Tribology Transactions

ISSN: 1040-2004 (Print) 1547-397X (Online) Journal homepage: http://www.tandfonline.com/loi/utrb20

Influence of Polyfluo-Wax on the Friction and Wear

Behavior of Polyimide/Epoxy Resin–Molybdenum
Disulfide Bonded Solid Lubricant Coating

Hongqi Wan, Yinping Ye, Lei Chen, Jianmin Chen & Huidi Zhou

To cite this article: Hongqi Wan, Yinping Ye, Lei Chen, Jianmin Chen & Huidi Zhou
(2016) Influence of Polyfluo-Wax on the Friction and Wear Behavior of Polyimide/Epoxy
Resin–Molybdenum Disulfide Bonded Solid Lubricant Coating, Tribology Transactions, 59:5,
889-895, DOI: 10.1080/10402004.2015.1118585

To link to this article: https://doi.org/10.1080/10402004.2015.1118585

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Nov 2015.
Published online: 24 Jun 2016.

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TRIBOLOGY TRANSACTIONS
2016, VOL. 59, NO. 5, 889–895
http://dx.doi.org/10.1080/10402004.2015.1118585

Influence of Polyfluo-Wax on the Friction and Wear Behavior of Polyimide/Epoxy

Resin–Molybdenum Disulfide Bonded Solid Lubricant Coating
Hongqi Wan, Yinping Ye, Lei Chen, Jianmin Chen, and Huidi Zhou
State Key Laboratory of Solid Lubrication, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou, P. R. China

ABSTRACT ARTICLE HISTORY

Polyimide/Epoxy resin–molybdenum disulfide bonded solid lubricant coatings (denoted as PI/EP-MoS2) Received 28 July 2015
were prepared. The influence of polyfluo-wax (denoted as PFW) on the microhardness and friction and Accepted 6 November 2015
wear behavior of as-prepared PI/EP-MoS2 lubricant coating was measured using a microhardness tester KEYWORDS
and a reciprocating ball-on-disc tribometer, respectively. The worn surfaces of the lubricant coatings were Polyimide/epoxy resin;
observed with a scanning electron microscope, and their wear rate was determined with a Micro XAM molybdenum disulfide;
surface mapping microscope. Moreover, the transfer films formed on the counterpart steel ball surfaces bonded solid lubricant
were analyzed by X-ray photoelectron spectroscopy. Results indicate that the incorporation of a proper coating; polyfluo-wax;
content of PFW filler is effective at improving the antifriction performance of the PI/EP-MoS2 lubricant friction and wear behavior
coating while maintaining better wear resistance. Moreover, the friction coefficient of the lubricant
coating decreases with increasing content of PFW from 2 to 10%, and the one with a filler content over 6%
PFW has a steady friction coefficient of 0.07. The improvement in the antifriction performance of the
lubricant coating with the incorporation of the PFW filler is attributed to the excellent lubricity of
homogeneously distributed PFW.

