preventing severe wear and seizure. Detergents,
surface modified CNTs. The effect of MWCNTs, as well
dispersants, anti-acids, friction modifiers and viscosity
as surface modification technique on the tribological
modifiers are always included in motor oils as additives.
properties, has been studied. A simpler surface modifi-
The role of these additives is to keep metal surfaces
cation technique to stabilise the MWCNTs is employed.
clean, make the oil carry particle impurities, neutralise
The effect of additives along with surface modified
the acids produced in the engine, maintain the viscosity
MWCNTs has resulted in the use of lesser amount of
across the broadest range of temperatures and condi-
MWCNTs in the lubricant dispersion compared to stud-
tions and improve the oil’s anti-friction and anti-wear
ies reported in the literature.
properties under high-pressure conditions. Engine oils
dispersed with nanomaterials are investigated for tri-
bological property enhancement by several researchers Experimental procedure
[1–21]. Allotropes of carbon such as graphite, fullerenes, Materials and characterisation
carbon nanotubes and graphene, have caused interest in
the researchers due to their special properties. Although In the present study, multi walled carbon nanotubes
constituted of the same element, the properties of the produced by CVD method have been procured from
carbonaceous nanomaterials are very different from Cheaptubes Inc., U.S.A. The size of MWCNTs is
such material on the macro scale due to the electron 20–40 nm diameters, 10 microns length and about 95%

CONTACT  V. Srinivas  vsvas1973@yahoo.com

© 2018 Institute of Materials, Minerals and Mining and Informa UK Limited, trading as Taylor & Francis Group
2   V. SRINIVAS ET AL.
purity. The MWCNTs are characterised using HRSEM to
verify the size and shape as shown in Figure 1. All other
chemicals purchased are of GR grade. The surfactants
are AR grade procured from M/s Sigma Aldrich India
Pvt. limited.
Base lubricant and preparation of lubricant
samples
CI 4 plus grade car engine oil is selected as the base
lubricant and multiwall carbon nanotubes in 0·5 weight
per cent is dispersed in base lubricant to prepare the
nano lubricant samples. The composition of base lubri-
cant is estimated by Inductively Coupled Plasma Atomic
Emission Spectrometry (ASTM D 5185) is given in Table
1.
Surface modification of MWCNTs
As the MWCNTs tend to agglomerate and form large
particles clusters, it is required to modify the surface
of MWCNTS with a surfactant to create stearic repul-
sions between individual nanotubes. To stabilise the
nano particles in the liquid medium, two kinds of sur-
factants: SPAN 80 and Cetrimonium bromide (CTAB)
are used to modify the surface of MWCNTs during the
preparation of oil. Span80 is a nonionic surfactant with
a hydrophilic-lipophilic balance of 4·6 which is ide-
ally suitable for oils. Cetrimonium bromide (CTAB) is
a quaternary ammonium nonionic surfactant. It adsorbs
on the surface of nanoparticles reducing their surface
energy thereby preventing aggregation and settling of
nanoparticles.
During the process of surface modification, sur-
factant and nanoparticles in the ratio of 2:1 are taken and
mixed in a solvent isooctane. The mixture is ultrasoni-
cated for 30 minutes and due to an ultrasonic -chemical
reaction, the surface of the MWCNTs is coated with the
surfactant. The surface modified CNTs are characterised
by functional groups on the surface using Fourier trans-
forms infrared spectroscopy as shown in Figures 2–4.
Figure 1. HRSEM Image of multi walled carbon nano tubes.
Figure 2 shows pristine MWCNTs with no characteristic
peak detected. Figures 3 & 4 show MWCNTs surface
modified with SPAN 80 and CTAB, respectively, with
lipophilic groups detected in the wavelength band of
1400–1500 cm−1. 
The surface modified MWCNTs in 0·5 weight per
cent is dispersed lubricating oil and sonicated using an
ultra-sonic probe for about 40 min. The stability of the
nanofluid for a period of 30 days is monitored by visual
observations. The stability of test oils immediately after
preparation and after one month in terms of settling is
shown in the Figure 5. From Figure 5 it can be seen that
lubricant dispersed with pristine MWCNTs has layers of
separation while the surface modified MWCNTs could
remain stable in the solution.
Effect of surface modification on physico-chemical
properties
The lubricants oils are formulated by blending base
stocks and additive components to meet the require-
ments of standards. Compliance to physicochemical
properties as envisaged in standards is not only a man-
datory requirement for statutory purpose rather it is
directly related to the optimum performance of engine
crankcase /gears and other associated parts. It is of vital
significance to ensure that there is no change in phys-
icochemical properties beyond limiting values (Min or
maximum as the case may be) when lubricants are dis-
persed with nanoparticles. Most important properties
to be taken into consideration are foaming tendency,
viscosity index and pour point. In the present study apart
from tribological properties, the effect of surface modifi-
cation on physico-chemical properties is also evaluated.
All the properties are evaluated in 5 replicable experi-
ments and the average values are reported.
Effect of surface modification on foaming
tendency of oil
Engine and gears oils contain foaming additives to keep
the engine parts clean. However, excessive foam in the
engine and gears result in loss of lubrication and even-
tually mechanical failure of the components. Surfactants
used for surface modification of nanomaterials often
generate foam under high temperature conditions and
hence tend to be deleterious.
The foaming tendency of the lubricant samples is
tested as per ASTM D 892 method and the test is done in
two sequences. In sequence one, the sample maintained
at a temperature of 24°C is blown with air at a constant
rate of 95 mL/min for 5 min and then allowed to settle
for 10 min. The volume of foam is measured at the end of
both periods. In sequence two, the test is repeated on the
sample at 93·5°C. The generated foam volume in both
the sequences is reported and care is taken in optimising
the amount of surfactant to prevent excessive foaming of
 TRIBOLOGY – MATERIALS, SURFACES & INTERFACES   3

