Tribol Lett (2011) 41:209–215
DOI 10.1007/s11249-010-9702-5
ORIGINAL PAPER
Modification of Graphene Platelets and their Tribological
Properties as a Lubricant Additive
Jinshan Lin • Liwei Wang • Guohua Chen
Received: 18 April 2010 / Accepted: 20 September 2010 / Published online: 6 October 2010
Ó Springer Science+Business Media, LLC 2010
Abstract Graphene platelets were chemically modified in
a reflux reaction with stearic and oleic acids. Examination
of the surface features of the graphene platelets before and
after modification by infrared spectroscopy and ultraviolet–
visible spectrophotometer revealed that the modification
led to an improvement in the dispersion of graphene
platelets in base oil. The tribological behavior of the
lubricating oil containing modified graphene platelets
(MGP) was further investigated using a four-ball machine.
The results indicated that the oil containing only 0.075
wt% of MGP clearly improved the wear resistance and
load-carrying capacity of the machine. Scanning electron
microscopy and energy dispersive spectrometer performed
to analyze the wear scar surfaces after friction confirmed
that the outstanding lubrication performance of MGP could
be attributed to their small size and extremely thin lami-
nated structure, which allow the MGP to easily enter the
contact area, thereby preventing the rough surfaces from
coming into direct contact.
Keywords Graphene platelets
Surface modification

