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Study Tribological Properties of MoDTC and Its Interactions With Metal

Detergents

Article  in  Journal of Tribology · December 2020

DOI: 10.1115/1.4047457

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 Dongya Zhang1
Key Laboratory of Manufacturing Equipment of the
Shaanxi Province,
School of Mechanical and Precision Instrument
Engineering,
Xi’an University of Technology,
Xi’an 710048, Shaanxi, China
e-mails: dyzhang@xaut.edu.cn;
zhangdy0241@126.com

Zhongwei Li
Study Tribological Properties

Key Laboratory of Manufacturing Equipment of the
Shaanxi Province,
School of Mechanical and Precision Instrument
Engineering,
Xi’an University of Technology,
Xi’an 710049, Shaanxi, China
e-mail: lzwxwb@163.com
Xian Wei
Key Laboratory of Manufacturing Equipment of the
Shaanxi Province,
School of Mechanical and Precision Instrument
Engineering,
Xi’an University of Technology,
Xi’an 710049, Shaanxi, China
e-mail: weixian0506@126.com
Liping Wang1
Petro China Lanzhou Lubricating Oil R & D
Institute,
Lanzhou 730060, Gansu, China
e-mail: wanglipinglz_rhy@petrochina.com.cn
Jinbao Xu
Petro China Lanzhou Lubricating Oil R & D
Institute,
Lanzhou 730060, Gansu, China
e-mail: xujinbao_rhy@petrochina.com.cn
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of MoDTC and Its Interactions
With Metal Detergents
Recently, the synergistic tribological properties between molybdenum dialkyldithiocarba-
mate (MoDTC) and metal detergents have been the focus of significant attention due to
the high requirements of engine oil. In this study, an SRV tribometer and four-ball
machine were used to study the tribological performance of MoDTC combined with three
types of metal detergents with different base numbers. Meanwhile, the detergency of the
three metal detergents was also investigated using the hot tube test and crankcase simula-
tion test. The results showed that (i) a high-based detergent possessed an excellent deter-
gency performance compared with that of low-based detergents. (ii) The tribological
properties of the base oil with a content of 0.75% MoDTC were superior to those of
other contents at elevated temperatures. (iii) The metal detergents with a higher base
number showed the best thermal stability, detergency performance, and anti-wear perfor-
mance among the three types of metal detergents. The anti-wear mechanism was that the
synergistic action of active elements in MoDTC and metal detergents promoted the gener-
ation of a tribological film. [DOI: 10.1115/1.4047457]
Keywords: MoDTC, metal detergents, detergency, tribological properties, tribological
film, lubricant additives, anti-wear mechanism

Yufeng Liu
Petro China Lanzhou Lubricating Oil R & D
Institute,
Lanzhou 730060, Gansu, China
e-mail: liuyufeng_rhy@petrochina.com.cn

1 Introduction 200–300 °C and a high speed of 6000 rpm [4]. With the develop-
ment of engine technology, a lubricating oil with a long service
Friction between moving pairs of the automobile engine can
life, excellent degradability, and high thermal stability is required
cause tremendous energy loss and even results in serious wear
to satisfy the demand for severe working conditions.
and early-stage failure during poor and complex working condi-
It is well known that the addition of appropriate additives to the
tions. Taking a report of American passenger cars for example, if
base oil can reduce friction and enhance the anti-wear performance
a 10% reduction in engine friction was applied to all US passenger
of engine components [5–7]. Molybdenum dialkyldithiocarbamate
cars, 3.4 billion gallons of fuel would have been economized in
(MoDTC) can be dissolved in lubricating oil and generate a Mo
2007 [1]. Among all friction pairs of the engine, the assembly of
composite transfer film on the frictional surface, thus, reducing fric-
the cylinder liner and piston ring is one important component,
tion and showing an excellent friction and wear performance [8,9].
50% of the friction losses is due to the piston/cylinder system,
Yajun et al. [10] reported that the friction and wear of piston rings
which thus directly affects the service life and performance of the
were reduced when lubricated with MoDTC-oil, when compared
engine [2]. Lubricating oil can effectively reduce friction and
with GF-3 base oil. This study revealed that a tribochemical inter-
wear and prolong the lifetime of the engine [3], even the system
action occurred and then apparently formed MoS2 film on the fric-
works under serious conditions, such as a high temperature of
tion surface. Zhou et al. [11] studied the effect of the MoDTC
content on the tribological performance of a WC/a-C(Al) coating,
1
and the friction-reducing and anti-wear properties of the coating
Corresponding authors. were enhanced at an MoDTC content of 1%; however, the tribolog-
Contributed by the Tribology Division of ASME for publication in the JOURNAL OF
TRIBOLOGY. Manuscript received December 17, 2019; final manuscript received May ical property was worse the additive was at a higher content.
13, 2020; published online June 19, 2020. Assoc. Editor: Satish V. Kailas. Recently, solid–liquid composite lubrication technology, which