Table 1. Elemental analysis of base lubricant. Multiwalled carbon nanotubes has been limited to 2:1
Elements Quantity by optimisation from foam test.
Calcium (mg/Kg) 9·5
Zinc (mg/Kg) 10·2
Phosphorous (mg/Kg) 157 Effect of surface modification on viscosity index
Sulphur (Wt%) 2·14
Kinematic viscosity and viscosity index are the measure
of lubricating oil performance at elevated temperatures.
nanomaterials dispersed lubricants in comparison with The effect of surface modification and dispersion of car-
base lubricant stock. bon nanotubes on the viscosity index are evaluated as per
From the Table 2, it can be observed that the surface ASTM D2270 to predict the oil behaviour at higher tem-
modification of MWCNTs with surfactant in the ratio peratures. The results are tabulated as given in Table 3.
2:1 has little effect. With a surfactant ratio of 3:1 there is As can be observed from the table, as the ratio of sur-
considerable foam generated in both blowing periods as factant to nanomaterials increases beyond 2:1, there is a
well as settling period. Thus the amount of surfactant to sharp decrease in the viscosity index due to thinning of
the oil at elevated temperatures by surfactant molecules.

Figure 2. FTIR analysis of Pristine MWCNTs.

Figure 3. FTIR analysis of MWCNTs surface modified by SPAN 80.

4   V. SRINIVAS ET AL.

Figure 4. FTIR analysis of MWCNTs surface modified by CTAB.

Figure 5. Stability of CI 4 grade oils (A) after preparation (B) after 1 month.

Table 2. Results of foaming tendency test (ASTM D 892).

Foam volume (ml)
Sequence I at 24oC Sequence II at 93·5oC
Ratio of Surfactant to At the end of 5 min At the end of 10 min At the end of 5 min At the end of 10 min
Test oil MWCNTs blowing period settling period blowing period settling period
Base oil (CI 4 Engine oil) 0 5 Nil 30 Nil
Base oil + 0·5% Pristine 0 5 Nil 30 Nil
MWCNTs
Base oil + 0·5% modified 2:1 6 Nil 32 Nil
MWCNTs (SPAN 80)
Base oil + 0·5% modified 3:1 12 5 52 14
MWCNTs (SPAN 80)
Base oil + 0·5% modified 2:1 8 Nil 35 Nil
MWCNTs (CTAB)
Base oil + 0·5% modified 3:1 15 8 52 12
MWCNTs (CTAB)

Effect of surface modification on pour point of oil temperature performance while the decrease in pour
point below rated value will inhibit lubrication perfor-
Pour point is a measure of lubricant performance at
mance. The pour point of the test oil is measured as per
lower temperatures. Any increase in the pour point
ASTM D97 and tabulated in Table 4
will increase the viscosity index hindering the high
 TRIBOLOGY – MATERIALS, SURFACES & INTERFACES   5

From the table it can be seen that up to optimum
surfactant to MWCNTs ratio of 2: 1 the pour point value
of nanofluid matches the value of base lubricant and
beyond optimum value, there is a slight decrease in the
rated pour point indicating the dependence of pour
point on surfactant.
indicates incipient seizure characterised by a sharp rise
in the frictional torque. This is called seizure load which
is an important factor in determining the effectiveness
of the lubricant. All the tests are conducted in ten sets
to ascertain the influence of nano particles in terms of
repeatable and reproducible results.