Introduction
Friction and wear may lead to service failure of many assemblies
of engineering components through rapid crack formation and
surface wear. In order to reduce or eliminate damage induced by
friction and wear, engineers usually need to employ a low-fric-
tion lubricant coating to separate the immediate contact between
two solid surfaces (Korsunsky, et al (1); Xu, et al (2), (3); Cao
and Xiao (4)). Bonded solid lubricant coating is one of the main
types of solid lubricating materials and is applicable to mitigating
wear, adhesion, and scuffing of mechanical parts whose effective
lubrication cannot be ensured by fluid lubricants (Johnson and
Wilson (5); Gamulya, et al (6); Carton, et al (7); Tian, et al (8);
Zhang, et al (9)), thereby ensuring the stability and dependability
of the mechanisms. Compared to film deposition techniques
such as vacuum evaporation, sputtering, and thermal spraying,
the technique for fabricating bonded solid lubricant coating is
more economic and facile, which accounts for its rapid develop-
ment and broadened application in dry lubricating engineering
(Ye, et al (10), (11); Hiraoka (12); Langlade, et al (13); Liu, et al
(14)). Molybdenum disulfide (MoS2), graphite, and polytetra-
fluoroethylene (PTFE) are the three most commonly used solid
lubricants in bonded solid lubricant coating (Guu and Lin (15)).
In particular, the bonded solid lubricant coating containing
MoS2 as the solid lubricant has been extensively applied in
industry, due to its high load-carrying capability and excellent
antifriction performance (Beall (16); Hiraoka and Sadaki (17);
Luo, et al (18), (19); Lince (20)).
A perfect bonded solid lubricant coating would possess
higher wear resistance and a lower friction coefficient. Great
efforts have been made by many researchers to improve the
wear resistance of the various bonded MoS2 solid lubricant
coatings. Tian, et al (8) reported that Fe3O4 nanoparticles can
significantly improve the wear resistance of epoxy-bonded
composite coatings. Ye, et al (10), (21) and Yu, et al (22) sepa-
rately reported that nanosized LaF3 and microsized rare earth
trifluorides can improve the wear resistance and corrosion
resistance of bonded solid lubricant coating containing MoS2
solid lubricant. The incorporation of nanoparticles would
enhance the filling densification of the bonded solid lubricant
coatings, though it is ineffective in reducing the friction coeffi-
cient of the lubricant coatings (Ye, et al (10)). These research
works are of special significance for the development of high-
performance bonded solid lubricant coatings with higher wear
resistance. However, the improvement in antifriction perfor-
mance is still a challenge for bonded solid MoS2 lubricant coat-
ings, and few reports are currently available.
Polyfluo-wax (PFW), a specially formulated mixture of
PTFE and polyethylene, exhibits excellent self-lubricating
capacity, and as a solid lubricant it is superior to PTFE
(Song and Zhang (23); Guo, et al (24)). During our prelimi-
nary work, the Polyimide/Epoxy resin–PFW bonded solid
lubricant coating, when evaluated using a reciprocating ball-
on-disc tribometer (load 20 N, sliding speed 0.48 m/s),
achieves a lower friction coefficient (0.06) than that of the