Journal of Tribology Copyright © 2020 by ASME DECEMBER 2020, Vol. 142 / 122201-1
combined with surface coating or surface texture and oil lubrication, Table 1 Characterization of the detergents
can compensate for the shortage of a single lubricant and extend the
service life of mechanical parts [12–15]. Yue et al. [16] reported that Low-based High-based Middle-based
a sulphur-nitride surface showed a lower friction coefficient and synthetic synthetic calcium alkyl
wear-rate while being lubricated with MoDTC, when compared calcium sulfonate calcium salicylate
Analysis item (T104) sulfonate (T106) (T109)
with those of a nitride surface, and the reason was that a composite
film of MoS2 and FeS formed on the sulphur-nitride surface. Total base 29.2 mg KOH/g 305 mg KOH/g 176 mg KOH/g
Metal detergents can neutralize the organic acid generated by the number
oxidation of lubricating oil and prevent the deterioration of lubricat- S content (%) 2.44 1.44 –
ing oil and additives [17]. In addition, the detergent can disintegrate Ca content (%) 2.82 11.82 6.42
the paint film and carbon deposition to minuscule impurities that are Structure
easily filtered out during the oil cycle [18], which expands the usage
time of the lubricating oil [19]. In addition, many studies have

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shown that the nanoparticles in the detergent micelle have a good
anti-wear effect [20,21]. Topolovec-Miklozic et al. [22] studied
the tribological properties of overbased calcium sulfonate deter-
gents and concluded that calcium sulfonate could form a protective
film with a thickness of 100–150 nm on the metal surface, which
had an excellent protective effect. Costello and Riff [23] studied Table 2 Test oil containing agents
the anti-wear mechanism of a calcium alkyl benzene sulfonate
Oil code Test oil composition
detergent under the boundary lubrication condition, and the
results showed that the detergent could generate a stable protective Oil 1.0 YU6
film on the metal friction surface at a lower temperature. Oil 1.1 YU6 + 2.0% T104
However, interactions between additives are very complicated Oil 1.2 YU6 + 2.0% T106
and are influenced by many factors, such as additive structure and Oil 1.3 YU6 + 2.0% T109
additive content. In addition, the test temperature also influences Oil 2 YU6 + 0.25% MoDTC
the performance of the additives. Thus, in this paper, the tribologi- Oil 3 YU6 + 0.50% MoDTC
cal performances of MoDTC combined with three metal detergents Oil 4 YU6 + 0.75% MoDTC
at elevated temperatures were investigated. Scanning electron Oil 5 YU6 + 1.00% MoDTC
microscopy (SEM), energy dispersive spectrometry (EDS), and Oil 6 YU6 + 0.75% MoDTC+2.0% T104
Oil 7 YU6 + 0.75% MoDTC+2.0% T106
laser confocal microscopy were used for the surface analysis of Oil 8 YU6 + 0.75% MoDTC+2.0% T109
the wear scars, and finally, the lubrication mechanisms of the
MoDTC and metal detergents were discussed.