Tests for tribological properties Results and analysis

The lubricants prepared along with base lubricants are The results of wear test conducted as per ASTM D4172
tested for tribological properties on a 4 ball tester. The and friction test conducted as per ASTM D 5183 are as
weight percentage of MWCNTs is maintained as 0·5 Wt given below for different test oils (Tables 5 and 6).
%. In case of lubricants dispersed with surface modi- The 10 sets of results of repeatable wear and fric-
fied MWCNTs, the ratio of surfactant to MWCNTs is tion characteristics are plotted over the average line in
maintained as 2:1. The general principle of the test is the graph shown in Figure 6. There is an insignificant
a rotating steel ball is pressed against three steel balls change in the friction coefficient and wear scar diame-
firmly held together and immersed in lubricant. The test ter with the dispersion of pristine MWCNTs. However,
load, duration, temperature and rotational speed are set surface modified MWCNTs could improve the friction
in accordance with the standard test schedule. In anti- and wear properties profoundly. The detailed analysis
wear performance test done as per ASTM D 4172, the of the results shows that the surface modified multi
average scar diameter on the bottom three balls shows walled carbon nanotubes besides being stable in lubri-
the ability of the lubricant to prevent wear. A larger cant could significantly improve the tribological prop-
diameter indicates poor anti-wear performance while erties of the base oil. With the dispersion of surface
a smaller indicates superior wear preventive property. modified MWCNTs, the wear scar diameter and fric-
The conditions of wear test are as follows tion coefficient have decreased significantly indicating
Temperature of oil: 75 ± 2°C Speed of rotation: 1200
RPM
Table 4. Pour point of engine oils.
Duration: 1 hour (for wear in) Load applied: 40 kgf
Test oil (CI 4 Engine oil Ratio of Surfactant to
The friction test is carried out to find the friction coeffi- base) MWCNTs Pour point, °C
cient offered by the lubricant as per ASTM D 5183 code. Base oil 0 −25
Base oil + 0·5% Pristine 0 −25
The conditions wear in for friction test is as follows MWCNTs
Temperature of oil: 75 ± 2°C Speed of rotation: 600 RPM Base oil + 0·5% modified 2:1 −25
MWCNTs (SPAN 80)
Base oil + 0·5% modified 3:1 −28
Duration: 1 hour (for wear in) Load applied: 40 kgf. MWCNTs (SPAN 80)
Base oil + 0·5% modified 4:1 −30
After wear in, the used lubricating oil is discarded and MWCNTs (SPAN 80)
balls are cleaned. Fresh lubricant sample is taken in the Base oil + 0·5% modified 2:1 −25
ball cup with the same worn test balls in place. The test MWCNTs (CTAB)
Base oil + 0·5% modified 3:1 −29
is again started under the above conditions with the load MWCNTs (CTAB)
varying from an initial load 10 kgf and increased by 10 Base oil + 0·5% modified 4:1 −30
MWCNTs (CTAB)
kgf at the end of each successive 10 min interval up to
the point where the Frictional Torque – Time graph

Table 5. Wear test results of test oils at 40 kgf load.

Table 3. Viscosity index values of test lubricants (ASTM D2270).
Oil Wear scar in μm
Test oil (CI 4 Engine oil Ratio of Surfactant to
base) MWCNTs Viscosity index Base oil 380·22
Base oil + 0·5% Pristine MWCNTs 372·42
Base oil 0 122 Base oil + 0·5% MWCNTs modified with SPAN 80 348·24
Base oil + 0·5% Pristine 0 121 Base oil + 0·5% MWCNTs modified with CTAB 350·28
MWCNTs
Base oil + 0·5% modified 2:1 121
MWCNTs (SPAN 80)
Base oil + 0·5% modified 3:1 110 Table 6. Friction test results of test oils.
MWCNTs (SPAN 80)
Base oil + 0·5% modified 4:1 85 Oil Seizure load, kgf Coefficient of friction
MWCNTs (SPAN 80) Base oil 120 0·0911
Base oil + 0·5% modified 2:1 121 Base oil + 0·5% Pristine 110 0·0922
MWCNTs (CTAB) MWCNTs
Base oil + 0·5% modified 3:1 110 Base oil + 0·5% MWCNTs 140 0·0759
MWCNTs (CTAB) modified with SPAN 80
Base oil + 0·5% modified 4:1 88 Base oil + 0·5% MWCNTs 130 0·0766
MWCNTs (CTAB) modified with CTAB
6   V. SRINIVAS ET AL.