CONTACT Hongqi Wan wanhq@licp.cas.cn; Lei Chen chenlei@licp.cas.cn

Color versions of one or more of the figures in this article can be found online at www.tandfonline.com/utrb.
Review led by Thierry Blanchet
© 2016 Society of Tribologists and Lubrication Engineers
890 H. WAN ET AL.
lubricant coating containing MoS2 (0.11), but the wear rate
of the Polyimide/Epoxy resin–PFW lubricant coating is
much higher than that of the lubricant coating containing
MoS2. Enlightened by this finding, in the present research
we incorporate PFW into a Polyimide/Epoxy resin–MoS2-
bonded solid lubricant coating, hoping to obtain a novel
bonded solid lubricant coating with greatly improved wear
resistance and antifriction performance. This article reports
the preparation of the Polyimide/Epoxy resin–MoS2-bonded
solid lubricant coating as well as the evaluation of their fric-
tion and wear behavior in association with structural
characterization.
Experiments
Materials
Polyamide acid was purchased from Beijing Sino-Rich Com-
pany Ltd. (Beijing, China, mass fraction: 33%). Epoxy resin
(commercial code: AG-80) was provided by Shanghai Research
Institute of Synthetic Resins (Shanghai, China). MoS2 with an
average diameter of less than 5 mm was supplied by Dandong
Yalu Lubricating Material Company Ltd. (Dandong, China).
Polyfluo 150 wax with a diameter of approximately 3–4 mm
was provided by Micropowder Company (New York). A mix-
ture of N-methylpyrrolidone and N,N-dimethylformamide
(volume fraction: 1:1) was employed as the solvent. AISI-1045
steel (12.7 mm £ 12.7 mm £ 19 mm, 28–32 HRC, Ra D
0.05 mm, E D 210 £ 103 MPa) was used as the substrate to pre-
pare Polyimide/Epoxy resin–molybdenum disulfide–bonded
solid lubricant coating, and a GCr15 bearing steel ball
( ; 12 mm, 58–61 HRC, Ra D 0.02 mm, E D 208 £ 103 MPa)
was used as the counterpart material of the lubricant coating.
The chemical composition of the AISI 1045 steel and GCr15
bearing steel is shown in Table 1.
Preparation of PI/EP-MoS2-bonded solid lubricant coating
AISI-1045 steel substrate (12.7 mm £ 19 mm) was rough-
ened by sandblasting to a surface roughness (Ra) of 2.00 §
0.20 mm in order to improve the bond strength between the
lubricant coating and the substrate (prior to lubricant coat-
ings preparation, the roughened steel substrate was cleaned
with acetone in an ultrasonic bath for 10 min). Polyamide
acid (18.6 g, mass fraction: 33%), epoxy resin (1.6 g), and
PFW (1.2 g) were dispersed in the mixed solvent of N-meth-
ylpyrrolidone and N,N-dimethylformamide (20 ml) by
mechanical stirring in association with ultrasonic vibration
to achieve a homogeneous dispersion. MoS2 (11.0 g) was
then added to the resultant dispersion and dispersed in the
Table 1. Chemical composition of AISI 1045 steel and GCr15 bearing steel.
Steel C Si Mn
AISI 1045 steel 0.42–0.50 0.17–0.37 0.50–0.80
GCr15 bearing steel 0.90–1.05 0.10–0.35 0.25–0.45
same mixed solvent (20 ml) by 48 h of mechanical ball mill-
ing under vigorous stirring. The solid content of the final
mixed dispersion was adjusted to 20% by introducing a
proper amount of the mixed solvent. The mixture was
sprayed onto the surface of the steel substrate using a spray
gun under 0.2 MPa of nitrogen gas, and the final PI/EP-
MoS2-bonded solid lubricant coating filled with 6% PFW
was obtained after solvent evaporation in combination with
curing at 150 C for 0.5 h and at 170 C for 1 h. In order to
discuss the role of PFW in the lubricant coating, other target
products with respect to different concentrations of PFW
were produced in the same manner as above; the mass frac-
tions of PFW in the cured coatings were fixed at 0, 2, 4, 6, 8,
and 10%, respectively, and the thickness of the coatings,
measured with a coating thickness gauge, was 25–30 mm.
Friction and wear test
A commercial reciprocating ball-on-disc tribometer was employed
to evaluate the friction and wear behavior of the PI/EP-MoS2-
bonded solid lubricant coatings under dry sliding conditions, in
which the GCr15 bearing steel ball reciprocally slid against the
coatings at an amplitude of 2 mm, a normal load from 10 to 30 N,
a sliding speed from 0.16 to 0.80 m/s, and a sliding time of 60 min.
Before each test, the steel ball was cleaned with acetone and dried
in air. The wear volume of the bonded solid lubricant coatings was
measured with a surface mapping microscope, and the wear vol-
ume loss was converted into the wear rate (unit: mm3/(N¢m)) after
dividing by the sliding distance and applied load. All friction and
wear tests were run at an ambient temperature of 20–30 C and rel-
ative humidity of 40–50%; three repeat measurements were con-
ducted under each preselected test condition. The average of the
repeat tests is reported in this article.
Characterization
The microhardness of the lubricant coatings was measured
using an MH-5-VM type microhardness tester (25 g, 5 s), and
each sample was measured six times and averaged. The worn
surfaces of the PI/EP-MoS2-bonded solid lubricant coatings
were observed with a JEM-1200EX model scanning electron
microscope. A PHI-5702 multifunctional X-ray photoelectron
spectroscope (XPS; monochromated Al Ka irradiation, pass
energy 29.4 eV) was used to determine the chemical states of
the transfer film formed on the surface of the counterpart steel
ball. The binding energy of the core levels was calibrated
against the binding energy of contaminated carbon (C1s: 284.8
eV) and recorded at an accuracy of §0.2 eV.
Composition (mass fraction, %)
P S Cr Ni Cu Fe
0.035 0.035 0.25 0.25 0.25 Balance
0.0025 0.0025 1.40–1.65 — — Balance