temperature of 300 °C. Subsequently, the sediment produced in

2 Experiments
2.1 Base Oil and Additives. API Group III mineral oil
(Yubase 6, available from SK Industries Co., Ltd) was obtained
as the base oil, which had a kinematic viscosity of 32 cSt at 40 °C.
MoDTC (obtained from ADEKA Co.) was added into the base oil
and acted as a friction improver. Three detergents with different
total base numbers were selected and added into the base oil. The
detergents were the low-based synthetic calcium sulfonate (T104),
high-based synthetic calcium sulfonate (T106), and middle-based
calcium alkyl salicylate (T109). The characterization of the deter-
gents is shown in Table 1.
2.2 Test Oils. The test oils containing additives of MoDTC
and a detergent were selected to study the tribological perfor-
mances. (i) The detergents of T104, T106, and T109 with a
content of 2.0 wt% were added into the base oil separately, with
coding as Oil 1.1, Oil 1.2, and Oil 1.3; (ii) MoDTC in contents of
0.25, 0.5, 0.75, and 1.0 wt% was added into the base oil and
coded as Oil 2–Oil 5; (iii) The detergents T104, T106, and T109
with 2.0 wt% were added into 0.75 wt% MoDTC-base oil, and
the oils were coded as Oil 6–Oil 8. In addition, the base oil
without MoDTC and detergent was used as a reference for compar-
ison. The details of the test oils are shown in Table 2.
2.3 Characterization Test Methods. A thermal analyzer
(type of TA-9900) was applied to evaluate the thermal stability of
the three detergents. The experiment was performed by heating
the detergent sample from 25 °C to 800 °C at a rate of 20 °C/min
in an N2 atmosphere.
A BIRGY-950 heat pipe oxidation tester was used to measure
and evaluate the high-temperature detergency of the detergent.
The test oil and air were blown into the glass tube at rates of
0.30 ml/h and 10 ml/min, respectively, and heated for 16 h at a
the glass tube was evaluated to mark the lacquer formation on the
basis of 10 points. A higher value means that the lacquer is low
and the detergency is better.
The coking test was used to estimate the high-temperature deter-
gency of the test oil according to the FTM 791-3462 procedure. The
test oil was sprayed onto a high-temperature aluminum sheet, and a
coking film was deposited on the sheet due to the oxidation of the
oil. The test was performed as follows: the test oil temperature
was kept at 150 °C and the aluminum sheet temperature was
320 °C. The oil was splashed for 15 s and stopped for 45 s per
minute, and the test was maintained for 60 min. Each oil was
tested three times, and the average coking film weight on the alumi-
num sheet was adopted.
2.4 Tribological Test. To systematically investigate the tribo-
logical performance of the test oils containing a combination
of MoDTC and detergents, the tests were carried out as follows:
(i) the tests of the friction-reducing and anti-wear properties were
performed on an Optimol SRV-IV reciprocating tribometer
(Optimol Instruments, Munich, Germany) at room temperature
and elevated temperatures; (ii) the anti-wear performance of the
test oils, evaluated by the wear scar diameter (WSD) of the test
ball, was obtained using an MS-10 four-ball machine (Xiamen
Tenkey automation Co. Ltd., China).
For the friction-reducing test on the Optimol SRV-IV tribometer,
an AISI 52100 steel disc with a 60 mm diameter and 5 mm thick-
ness acted as the lower sample and was polished to a surface rough-
ness Ra of 0.05 μm. The hardness of the disc sample was HRC 63.
A commercial AISI 52100 steel ball with a diameter of 10 mm and
hardness of HRC 62 was acted as the upper sample. The test condi-
tions were set as follows: the normal load was 400 N, reciprocating
stroke was 1.5 mm, reciprocating frequency was 50 Hz, and sliding
duration was 45 min. The test temperatures were (a) a fixed temper-
ature of 25 °C and (ii) an increase in temperature from 40 °C to

122201-2 / Vol. 142, DECEMBER 2020 Transactions of the ASME

 









D2
h = R − R2 − (2)
4
where V is the wear volume of the ball, h represents the worn depth
of the ball, R is the ball radius, and D is the wear scar diameter on
the ball.
For the anti-wear performance on a four-ball machine, AISI
52100 steel balls (diameter of 12.7 mm, hardness of HRC 60, and
surface roughness of Ra 0.025 μm) were applied as the test balls.
Details of the test conditions are given in Table 3. The WSD of
the test ball was analyzed using a digital optical microscope
(VH-8000), each test was also replicated three times, and the
average value was taken as the WSD result. Before and after each

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friction test, the test ball was ultrasonically cleaned with acetone
for 10 min successively thrice to ensure the proper removal of resid-
ual pollutant and then dried by a blower. The wear surface was ana-
lyzed by using a field emission scanning electron microscope
(Magellan 400, Hillsboro, OR). Energy dispersive spectrometry
was adopted to detect the tribological film on the wear scars.
Fig. 1 Heating pattern of SRV tribological tester