SEM
TEM
Additive-deposited films
1 Introduction
Graphene platelets have been the focus of interest in both
theoretical research and in studies on practical applications
due to their unique structure and remarkable properties [1–5].
Recent studies have shown that graphene platelets have
J. Lin
L. Wang
G. Chen (&)
Institute of Polymer and Nanomaterials, Huaqiao University,
Quanzhou 362021, China
e-mail: hdcgh@hqu.edu.cn
extraordinary electronic transport properties when they
were incorporated in composite materials and distributed
homogeneously throughout the matrix [6–8]. Graphene has
also been used to fabricate a number of simple electronic
devices, such as field-effect transistors [9, 10] and resonators
[11], due to its fundamental electronic properties and semi-
metallic nature. Moreover, graphene platelets are promising
candidates as components in applications such as organic
photovoltaic cells [12], energy-storage materials [13], ‘‘paper-
like’’ materials [14, 15], and liquid crystal devices [16].
However, very few studies on the tribological applica-
tions of graphene platelets have been reported. Peterson
et al. [17] pointed out that effective solid lubricants gen-
erally have a number of basic properties, such as thermal
stability, low shear strength, surface adherence, and char-
acteristics of lamellar structure. A number of researchers
have reported that graphite [18] and some graphite deriv-
atives [19, 20] as well as other lubricant materials [21, 22]
together have the above desirable properties. Graphene
platelets are the building block of the common macro-
scopic solid lubricant graphite, and they also are charac-
terized by possessing the above-mentioned advantages
[23]. Huang et al. [24] investigated the tribological prop-
erties of graphite nanosheets as an oil additive. They found
that the load-carrying capacity and antiwear ability of the
lubricating oil were improved when graphite nanosheets
were added to the paraffin oil at the optimal concentration.
Filleter et al. [25] explored friction and dissipation in
epitaxial graphene films, revealing that bilayer graphene as
a lubricant outperforms even graphite due to reduced
adhesion. Wang [26] suggested the thin films of solid
lubricant materials would be an outstanding solid lubricant
at temperatures ranging from -270 to more than 1,000°C.
Based on these results, it can be inferred that graphene
platelets would be an effective solid lubricant.
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Graphene platelets that are derived from graphite gen-
erally bear hydroxyl and carboxyl functional groups on their
sheet edges [2], which make graphene platelets strongly
hydrophilic and easy to coagulate in oil. Hence, when
graphene platelets are added to the base oil as a lubricant
additive, it is necessary to ensure uniform dispersion
without any agglomeration of graphene platelets in the base
oil. Two main approaches are currently used to solve the
suspension problem. One is that the graphene platelets and
effective dispersant are mixed with the base oil. It has been
proven that the dispersant can enwrap one nanoparticle to
repel another and thereby form a uniform suspension [24,
27]. Nevertheless, due to this action, excessive or too little
dispersant may greatly affect the effectiveness of the sus-
pension [27]. The second approach is to modify the
graphene platelets with a proper modifier. It has been
demonstrated [28–30] that modifying nanoparticles with the
appropriate modifier is an effective way to prevent the
coagulation of nanoparticles in suspension. Chen et al. [31]
reported that multi-walled carbon nanotubes (MWNTs)
modified with stearic acid under the influence of gravity
could be suspended homogeneously in base lubricant for
over 6 months at room temperature, whereas the non-
modified MWNTs were entirely coagulated at the bottom
after 2 months. Structurally, MWNTs consist of multi-
graphene cylinders with end seamless caps.
Here, we report on our use of the second approach to
improve the stability of graphene platelets in oil. However, in
our approach, the selection of an appropriate modifier is the
key. We therefore tested a large number of surface modifiers,
such as sodium dodecyl benzene sulfonate, stearic acid,
dodecyl trimethyl ammonium chloride, oleic acid, sorbitan
monooleate, as well as polysorbate and others, which
involved a considerable research effort. Our results demon-
strated that stearic and oleic acids are the most suitable
modifiers for graphene platelets. We then modified the
graphene platelets with a certain proportion of stearic and
oleic acids and subsequently added the modified graphene
platelets (MGP) into the oil to enhance tribological properties
of lubricating oil. The surface features of the graphene
platelets before and after modification were examined by
Fourier transformed infrared spectroscopy (FTIR) and ultra-
violet–visible spectrophotometry (UV–VIS). Scanning elec-
tron microscopy (SEM) and energy dispersive spectrometry
(EDS) were used to analyze wear scar surfaces after friction.
2 Experimental
2.1 Materials
The graphene platelets and natural flake graphite (particle
size: 25 lm) were provided by the Fujian Kaili Specialty
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Tribol Lett (2011) 41:209–215
Graphite Co.(China). Base oil SN350 was supplied by the
Shishi Zerun Lubricating Oil Co. (China). Stearic acid was
purchased from Shanghai Reagent General Plant (Shang-
hai, China). Oleic acid, cyclohexane, petroleum ether,
ethanol, and acetone, all analytical reagent grade, were
purchased from the Shantou Xilong Chemical Co. (Shan-
tou, China).
2.2 Chemical Modification of Graphene Platelets
and Natural Flake Graphite
Stearic and oleic acids (mass ratio 3:5) were mixed by
sonication in 40 ml cyclohexane for 30 min. Dried graph-
ene platelets were added to the above solution and the
suspension sonicated for 30 min at ambient temperature.
The suspension of graphene platelets was then stirred and
refluxed at 80°C for 5 h, then cooled to ambient tempera-
ture. To remove the residual stearic and oleic acids, the
resulting graphene platelets were filtered and washed with
acetone. The final step was to dry the products under
vacuum at 100°C. For comparison, natural flake graphite
was also modified using the above process.
2.3 Stability Test of Modified Graphene Platelets
The 350SN base oil was used as base lubricant in this test.
The MGP were dispersed in 350SN base oil by sonication
followed by stirring with a magnet for 1 h at 80°C (rotate
speed R = 600 r/min). To evaluate the stabilization of the
MGP in base oil, following the dispersion of the MGP as
described above, the MGP lubricant was diluted 50 times
with pure base oil and precipitated by centrifugation at
1,000 rpm. The supernatant fluid was then decanted at
30-min intervals to evaluate absorbance using a UV–VIS
spectrophotometer. Based on the Lambert–Beer law,
absorbance is proportional to concentration. The concen-
tration of graphene platelets in the supernatant fluid is an
indicator of the suspension property, with higher concen-
trations associated with better suspension properties.
Therefore, the dispersion stability of MGP in base oil was
evaluated by assessing the absorbance. For comparison,
pristine graphene platelets were obtained by the same
process.
2.4 Tribological Properties of MGP as an Oil Additive
The maximum nonseized load (PB), friction coefficient and
the wear rate of the lubricating oil with MGP were tested
on a MS-10A four-ball machine (Xiamen Tenkey Auto-
mation Co., China) and compared to those of the base oil
and the oil with modified natural flake graphite (MNFG).
The PB of the lubricating oil was determined according to
the ASTM D2783 standard method. The machine was
Tribol Lett (2011) 41:209–215 211

conducted at a drive shaft speed of 1,450 rpm and in the

temperature range 18–35 °C. The friction and wear tests
were carried out according to the ASTM D4172-82 stan-
dard method and conducted at a rotating speed of
1,200 rpm and under a constant load of 147 N for a test
duration of 60 min; a temperature of 75 ± 2°C was
maintained throughout the whole test process. The 12.7-
mm diameter test balls used in this study were made of
GCr15A bearing steel (AISI 52100) with a hardness of 64
HRC. Before each test, all test-section components were
cleaned ultrasonically with petroleum ether, rinsed in eth-
anol, and dried. The wear scar diameters on the steel balls
were measured using an optical microscope. The worn
surfaces of the balls after the friction test were examined
with SEM and EDS.

