Wear 360-361 (2016) 87–96

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Wear
journal homepage: www.elsevier.com/locate/wear

Role of treatment to graphite particles to increase the thermal

conductivity in controlling tribo-performance of polymer composites
Jitendra Narayan Panda a, Jayashree Bijwe a,n, Raj K. Pandey b
a
Industrial Tribology Machine Dynamics and Maintenance Engineering Centre, Indian Institute of Technology Delhi, Hauz Khas, New Delhi 110016, India
b
Mech. Engineering Department Indian Institute of Technology Delhi, Hauz Khas, New Delhi 110016, India

art ic l e i nf o a b s t r a c t

Article history: A novel type of graphite (thermographite) having higher thermal conductivity (TC) due to a patented
Received 5 January 2016 treatment is commercialized recently. It was anticipated that such particles would be more effective in
Received in revised form conducting away frictional heat generated on the tribo-surfaces leading to the enhanced performance.
15 April 2016
Hence two composites were developed based on high performance Polyarylether ketone (PAEK) (50% by
Accepted 16 April 2016
wt) containing 30% short glass fibers (GF) and hexa-boron nitride (hBN) 10% apart from 10% graphite.
Available online 22 April 2016
First composite designated as CNG contained 10% natural graphite (NG) while the other designated as CTG
Keywords: contained 10% thermographite (TG). These were processed by identical method (twin screw extrusion
PAEK followed by injection molding). The tribo-performance was evaluated in a pin on disc (mild steel)
Polymer composite
configuration under very high load and speeds. It was observed that both the composites exhibited
Tribology
excellent tribo-performance. However, CNG performed better than the CTG in all respects only under
Natural graphite
Thermo-graphite severe operating conditions. Under low PV conditions, difference was not clear. It showed lower friction
coefficient, and wear rate as compared to CTG. CNG showed PVlimit value 96.6 MPa-m/s which was deci-
sively superior to CTG (91 MPa-m/s). CNG could sustain higher speed (3.45 m/s) than the CTG (3.25 m/s)
under 900 N in spite of slightly lower TC. It was concluded that during treatment (patented by the
company) TG has slightly distorted layer-lattice structure as compared to the natural graphite, which
could be responsible for transferring less beneficial film under severe operating conditions. SEM and
EDAX studies were conducted to understand wear mechanisms. Such composites with such high PVlimit
values low, m (0.04) and low wear rates (1
10  16 m3/Nm) are not reported in the literature and may
prove as ideal materials for dry bearings in harsh operative conditions.
& 2016 Elsevier B.V. All rights reserved.

1. Introduction the situation is extremely challenging since thermal stability and

When a tribo-couple slides against each other, frictional heat
generated due to frictional torque, is a function mainly of friction
coefficient (m) and PV condition where V is sliding speed and P is
pressure. The frictional heat is responsible for drastic changes in
friction and wear mechanism and hence tribo-performance. It is
dissipated to the environment by conduction, convection and
radiation which, depends mainly on the temperature difference
between tribo-couple and ambience apart from various thermo-
physical properties of both the surfaces such as specific heat,
thermal conductivity (TC), diffusivity (TD) etc. Higher TC and TD
enhance the heat flow from the tribo-surface and hence minimize
the damage to the surface, as observed typically in the case of
metal sliding against metal. In the case of polymer against metal,
n
Corresponding author. Tel.: þ 91 11 26591280.
E-mail address: jbijwe@gmail.com (J. Bijwe).
TC of polymers are very low resulting in excessive accumulation of
heat on the surface leading to various phenomena occurring in
successive steps such as loss in strength, thermal degradation and
melting of the polymeric surface.
The polymers, though are known as a special class of tribo-
materials because of very low m against metals in dry condition,
very good resistance to wear, corrosion and impact (leading to
damping property and hence quiet operation), very high specific
strength etc. [1–15]; suffer serious limitations such as low
thermal and thermo-oxidative stability, low TC and strength etc.
The strength can be enhanced to some extent by fiber reinfor-
cement, while issue of thermal stability can be addressed to
some extent by selecting high performance specialty polymers
such as PEKs (polyether–ketones), Polyimides (PIs) etc. The
issue of low TC can be handled by incorporating appropriate
fillers having higher TC. Hence, while selecting solid lubricants
such as PTFE (Poly tetrafluoroethylene), hBN (hexa boron