3 Results and Discussion

3.1 Characterizations of Detergents. Metal detergent com-
Table 3 Test conditions under the SRV-IV tribometer and
four-ball machine
prises surfactant, metal carbonates, and a certain amount of oily
solvent, and it exists as micelle particles with nano-scale size.
Test 1 Test 2 Test 3 Metal carbonates and a small amount of metal hydroxide constitute
the micelle, and the nano-micelle is dispersed in the solvent oil,
Tribometer SRV-IV Four-ball forming a stable solution. Figure 2 shows the freeze-etching replica-
Normal load 400 N 196 N tion transmission electron microscopy (FERTEM) images of the
Sliding speed 50 Hz 1450 rpm three detergents, which evidence that the detergent micelles with dif-
Temperature 25 °C 40–120 °C 25 °C ferent shapes and sizes. The micelle in T104 is an irregular shape, and
Test time 45 min 10 °C/5 min 60 min the average size is 150 nm; the micelle sizes in T106 and T109 are in
Test oil Oil 1.0–Oil 1.3 and Oil 2 Oil 1–Oil 8 Oil 1–Oil 8
a range of 60–80 nm. Meanwhile, the micelle distributions of T106
Test items Friction coefficient and wear volume WSD
and T109 are more uniform than that of T104. A small size can
increase the specific surface area and enhance the adsorption
amount of the surfactant so that the stability of the particles in the
120 °C [24]. SRV-IV reciprocating type tribometer is a common oil does not lead to deposition with gravity, thus, the suspension of
commercial standard friction testing machine and has been widely the detergents is more stable as particles become smaller and have
used to measure high-temperature tribological performance of lubri- a more regular sharp. The nanoparticles may cause the rolling
cating oil. The tribometer is shown in Fig. 1, the temperature sensor effect between the rubbing surfaces under the boundary lubrication
of thermocouple is marked in the picture, and a thermocouple mea- condition and achieve a good anti-wear performance [26].
sures the temperature of oil cup, the oil cup has a high conduction
coefficient, and the temperature of the lubricating oil is approxi- 3.1.1 Thermal Stability. Thermal stability has an important
mately equal to that of the oil cup during the test. influence on the performance of the metal detergent. If the metal
The wear volume of the test ball was used to estimate the anti- detergent decomposes when heated at a certain temperature, the
wear performance of the additives. Each test was replicated three usable range of the detergent would be restricted. Thermal gravi-
times, and the average value was taken as the wear volume. The metric analysis curves of the three detergents are presented in
wear volume of the test ball was calculated using the following Fig. 3. The first decomposition temperature of T106 (315 °C) is dis-
equation [25]: tinctly lower than that of T104 (350 °C) and T109 (350 °C), and the
weight loss is lower than that of T104 and T109. Another obvious
decomposition temperature stage is in the range of 400–700 °C, and
πh2 (3R − h) the weight losses of T104 and T109 are lower than 20.0%, while the
V= (1)
3 weight loss of T106 is 39.5%, which is mainly attributing

Fig. 2 FERTEM images of the nano-micelles in the detergent: (a) T104, (b) T106, and (c) T109

Journal of Tribology DECEMBER 2020, Vol. 142 / 122201-3

 The coking test results of the oils is shown in Fig. 5. It can be seen
that the brown coking films of the three detergents possess obvious
differences on the aluminum plates, and the coking film area of
T106 is the smallest. Furthermore, the coking amounts of T104
and T109 are 65.2 mg and 54.1 mg, but the coking amount of
T106 is 42.7 mg, which is obviously lower than that of T104 and
T109. It also verifies that detergency of T106 is superior to T104
and T109. The reason is that the acid neutralization ability of the
detergent is enhanced with the increase in the total base numbers
and has a greater inhibitory effect on the generation of coke.
T106, with the highest total base number among the three deter-
gents, thus has an excellent high-temperature detergency.

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3.2 Tribological Properties
3.2.1 Effect of a Single Additive. Figure 6 shows the friction
coefficient when lubricated with the base oil (Oil 1.0) and with
the base oil contains a single additive (Oil 1.1, Oil 1.2, Oil 1.3,
Fig. 3 Thermal gravimetric analysis curves of T104, T106, and
T109 and Oil 2) at a fixed temperature of 25 °C (Test 1).
It is clear that the friction coefficient curves show obviously dif-
ferent tendencies. For Oil 1.0 and Oil 2, their friction coefficient
decomposition of CaCO3 to CaO [19]. In addition, the binding force curves decline at first, then reach a certain peak value at the start
of the SO3 group is stronger than that of the COO- group. This result stage, and slowly decrease to a stable value with the prolong of
implies that T106 exhibits a better thermal stability which can be of sliding time. To be specific, the friction coefficient of Oil 1 is as
service under high-temperature conditions. high as 0.21 at the beginning stage, which is twice that of Oil
The lubricating oil is usually influenced by the prevailing temper- 2. It is worth mentioning that the friction coefficient of Oil 2 is in
atures at the surfaces of the engine component. In internal combus-
tion engines, automotive crankcase oils experience a wide variety of
hot-spot temperatures, ranging from 90 °C at the connecting rod and
cylinder head, to 426 °C at the piston crown under normal operating
conditions [27]. Generally, the ideal lubrication condition for a real
engine oil is hydrodynamic lubrication, which requires a high oil
viscosity, and the normal engine oil temperature is limited lower
to 100 °C. However, oil acidity of the commercial oils is rapid
increased as temperatures above 140 °C [28].
In this paper, the temperature of high-temperature tribological
test is suggested at 120 °C, the reason is that a higher oil tempera-
ture is not allowed for the car engine. Furthermore, the decomposi-
tion temperature of metal detergent is over 300 °C (obtained by
thermogravimetric tests), which means that these metal detergent
can work well at temperatures above 120 °C.