3 Results and Discussion

3.1 Characterization of Graphene Platelets

Fig. 2 Transmission electron microscopy image of graphene platelets

Figure 1 is a typical SEM image of graphene platelets and

shows that the graphene platelets retain their original
25
laminated structure, with an average diameter of 1.2 lm.
The thickness of the graphene platelets is about 10–15 nm
20
(Fig. 2) as determined by transmission electron microscopy
(TEM). 15
after modification
T(%)

3.2 Characterization of MGP

1629
10
2862

The FTIR spectrum of graphene platelets before and after 5

2921
3485

modification is shown in Fig. 3. Pure graphene platelets

1629
0
only showed a weak peak at 1,629 cm-1, which refers to before modification
C=C bonds. After modification with stearic and oleic acids,
-5
the peak at 1,629 cm-1 was strengthened, likely due to the 4000 3500 3000 2500 2000 1500 1000 500
absorption of oleic acids on the graphene platelets. Wavenumber(cm-1)

Fig. 3 Infrared spectrum of modified graphene platelets (MGP) and

pristine graphene platelets

Simultaneously, three new peaks at approximately 2,862,

Fig. 1 Scanning electron microscopy image of graphene platelets
2,921, and 3,485 cm-1 were clearly observed. The peaks at
2,862 and 2,921 cm-1 are attributed to CH3 and CH2
stretching mode, respectively, while the broad peak at
3,485 cm-1 can likely be attributed to -OH bonds. Coates
[32] reported that the impact of hydrogen bonding could
produce significant band broadening as well as lower the
mean absorption frequency, as shown in Fig. 3. Therefore,
we concluded that the surfaces of graphene platelets were
chemically modified by stearic and oleic acids.
Figure 4 shows the suspension stability of the two
lubricating oils as evaluated by UV–VIS spectrophotome-
try, which measured the UV intensity of the lubricating oil

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212 Tribol Lett (2011) 41:209–215

750
1.00
pristine graphene platelets
oil with modified graphene platelets
0.95 modified graphene platelets 700
oil with modified natural flake graphite
Relative Concentration

0.90
650
0.85
600

PB(N)
0.80

0.75 550

0.70 500
0.65
450
0.60
400
0 50 100 150 200 250
0.00 0.02 0.04 0.06 0.08 0.10 0.12
Time(min)
C(wt%)
Fig. 4 Suspension stability of the lubricating oils with MGP and
Fig. 5 Effect of MGP and modified natural flake graphite (MNFG)
graphene platelets as determined by ultraviolet–visible light (UV–
concentration on maximum nonseizure load of the oil
VIS) spectrophotometry

solution by evaluating the rate of nanoparticle sedimenta- 1.2

tion. The relative concentration was calculated by the ratio 1.1
of the particle concentration intensity of the supernatant oil with modified natural flake graphite
1.0
oil with modified graphene platelets
fluid at each measurement time divided by the initial con- 0.9 pure base oil
centration intensity of the suspension. A value of 1.0 at the
Wear rate(%)

0.8
relative concentration means excellent stability of the
0.7
lubricating oil solution without particle sedimentation.
0.6
Figure 4 shows that the particle concentration of the two
different suspensions was nearly equal before centrifuga- 0.5

tion. Following a long period of centrifugation, rapid pre- 0.4

cipitation was observed for the suspension with the pristine
graphene platelets, indicating that unmodified graphene
platelets were heavily agglomerated in base oil. In contrast,
little MGP precipitation was observed in the suspension
with the MGP. This result indicates that the addition of
MGP to the lubricating oil had produced an excellent stable
suspension and that this improvement could be attributed to
the effectiveness of the surface modification. Following the
modification of the graphene platelets with stearic and oleic
acids, the hydrophilic segments of the stearic and oleic acids
molecules were anchored onto the surface of the graphene
platelets. When the MGP were dispersed in the base oil, the
long hydrocarbon segments easily stretched into the base oil
and therefore produced a typical steric hindrance effect
[31], which effectively helped to separate the graphene
platelets from each other. At the same time, the steric hin-
drance force could conquer gravity and prevent the graph-
ene platelets from coagulating. Therefore, the lubricating
oil with MGP formed a uniform and stable suspension.
3.3 Tribology Tests of the Lubricating Oil with MGP
or MNFG
Bartz [33] pointed out that an optimal concentration of
solid additive, such as graphite, exists in liquid lubricant. In
0.3
0.2
0.1
10 20 30 40 50 60
Friction time(min)
Fig. 6 Wear rate as a function of friction time (four-ball, 1,200 rpm,
147 N, 60 min, 75 ± 2°C)
order to determine the concentration of additive giving the
best tribological behavior, we tested several dispersions of
MGP (0.015, 0.035, 0.055, 0.075, 0.095, and 0.105 wt%)
and MNFG. Figure 5 shows the influence of MGP and
MNFG concentration on maximum nonseizure load (PB) of
the oil. The PB represents the load-carrying capacity of the
lubricating oil; in the pure base oil with 0 wt% of graphite
particles, the PB value was 418.5 N. There was a remark-
able increase in the PB values of the lubricating oil with the
addition of increased concentrations of MGP and MNFG,
respectively, to the base oil. When the concentration of
MGP and MNFG reached 0.075 wt%, both PB values
reached their maximum, but the largest PB value of the oil
with MGP was 627.2 N, which was much higher than that
of oil with MNFG (523 N). These results indicate that the
oil with MGP had a better load-carrying capacity than the
base oil and oil with MNFG. When the concentration was