Figure 1. SEM morphologies of the PI/EP-MoS2-bonded solid lubricant coating filled with 6% PFW: (a) surface of the lubricant coating, (b) cross section of the lubricant
coating, and (c) X-ray map of F element distribution in the lubricant coating.
Results and discussion
Microstructure and microhardness of the PI/EP-Mos2
lubricant coating
Figure 1 shows the scanning electron microscopy (SEM) mor-
phologies of the PI/EP-MoS2-bonded solid lubricant coating
filled with 6% PFW. It is seen that the lubricant coating is uni-
form and seems to contain few cavities (Fig. 1a). In the mean-
time, the lubricant coating is well bonded with the steel
substrate (Fig. 1b), and its thickness is about 30 mm. Moreover,
F element is uniformly distributed on the lubricant coating sur-
face (Fig. 1c), which is attributed to the good dispersion of
PFW in the lubricant coating and should be favorable for
acquiring good tribological performance.
Figure 2 shows the microhardness of the PI/EP-MoS2-
bonded solid lubricant coating as a function of PFW content. It
can be seen that the microhardness of the lubricant coating
without PFW is 364 MPa (25 g, 5 s) and decreases slowly with
increasing content of PFW from 2 to 6% and then decreases
quickly with a further increase in PFW content above 6%. This
is because PFW usually exhibits poor bonding to polymer
binder, and the incorporation of PFW filler would weaken the
Figure 2. Microhardness of the PI/EP-MoS2-bonded solid lubricant coating as a
function of PFW content (25 g, 5 s).
TRIBOLOGY TRANSACTIONS 891
interfacial adhesion of the lubricant coating. As a result, the
microhardness decreases with an increase in PFW content.
Friction and wear behavior
Figure 3 shows the friction coefficient and wear rate of the PI/
EP-MoS2-bonded solid lubricant coatings as functions of PFW
content. It can be seen that the lubricant coating without PFW
exhibits a friction coefficient of 0.11, and the one filled with 6%
PFW has a decreased friction coefficient of 0.07. In addition,
the friction coefficient of the lubricant coatings decreases rap-
idly with increasing content of PFW from 2 to 6% and then sta-
bilizes with a further increase in PFW content above 6%. This
implies that the self-lubricating capability of PFW is exerted to
the maximum degree when its dosage in the bonded solid lubri-
cant coatings is adjusted at 6%. Furthermore, the wear rate of
the PI/EP-MoS2 lubricant coatings remains nearly unchanged
when the content of PFW is less than 6%. The reason should be
the interaction of the increased lubricating capacity and
decreased microhardness of the lubricant coating, which would
lead to a balance of the wear rate. The wear rate of the coating
increases substantially when the content of PFW is more than
Figure 3. Friction coefficient and wear rate of the PI/EP-MoS2-bonded solid lubri-
cant coatings as a function of PFW content (sliding speed 0.48 m/s, load 20 N, slid-
ing time 60 min).
892 H. WAN ET AL.
Figure 4. Friction coefficient of the PI/EP-MoS2-bonded solid lubricant coatings
filled with 6% PFW as a function of sliding time.
6%. This is caused by the sharp decrease in microhardness of
the lubricant coating, which would lead to serious abrasion.
These friction and wear test data indicate that PFW is effective
in improving the antifriction performance of the PI/EP-MoS2-
bonded solid lubricant coating (the optimal content of PFW in
the film is suggested to be 6%), but it is unable to improve the
wear resistance of the lubricant coating.
Figure 4 shows the friction coefficient of the lubricant coat-
ings filled with 6% PFW as a function of sliding time (load 20
or 30 N, sliding speed 0.48 or 0.80 m/s). These are typical
curves of the variation in friction coefficient with sliding time
for this material. It can be seen that the friction coefficient
curves contain two stages: a running-in stage and steady-state
stage. In the running-in stage, the friction coefficient gradually
increases and then decreases rapidly with increasing sliding
time. The variation in the friction coefficient is caused by the
uneven surface of the lubricant coating. However, the uneven
surface can be smoothed quickly along with the friction, and
then the friction coefficient decreases subsequently to a steady
state at about 8 min. At a load of 30 N and sliding speed of 0.48
m/s, the mean friction coefficient of the lubricant coating is
0.06, and the mean friction coefficient of the lubricant coating
declines to 0.05 at a load of 20 N and sliding speed of 0.80 m/s.
On the basis of the experimental results, we can conclude that
the PI/EP-MoS2-bonded solid lubricant coating would exhibit
Figure 5. Friction coefficient and wear rate of the PI/EP-MoS2-bonded solid lubricant coatings as a function of applied load at a sliding speed of 0.48 m/s (sliding
time 60 min).
excellent tribological performance under these experiment
conditions.
Figure 5 shows the friction coefficient and wear rate of the lubri-
cant coatings as a function of applied load from 10 to 30 N (sliding
speed 0.48 m/s, sliding time 60 min). It can be seen that the friction
coefficient of the lubricant coatings decreases rapidly with an
increase in applied load (Fig. 5a), which can be explained by Bow-
den’s friction theory (Bowden and Tabor (25)). The friction coeffi-
cient may be expressed in terms of m D Ars/N (where Ar is the real
contact area, which is directly proportional to the friction force, s is
the shear strength, and N is the applied load). The real contact area
between the lubricant coating and the steel ball increases with an
increase in applied load, whereas the increasing extent of the real
contact area is much less than that of the applied load. As a result,
the friction coefficient decreases rapidly with an increase in applied
load. This result is consistent with the finding of Ye, et al (10). In
addition, the lubricant coating filled with 6% PFW exhibits a lower
friction coefficient than the lubricant coating without PFW under
the same testing condition, which is attributed to the excellent
lubricity of homogeneously distributed PFW. Moreover, the wear
rate of the lubricant coatings decreases rapidly with an increase in
applied load, but the wear rate of the lubricant coating filled with
6% PFW is close to that of the lubricant coating without PFW
(Fig. 5b).
Figure 6 shows the friction coefficient and wear rate of the lubri-
cant coatings as a function of sliding speed at a load of 20 N. It can
be seen that the friction coefficient and wear rate of the lubricant
coatings decrease rapidly with an increase in sliding speed, and a
decrease in the friction coefficient is due to the decrease in real con-
tact area with an increase in sliding speed (Jin (26)). In addition,
the lubricant coating filled with 6% PFW exhibits a lower friction
coefficient than the lubricant coating without PFW within a range
of sliding speed from 0.16 to 0.80 m/s, but the wear rate of the two
kinds of lubricant coatings is virtually the same under varying slid-
ing speed. This again demonstrates that the incorporation of a
proper content of PFW filler is effective in improving the antifric-
tion performance of the lubricant coating in maintaining better
wear resistance.
XPS analysis of the worn surface of counterpart steel ball
The friction and wear behavior of lubricant coatings is strongly
influenced by their ability to form a transfer film on the counter-
part surface (Fayeulle, et al (27), (28); Bahadur and Tabor (29)).