3.1.2 Detergency Performance. Detergency can be evaluated

by the degree of a lacquer formed on the glass tube, and the
lacquer is rated using a color merit scale from level 0 (dark) to
Fig. 5 Coking test results of the test oils containing detergents
level 10 (clear) [29]. It is considered that the detergency perfor- of T104, T106, and T109
mance is improved with the increase in level value, and level 10
indicates the detergent has a superior high-temperature detergency
performance. Figure 4 shows the hot tube test results of the test
oils. In the case of the base oil, the lacquer formed in the tube is
the darkest, indicating a poor detergency. The level values of the
oil with T104, T106, and T109 are 4, 6, and 5, which shows that
the detergency performance of the base oil is improved after
adding the detergent. Furthermore, the T106 shows the best deter-
gency performance at high temperatures.

Fig. 4 Hot tube result of the test oil containing detergents of Fig. 6 Friction coefficient of base oil and single additive using
T104, T106, and T109 the SRV tribometer

122201-4 / Vol. 142, DECEMBER 2020 Transactions of the ASME

the range of 0.053–0.057 at the stable stage, indicating that the
lubricating properties of the base oil can be improved by adding
MoDTC. The reason is that tribochemical interactions occur
during the sliding test upon adding MoDTC, and similar results
were reported by previous studies [16,30]. While for Oil 1.1, Oil
1.2, and Oil 1.3, their friction coefficient curves increase at the
initial stage, and then decline to a stable value as sliding continues.
The friction coefficient of the base oil containing T104 remains at a
high value of 0.17, which is close to that of the base oil (Oil 1.0),
while the friction coefficient curves of the base oil containing
T106 and T109 are almost overlapped, and the average friction
coefficient is 0.15, which is clearly higher than that of Oil 2. This
result indicates that oil containing a single metal detergent has a

poor lubrication performance.
Figure 7 illustrates the WSD of the test ball lubricated with the
base oil (Oil 1.0) and the base oil containing a single additive
(Oil 1.1, Oil 1.2, Oil 1.3, and Oil 2) using the four-ball test
machine (test 3). The wear scar diameter of the base oil is as
large as 0.55 mm, while it declines to different degrees when a
single additive is added into the base oil. In addition, it can be
observed that the metal detergent and MoDTC have significantly
different effects on the wear scar diameter. The wear scar diameter
of the base oil containing MoDTC is 0.40 mm and that of the oil
containing T106 obtained the lowest value of 0.33 mm. Such an
improvement can be attributed to the transfer of MoDTC and
calcium carbonate to form a tribochemical film on the mating
contact surface.
3.2.2 Effect of the MoDTC Content. MoDTC is an excellent
friction modifier and has been widely used to enhance the tribolog-
ical performance of the base oil. In this section, a content of 0.25–
1% MoDTC was respectively added into the base oil, and the tribo-
logical performances were measured at a fixed temperature of 25 °C
and an elevated temperature of 40–120 °C separately.
Figure 8 shows the average friction coefficient of the balls lubri-
cated by the test oils with different MoDTC contents at an elevated
temperature (test 2). It can be seen from Fig. 8 that the friction coef-
ficient of Oil 1 gradually reduces at first and then increases with the
test temperature, and the friction coefficient fluctuates in the range
of 0.15–0.19 as the temperature increases from 40 °C to 120 °C.
When adding MoDTC, the friction coefficients of the test oils are
significantly reduced, and remain at a low and steady value.
During the test, the friction coefficient gradually reduces with the
increase in the additional amount MoDTC. In the case of 0.75%
MoDTC, the friction coefficient of Oil 4 is the lowest and with a
value of 0.06. In addition, the friction coefficient of the MoDTC-
base oil is substantially lower at the temperature of 60 °C and
70 °C. MoDTC has an excellent anti-friction performance,
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Fig. 8 Effect of elevated temperatures on the friction coefficient
of the test oils with different MoDTC content using the SRV
tribometer
because MoDTC decomposes easily under high temperatures, and
the amounts of Mo and S increase with the temperature [31]. Mean-
while, the MoS2 protective film forms on the fresh steel surface with
the decomposition of MoDTC, and thus, MoDTC endows a remark-
able lubrication and anti-wear performance under high temperature.
Similar experimental phenomena and mechanism were suggested
by previous study [32].
In short, the friction coefficient lubricated with MoDTC is high at
the beginning then gradually drops to a lower value, and the lowest
friction coefficient is obtained at the temperature of 70 °C, finally
gradually reaching a steady state and with a slight fluctuation. In
addition, the lowest friction coefficient was obtained at a critical
content and/or critical temperature [33]. The lubrication perfor-
mance of MoDTC may decrease or even be lost in a high tempera-
ture and/or oxidation-friendly environment [34]. The main reason is
that the tribo-film of MoS2 is oxidized to MoO3, and the lubrication
property of MoO3 is poor [35].
Figure 9 presents the wear volume of the balls lubricated by the
test oil with different MoDTC contents at elevated temperatures
(test 2), and the wear volumes of the test balls lubricated by the
MoDTC-base oil are significantly lower than that of the base oil.
Even with a low amount of 0.25% MoDTC (Oil 2), the wear
volume is 25% of the base oil (Oil 1). This result confirms that
the selected content of MoDTC has a good anti-wear performance.
The reason is that the organic molybdenum additives can quickly