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Tribol Lett (2011) 41:209–215 213

0.22 higher than 0.075 wt%, excessive MGP also resulted in a

oil with modified graphene platelets
0.21 pure base oil
decrease in the PB value of the oil. One possible expla-
0.20 oil with natural flake graphite nation is that some coagulation of graphene platelets and
Friction coefficient µ

0.19 metallic debris occurred at higher concentrations of MGP/

0.18 MNFG owing to the friction effect, which made the friction
0.17 unstable or caused vibration, leading to a decrease in the
0.16 maximum nonseized load [34].
0.15 Figure 6 shows the wear rate of lubricating oils as a
0.14 function of friction time, with MGP and MNFG concen-
0.13 trations of 0.075 wt% and a load of 147 N for 60 min at a
0.12 speed of 1,200 rpm. It can be seen that the wear rates
0.11 increased with increasing friction time. However, the wear
rate of the oil with MGP increased to a lesser degree and
0 10 20 30 40 50 60
Friction time(min) more gradually than that of the base oil and the oil with
MNFG. A similar tendency was observed in Fig. 7, which
Fig. 7 Friction coefficient as a function of friction time (four-ball, displays the friction coefficient as a function of friction
1,200 rpm, 147 N, 60 min, 75 ± 2°C)
time. With increasing friction time, the friction coefficients

Fig. 8 The worn surface of the

steel ball and the corresponding
energy dispersive spectrometry
analysis. a Lubricated with base
oil, b lubricated with base oil
containing MNFG, c lubricated
with base oil containing MGP

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of both the base oil and the oil with MNFG increased
remarkably; in comparison, the friction coefficient of the
oil with MGP was relatively steady throughout the test.
Moreover, the friction coefficient of the oil with MGP was
much lower than that of the base oil and oil with MNFG.
The excellent anti-wear properties of MGP may possibly
be attributed to their small diameter and extremely thin
laminated structure, which allows MGP to easily enter the
contact area and deposit a continuous protective film that
prevents direct contact with the rough face. The MNFG
was unable to perform this efficiency due to the large size
of its lamellae.
3.4 Surface Analysis
The lubricating oil containing MGP presents excellent
anti-wear and friction-reducing properties, which were
confirmed by the results of the SEM and EDS analysis.
Figure 8 shows the SEM images of the rubbing surfaces
lubricated by three lubricating oils as well as the corre-
sponding EDS analysis. As shown in Fig. 8a, the metal
surface has been severely scratched due to the poor anti-
wear property of the pure base oil. The EDS analysis
showed that the content of C element on the metal surface
was only 3.6 wt%, which may be due to the basal com-
ponent of the steel ball and carbonizations of the oil layer.
The rubbing surface shown in Fig. 8b was smoother than
that in Fig. 8a, but it still showed obvious scratches and
extensive furrows. Correspondingly, the EDS analysis
displayed a content of C element of 10.2%, just a little
higher than that found in Fig. 8a. This result indicates that
natural flake graphite was barely deposited on the rubbing
surface, which confirms that this graphite has difficulty
entering the contact area and, consequently, forming a
continuous protective film. In contrast, it can be seen in
Fig. 8c that many graphene platelets were distributed on
the metal surface and that the surface had nearly none of
wear and scratch traces observed in Fig. 8a and b. In
addition the content of C element was up to 27.86%, which
is nearly ninefold and 2.7-fold higher than that shown in
Fig. 8a and b, respectively. This result clearly proves that
graphene platelets in oil easily form protective deposited
films to prevent the rubbing surfaces from coming into
direct contact and, thereby, improve the entirely tribolog-
ical behavior of the oil.
4 Conclusions
The results of our study clearly demonstrate that the
graphene platelets were effectively modified by stearic and
oleic acids, thereby enabling the MGP added as lubricant
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Tribol Lett (2011) 41:209–215
additive to stably disperse in oil. The wear resistance and
load-carrying capacity of the lubricating oil were greatly
improved with the addition of MGP at an optimal content
of 0.075 wt%. The friction coefficient of the oil with MGP
was much lower than that of the base oil and oil with
MNFG. In summary, the overall lubricious properties of
the lubricating oil were notably improved, and this
improvement can be attributed to the addition of MGP.
Acknowledgments This work is supported by National Science
Foundation of China (No. 20574025), Natural Science Foundation of
Fujian Province (E0820001), and Fujian Key Laboratory of Polymer
Materials (Fujian Normal University).
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