Figure 6. Friction coefficient and wear rate of the PI/EP-MoS2-bonded solid lubricant coatings as a function of sliding speed at a load of 20 N (sliding time 60 min).
In order to further study the friction and wear mechanism of the
PI/EP-MoS2 lubricant coating, we conducted XPS analysis of the
transfer films on the counterpart steel ball surfaces. The XPS
spectra of some typical elements are given in Fig. 7 (load 30 N,
sliding speed 0.80 m/s, sliding time 60 min), and the binding
energies from these plots were compared to the data listed in the
Handbook of X-ray Photoelectron Spectroscopy (Wagner, et al
(30)). It can be seen that the transfer film of lubricant coating
filled with 6% PFW shows a peak at 689.1 eV attributied to the
F1s of PFW and the peaks at 229.7 eV and 162.5 eV assigned to
Mo3d5/2 and S2p of MoS2, respectively. In the N1s spectrum, the
peak at 399.5 eV is assigned to the N in imide groups. Unsur-
prisingly, the transfer film of the lubricant coating without PFW
shows all of the above-mentioned peaks except for the peak of
F1s. These results indicate that the chemical composition of the
lubricant coating has not been changed during the friction
Figure 7. XPS spectra of the transfer films on the counterpart steel ball surfaces (load 30 N, sliding speed 0.80 m/s, sliding time 60 min): (a) F1s, (b) Mo3d5/2, (c) S2p, and
(d) N1s.
TRIBOLOGY TRANSACTIONS 893
process, and all of the composition of the lubricant coating can
be transferred onto the surface of the counterpart steel ball to
form a transfer film, thereby preventing direct contact between
the lubricant coating and the counterpart steel ball and improv-
ing the tribological properties of the lubricant coating.
SEM analysis of the worn surfaces of PI/EP-Mos2 lubricant
coatings
Figure 8 shows the SEM morphologies of the worn surfaces of
the PI/EP-MoS2-bonded solid lubricant coatings filled with and
without PFW (sliding speed 0.48 m/s, load 20 N, sliding time 60
min). It can be seen that the worn surfaces of the lubricant coat-
ings filled with 6% PFW and without PFW are intact and do not
show signs of holes and cracks (Figs. 8a and 8b), which agrees
well with their good wear resistance. However, the worn surface
894 H. WAN ET AL.