http://dx.doi.org/10.1016/j.wear.2016.04.018
0043-1648/& 2016 Elsevier B.V. All rights reserved.
88 J.N. Panda et al. / Wear 360-361 (2016) 87–96

nitride), graphite, MoS2 (Molybdenum di sulfide), WS 2 (Tung-
sten di sulphide) etc., preference is also given to the SLs such as
hexa-boron nitride (hBN) and graphite having higher TC. Table 1
shows some data on the most popular SLs [16–19].
Sometimes, efforts are made to increase the TC of the typical
ingredients/SLs by various treatments or coating for commercial
materials. Most of the times, such treatments are proprietary
[20,21]. It is expected that enhanced TC of a selected filler/fiber/SL
will improve the tribo-performance due to more heat exaction
from the tribo-surface. The efficiency of such techniques will be
reflected clearly in more severe conditions rather than mild
operating conditions of P and V. However, it has to be investigated
in details.
Thermo-graphite (TG) from Imerys Graphite & Carbon Ltd.
Switzerland is the latest addition of SL, with increased TC [22]. The
same TG when used in brake–pad materials (multi-ingredient
system) led to superior performance properties as compared to
natural graphite [23]. In our earlier work [24] on exploring
synergism between two solid lubricants, we had also reported
about the two composites differing in types of graphite viz. NG and
TG on tribo-properties in mild operating conditions. However, the
difference in performance was not clearly visible (Fig. 1(a) and (b))
[24] and the surface topography observed by SEM (Fig. 1(c) and
(d)) was also almost identical confirming that the potential of the
Table 1
Characteristic properties of high performance solid lubricants [16–19].
Material h-BN Graphite
Density (g/cm )3
 2.1  2.1
Bulk modulus (GPa) 36.5 34
Thermo- oxidative stability(°C) 1000 570
Thermal conductivity (W/m K) 600║; 30┴ 200–2000║; 2–800┴
Thermal expansion (10  6/°C)  2.7║; 38┴  1.5║; 25┴
Specific heat capacity(J/kg K) 710–830 840–1610
*║- parallel to planes/layers; ┴ perpendicular to planes
TG or NG could not be clearly reflected under selected PV (35.2–
44.8 MPa m/s) conditions. Hence, in this paper we have reported
on the performance of the two composites based on variation of
graphite under high PV conditions expecting that heat exaction
capability of TG will lead to better performance. The paper thus
has following objectives. The present paper thus had following
themes.
To develop more efficient tribo-composites, which could
show very good potential in adverse operating conditions of high
pressure and high speed and can be recommended for dry bearing
material.
To examine which factor (enhanced TC of graphite particles or
changes in their layer lattice structure) is dominant for controlling
tribo-performance.
Based on these, two composites differing in nature of graphite
particles were developed and investigated in details for perfor-
mance. The details are presented in subsequent sections.
2. Experimental details
2.1. Materials selection
Polyether ketone (PAEK) (Grade G-PAEK 1100P) was supplied
by Gharda Chemicals Ltd., Mumbai and properties are shown in
Table 1 [26]. Short fibers of glass (average diameter of 10 mm and
length of 3–4 mm) procured from Nippon Electric Glass (Malaysia)
were selected as a reinforcement (30% w).
PTFE
Micro-sized hBN (density 1.8 g/cc) was procured from Zibo
2.15 Jonye Ceramic Technologies Co., Ltd., China. It had platy crystal
1.8 structure having average particle size distribution between 3 and
260 15 mm (10% w).
0.25
Other solid lubricant (added in 10% by w) was graphite of two
 148
1000 varieties. The first one was natural graphite (NG), procured from a
local supplier with a density of 2.23 g/cc and the second variety of
graphite, designated as thermo-graphite (TG) was procured from

NG
NG 8
TG
0.07 TG
K0*10 -16 (m /Nm )
3

7
μ

0.06
6

0.05 5
700 800 900 700 800 900
Load (N) Load (N)

CNG 900 N CTG 900 N

Sliding direction Sliding direction

20 µm 20 µm
1000x 1000x

Fig. 1. (a) and (b) Friction and wear behavior of CTG and CNG under V 1.6 m/s, 700–900 N; PV -44.8 MPa-m/s ; (c) and (d) SEM of worn surfaces of CNG and CTG under 900 N.
 J.N. Panda et al. / Wear 360-361 (2016) 87–96 89