Fig. 7 Wear scar diameter of base oil and individual additive Fig. 9 Effect of MoDTC content on the wear volume of the test
using the four-ball test ball using the SRV tribometer

Journal of Tribology DECEMBER 2020, Vol. 142 / 122201-5

occupy and decompose on the frictional steel surface, and forming a
tribochemical film with good strength [36]; this film can slip easily
because of its layered structure, which can make a low friction
occurring on the soft film, and thus improve the tribological perfor-
mance. Meanwhile, the wear volume decreases at first and then
increases with the MoDTC content. When the content increases
to 0.75% (Oil 4), the wear volume of the test ball is as low as
8.3 × 104 μm3, which is lowest of the test oils with different
MoDTC contents.
3.2.3 Synergistic Effect of the Detergent and MoDTC.
Figure 10(a) shows the friction coefficient as a function of the tem-
perature when lubricated by the base oil containing a detergent
and MoDTC after sliding for 2700 s (test 2). It can be observed
that (i) with the increase in temperature and sliding time, the friction
coefficient of Oil 4 increases slowly and it reaches a high value of
0.071, while the friction coefficients of Oil 5, Oil 6, and Oil 7
exhibit fluctuations and gradually decline, and the lowest friction
coefficient is obtained when lubricated with Oil 6. (ii) The friction
coefficient can be significantly reduced by adding T104 and T106
into the base oil and MoDTC mixture in the temperature range of
40–120 °C during the whole test, while the friction coefficient
obtained with T109 is first higher than that of Oil 4 at the temper-
atures lower than 70 °C, and then, it reduces to lower than that of
Oil 4. This result shows that T106 combined with MoDTC presents
a synergistic effect of friction reduction performance.
Generally, the lubricating oil viscosity decreases with increasing
temperature, which induces a decrease in the thickness and stiffness
of the oil film. Thus, the lubrication condition shifts to a boundary
or mixed lubrication regime and causes direct contact of the asper-
ities of the two metal surfaces. Theoretically, a higher temperature
should lead to a greatly higher friction coefficient [37]. Meanwhile
(a)
(b)
Fig. 10 Effect of detergent on (a) friction coefficient and (b) wear
volume using the SRV tribometer
122201-6 / Vol. 142, DECEMBER 2020
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Fig. 11 Effect of detergent on the wear scar diameter using the
four-ball test
the MoS2 transfer film generated on the sliding surfaces, which also
provides an excellent anti-friction effect, and thus, the friction coef-
ficient curves of these test oils are relatively low and steady. The
micelles in the metal detergent release calcium carbonate nanopar-
ticles during the friction process and can form a CaCO3 deposition
film rapidly [36]; this film prevents the direct contact between the
friction surfaces and leads to a lubrication and an anti-wear perfor-
mance. T106 and T109 have a higher content of calcium, and their
deposition films of calcium carbonate are thicker than that of T104.
Thus, friction coefficients of the T106 and 109 are gradually
declined with temperature increases.
Figure 10(b) shows the wear volume of the test ball lubricated by
the oil containing three detergents using the SRV tribometer. When
the detergent is T104, the wear volume is 6.2% of that of Oil 4. For
T106 and T109, the wear volume of the test balls becomes lower
than that of Oil 4 and Oil 6. The results indicate the anti-wear per-
formance of the oil is improved when containing T106. Further-
more, the results suggest that with the base oil containing
MoDTC and T106 used as a lubricant, the dominating anti-wear
mechanism would be the depositing of CaCO3 and MoS2 film on
the worn surface.
The WSD with the content of the additives in the base oil under
196 N using the four-ball test is illustrated in Fig. 11. It can be
observed that the MoDTC can significantly reduce the wear scar
diameter of the test ball, for example, the wear scar diameter
decreases from 0.55 mm to 0.40 mm by adding 0.25% MoDTC.
The anti-wear performance is improved further as the additive
content increases, and the wear scar diameter decreases to
0.35 mm as the MoDTC content increases to 0.75%. Another inter-
esting effect is that the WSD value of the test balls is dramatically
reduced by the combination of MoDTC and detergent. When T104
and T109 are added into Oil 4, WSD values reduce to 0.30 mm and
0.29 mm. When T106 is added into Oil 4, the WSD obtains the
lowest value of 0.25 mm, 54% lower than that of the base oil,
which confirms the high-based synthetic calcium sulfonate (T106)
exhibits a good load carrying capacity. Thus, the detergent combi-
nation with MoDTC has a superior anti-wear performance, mainly
because the calcium carbonate and calcium oxide in the detergent
can form a protect film on the surface [38,39], and the thickness
of the protection film is influenced by the total base number; the
protection film has a better anti-wear performance when the oil con-
tains a detergent with a higher base number [40].
3.3 Wear Surface Analysis. Figure 12 presents the 3D
surface morphology of the wear scars of test balls lubricated by
oil containing different additives after the four-ball test. From the
3D micrographs depicted in Fig. 12(a), it is observed that the
worn surface is very rough, and the maximum wear scar diameter
Transactions of the ASME
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Fig. 12 3D images of four-ball test ball lubricated with (a) base oil, (b) 0.20% MoDTC, (c) 0.75% MoDTC, (d) 0.75% MoDTC + T104,
(e) 0.75% MoDTC + T106, and ( f ) 0.75% MoDTC + T109