Figure 6. Trends of repeated experimental results of test oils (a) wear scar diameter and (b) friction coefficient.

Figure 7. Variation of friction torque with time during friction test.

the effectiveness of surface modification. Figure 7 shows
the variation of friction torque with time during fric-
tion test for the case of base oil and oil dispersed with
pristine MWCNTs. From the graph, it can be observed
that dispersion of pristine MWCNTs could reduce the
frictional torque at lower loads below 60 kgf. Beyond
60 kgf load, there is an increase in the frictional torque
thereby decreasing the seizure load and increasing the
friction coefficient at the end of the test. This shows
that pristine MWCNTs due to their poor dispersion in

Figure 8. Variation of friction torque with time during friction test.
lubricant could not improve the anti-friction proper-
ties at higher loads thereby no significant improvement
in overall friction coefficient is observed. This could be
due to rapid agglomeration of MWCNTs at higher loads
due to lack of surface modification. Figure 8 plots the
frictional behaviour of base oil and oil dispersed with
surface modified MWCNTs. It can be seen that there is
a reduction in the frictional torque of nano lubricants
with a very significant decrease at higher loads indicat-
ing the effectiveness of surface modified nanomaterials
at higher loads. Moreover, with the dispersion of surface
modified MWCNTs, an improvement in seizure load
during friction test can also be found.
Conclusions
(1) The surface modification of multi walled carbon
tubes plays an important role in the improve-
ment of anti-wear and anti-friction properties
of engine oils.
(2) The surface modification of MWCNTs could
make them stable in the lubricant without com-
promising the foaming tendency.
(3) The viscosity index is strongly dependent upon
the surfactant to nanomaterials ratio. There is
the sharp reduction in the viscosity index with
the increase in the amount of surfactant.
(4) The pour point of the lubricant with surface
modified MWCNTs is also influenced by the
quantity of surfactant. There is a decrease in
the pour point with increase in the quantity of
surfactant.
(5) The optimum surfactant to nanomaterials ratio
is found out to be 2:1 for best results. Beyond
TRIBOLOGY – MATERIALS, SURFACES & INTERFACES   7
this ratio, it is found that there is a worsening
of physico-chemical properties.
(6) Pristine MWCNTs, when dispersed in lubri-
cants, could improve the wear performance
marginally but could not perform well in
friction test due to  possible agglomeration of
MWCTS under high loads resulting in deteri-
oration of frictional torque at higher loads.
(7) Surface modification of MWCNTs with both sur-
factants could improve wear and friction perfor-
mance at all loads due to their enhanced stability.
Acknowledgment
The authors gratefully acknowledge the support received
from Hindustan Petroleum Corporation Ltd., India for con-
ducting the tests. The authors acknowledge the assistance
from ARCI, Hyderabad in characterisation. The authors sin-
cerely thank the management of GITAM University, India for
the support extended
Disclosure statement
No potential conflict of interest was reported by the authors.
Notes on contributors
V Srinivas is a professor in the Department of Mechanical
Engineering GITAM (Deemed to be University). His areas of
interests are nanofluids, nanocomposites, nanocoatings and
tribology. He has completed several major research projects
funded by petroleum industries and defence research labora-
tories in India.
Ch. Kodanda Rama Rao is an assistant professor in the
Department of Mechanical Engineering, GITAM (Deemed to
 8   V. SRINIVAS ET AL.
be University). His research interests are bio-fuels, Lubricants
and emission characterization. He is presently working in a
major research project funded by Department of science and
technology, India to develop bio-lubricants.
N Mohan Rao is working as a professor in the Department
of Mechanical Engineering, JNT University, Kakinada, India.
His areas of interest are Mechanical Vibrations and Robot
Kinematics.
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