Figure 8. SEM morphologies of the worn surfaces of the PI/EP-MoS2-bonded solid lubricant coatings (sliding speed 0.48 m/s, load 20 N, sliding time 60 min): (a) without
PFW, (b) with 6% PFW, and (c) with 10% PFW.

Figure 9. SEM morphologies of the worn surfaces of the PI/EP-MoS2-bonded solid lubricant coating filled with 6% PFW under different loads and speeds: (a) 10 N and
0.48 m/s, (b) 15 N and 0.48 m/s, (c) 30 N and 0.48 m/s, (d) 20 N and 0.32 m/s, (e) 20 N and 0.64 m/s, and (f) 20 N and 0.80 m/s.

of the lubricant coating filled with 10% PFW shows signs of
holes and cracks and severe wear (Fig. 8c), which corresponds to
the observation that the lubricant coating filled with 10% PFW
has worse wear resistance than the one filled with 6% PFW. This
could be because excessive PFW weakens the interfacial adhesion
between the solid lubricant and binder of the lubricant coating.
As a result, the lubricant coating with a content of PFW filler
that is too high (e.g., 10%) exhibits a worse wear resistance.
The PI/EP-MoS2-bonded solid lubricant coating filled with
6% PFW was selected as an example to investigate the wear
mechanism. As shown in Fig. 9, scratches along the sliding
direction are formed on the worn surface of the lubricant coat-
ing after sliding at a low applied load and speed (Figs. 9a, 9b,
and 9d). With an increase in applied load, the morphology of
the worn surface of the lubricant coating does not exhibit
disparity (Fig. 9c). However, with an increase in sliding speed,
cracks occur on the worn surface of the lubricant coating
(Fig. 9e) and become serious at a sliding speed of 0.80 m/s
(Fig. 9f). The occurrence and expansion of cracks could lead
the lubricant coating to fracture and resut in increased wear.
These results indicate that the wear mechanism of the lubricant
coating is governed by fatigue wear.
Conclusions
Polyimide/Epoxy resin–molybdenum disulfide–bonded solid
lubricant coatings were prepared, and the effect of polyfluo-
wax on the friction and wear behavior of the PI/EP-MoS2
lubricant coatings was investigated. Results indicate that the
incorporation of PFW filler of less than 6% is able to improve

the antifriction performance of the lubricant coating in main-
taining better wear resistance. When the content of PFW is
more than 6%, the antifriction performance of the lubricant
coating does not increase further, whereas the wear resistance
decreases quickly caused by the sharp decrease in microhard-
ness. The lubricant coating filled with 6% PFW exhibits a lower
friction coefficient and comparable wear resistance compared
to the lubricant coating without PFW filler within a load range
between 10 and 30 N and within a sliding speed range from
0.16 to 0.80 m/s. Moreover, the wear mechanism of the lubri-
cant coating filled with 6% PFW is dominated by fatigue wear.
The improvement in the antifriction performance of the lubri-
cant coating by the incorporation of the PFW filler is attributed
to the excellent lubricity of homogeneously distributed PFW.
Funding
The authors are grateful to the National Natural Science Foundation of
China for financial support (Grant Nos. 51305430 and 51175491).
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