Fig. 13 SEM images of wear scar lubricated with test oils after four-ball test: (a) Oil 1, (b) Oil 2, (c) Oil 3, (d ) Oil 4, (e) Oil 5, ( f ) Oil 6,
(g) Oil 7, and (h) Oil 8

Journal of Tribology DECEMBER 2020, Vol. 142 / 122201-7

is obtained when lubricated with the base oil. When lubricated with
the base oil containing single MoDTC, both the diameter and
surface roughness of wear track presented in Figs. 12(b)–12(d)
decrease. In addition, the worn surface is relatively smoother
when lubricated by a higher MoDTC content. Furthermore, the
combined effect of detergent and MoDTC on anti-wear can also
be reflected in Figs. 12( f )–12(h). It can be easily observed that
the diameter of the wear scar of the base oil containing three deter-
gents and MoDTC is significantly less than that of the base oil con-
taining single MoDTC, as well as fewer furrows and scratches.
Apparently, the synergistic use of detergent and MoDTC results
in significantly shallower wear scars with substantially smaller
wear areas than those balls lubricated with single additive. The
above results clearly confirm the compounding effect of detergent
and MoDTC on the anti-wear performance.
Figure 13 shows the SEM images of the worn ball surfaces after
the four-ball test. When lubricated by the base oil, the wear scar dia-
meter and depth of the ball are large and deep (Fig. 13(a)). Such
evident surface damage indicates the inadequate lubrication and
severe wear during the sliding test (Fig. 6). When MoDTC is
added into the base oil, the WSD of the ball is substantially
decreased (Figs. 13(b)–13(e)), it is considered that the generation
of MoS2 film can avoid the wear between directly contact surfaces.
When detergent is added into Oil 4, there is an obvious further
decrease in the WSD of the balls. For the higher magnification of
the worn ball lubricated by the base oil, there are many scratches
Fig. 14 EDS spectra of wear scars on the test balls lubricated with (a) Oil 2 and (b) Oil 7 after four-ball test
122201-8 / Vol. 142, DECEMBER 2020
and deep furrows in the wear scar, while the wear scars of the
balls lubricated by MoDTC are similar, but only minor pits and
light furrows are observed (Figs. 13(b)–13(d )). Furthermore, the
surfaces lubricated by detergents are considerably smoother
(Figs. 13(e)–13(h)). These results demonstrate that the synthesized
MoDTC can improve the anti-wear property by a combination of
detergents. The reason is that the nano-calcium sulfonate micelles
are adsorbed on the metal surface, and they were crushed and
release calcium carbonate by sliding friction. Finally, a calcium car-
bonate film is generated under high-temperature and high-pressure
conditions and enhances the anti-wear performance.
To verify the mechanism of the tribochemistry film on the steel
ball surface lubricated with the addition of MoDTC and T106, the
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EDS results of the worn surfaces are shown in Fig. 14. From
Fig. 14(a), the peak of Mo on the wear scar surface can be found
when lubricated with MoDTC. In addition, there exist some film
on the wear track based on the SEM image (Fig. 13(b)), which is
attributed to the tribochemical reaction and the elements of Mo
and S indicate there might be the existence of the MoS2 tribo-film
[41,42]. However, the presence of a Ca peak might be a sign of
CaCO3 (Fig. 14(b)), which suggests that MoDTC and T106
undergo chemical reactions and the generation of the tribochemistry
films [43].
To explore the lubrication behavior of the base oil containing dif-
ferent additives, the wear scars were analyzed by EDS after the
four-ball test, and the element contents are summarized and
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 Table 4 Element contents of steel ball wear scar lubricated by different oils (wt%)

Oil code C O Si Cr Fe Mo S Ca

Base oil Oil 1.0 4.23 5.04 0.42 1.20 89.11 – – –

Single detergent Oil 1.1 6.38 3.48 0.34 0.81 88.76 – – 0.23
Oil 1.2 5.84 5.37 0.32 0.91 85.31 – – 2.25
Oil 1.3 7.09 8.58 0.23 1.23 80.83 – – 2.04
Single MoDTC Oil 2 5.42 3.82 0.25 1.38 86.35 1.86 0.92 –
Oil 3 5.34 3.75 0.36 1.33 86.28 1.96 0.98 –
Oil 4 5.41 3.15 0.25 1.20 87.09 2.04 0.86 –
Oil 5 5.45 3.48 0.29 1.31 86.4 2.06 1.01 –
MoDTC + detergent

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Oil 6 5.92 3.81 0.13 1.18 86.26 1.32 0.65 0.73
Oil 7 3.19 4.7 0.38 1.12 85.47 2.43 1.2 1.51
Oil 8 4.10 5.40 0.34 1.20 84.64 1.86 0.74 1.72

presented in Table 4. As shown in Table 4, the elements of Mo, S, Acknowledgment

and Ca are detected on the wear scars of the test balls, and this
reveals that the additives undergo tribochemical reactions on the
steel ball surface during the friction process and that a transfer
film is formed to protect the friction surface.
For the base oil containing a single metal detergent, only the
characteristic element of Ca can be found, indicating that calcium
salts in the detergent can form CaCO3 deposition film on the friction
surface. Mo and S are found when only MoDTC is added into the
base oil, it can be speculated that MoDTC can promote the forma-
tion of MoS2 transfer film. In addition, with the increase in MoDTC
content in the base oil, the contents of Mo and S also show an
increasing trend, indicating that a thicker or more uniform MoS2
film forms at higher MoDTC contents and enhance the lubrication
performance. Furthermore, when MoDTC and detergent are added
into the base oil, the presence of Mo, S, and Ca reveals that the com-
position of the transfer film contains MoS2 and CaCO3. Therefore,
compound additives have better tribological properties when com-
pared with those of a single additive.
4 Conclusions
In this study, the thermal stability and detergency performance of
detergents with different base numbers were analyzed, and the influ-
ence of MoDTC content on the tribological properties and the
synergistic tribological effects between MoDTC and detergent
were measured. Based on the above results and discussion, the fol-
lowing conclusions were drawn:
(a) The high-based synthetic calcium sulfonate (T106) pos-
sessed an excellent thermal stability and detergency perfor-
mance when compared with that of the low-based synthetic
calcium sulfonate (T104) and middle-based calcium alkyl
salicylate (T109). With increasing MoDTC content, the fric-
tion coefficient and wear volume of the test ball tended to
decline first and then increase. With a MoDTC content of
0.75%, the base oil with MoDTC had a remarkable anti-wear
performance.
(b) The friction coefficients of T104 and T109 gradually
increased, while that of T106 obviously declined with the
increase in temperature, and the friction coefficient of T106
was lower than that of T104 and T109 at temperatures over
70 °C. For the anti-wear performance, T106 showed a
remarkable anti-wear performance compared with that of
MoDTC, and the order of anti-wear performance is: T106,
T109, and T104.
(c) The EDS spectral analysis results indicated that the decom-
posed T106 and MoDTC adsorbed on the worn surface.
The Mo in MoDTC generated MoS2 tribological films, and
the CaCO3 protection film was generated due to calcium
nano-sulfonate, both of which contributed to the enhance-
ment of anti-wear performance.
The authors would like to thank the National Natural Science
Foundation of China (No. 51605381), National Key R&D
Program of China (No. 2017YFB0306700), Project of Panzhihua
Science and Technology (No. 2018CY-G-8), and Key Research
and Development Project of Shaanxi Province (Grant No.
2018ZDXM-GY-074).
Conflict of Interest
There are no conflicts of interest.
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