Imerys Graphite & Carbon Ltd. Switzerland under the trade name
C-Therm 011 in the form of soft granules. TG is characterized by
real density close to the theoretical density of graphite and high
specific surface area (BET- Brunauer–Emmett–Teller-24.3 m2/g) as
an indication of high aspect ratio of graphite particles. Spring-back
value 12.6% provides information regarding the resilience of
compacted graphite powder. It has density (bulk and real 0.15 and
2.24 g/cm3 respectively) and Ash(%)o 2.5. As claimed by the
manufacturer, TG functions by a phonon collision mechanism
(PCM), while metallic powders operate on percolation mechanism.
PCM along with particle morphology aids to meet the TC
requirement at lower additive levels without any abrasion issues.
SEM micrographs of particles of NG and TG are shown in Fig. 2.
Prior to the test, pin was slid against C-1000 emery paper at
low speed (15 mm/s) and low load (10 N) till the surface showed
complete and uniform contact with the counterface. The pin was
then cleaned ultrasonically with petroleum ether followed by
drying, weighing and refitting in the holder in identical position.
Loss in weight was recorded using a weighing balance with an
accuracy of 0.0001 g. In each experiment a new disc was used.
Each experiment was repeated at least three times and average of
two closest reading was considered as a weight loss for that PV
condition. Specific wear rate (K0) and time related depth wear rate
(Wt) [12] of a pin was calculated from the following equations;


K 0 ¼ Δm=ρ L d m3 =Nm ð1Þ

2.2. Development of composites W t ¼ K 0 :  P  V ¼ Δh=t nm=s ð2Þ

It was necessary to mix the solid lubricants (SLs) and PAEK
powder thoroughly and it is reported that probe sonication is
proven to be more efficient method [25]. Hence powders of PAEK
(50% by w), hBN (10%) and graphite (10%) were sonicated using
Chrome Tech probe sonicator with a gradual addition of SLs first,
followed by addition of PAEK powder in sonication medium
(acetone). Sonication was carried out in a step by step process with
pulse duration of 10 min. After sonication the samples were dried
in vacuum oven at 70 °C to remove the acetone. This mixture was
used for further processing during extrusion, followed by injection
molding. Cooperion Twin Screw Extruder ZSK 26 having L/D 40:1
was used and a powdery mixture of PAEK and SLs was fed through
main feeder. Short fibers of glass were fed from the side feeder.
The processing temperature was in the range 380–410 °C. The
specimens of composites for mechanical testing were then injec-
tion molded at 400–420 °C on Arburg 60 t machine.
Thus the two composites designated as CTG and CNG (Table 2)
were developed and characterized for various properties and the
data are collected in Table 2.
2.3. Tribological studies
where, Δm is a weight loss of a pin (kg); ρ is density (kg/m3); L is
load (N) and d is the distance slid in meters. Time related depth
wear rate is a convenient measure for design engineers to estimate
the height/depth loss of under selected PV conditions (assuming
that the wear rate of the steel counterpart is negligible). This can
help to calculate the development of a certain clearance in journal
bearing with time and thus to predict necessary maintenance
intervals in order to prevent catastrophic failure of a part. As per
Eq. (2), the Wt can be considered as a function of the PV factor,
resulting in the tribological parameters for evaluating the load
carrying capacity of bearing materials. Limiting PV (PVlimit) and
maximum safe PV (PVmax-safe) values are derived output para-
meters, which show the critical operating conditions under which
the material fails and below which they can be safely used. This is
achieved either by keeping speed constant and increasing load
gradually or vice- versa. In this work, load was kept highest pos-
sible to the capability of machine (900 N) and speed was varied in
the step till composite shows failure.
Table 2
Data on comparative properties of PAEK [26] and composites.

The composites were evaluated for adhesive wear performance Property PAEKa CNG CTG

as follows. Density in g/cc 1.30 1.62 1.57

Tensile strength (TS) (ASTM D638) (MPa) 105 115 103
2.3.1. Adhesive wear studies Tensile modulus (TM) (ASTM D638) (GPa) 4.2 15.77 20.60
Sliding wear tests in adhesive wear mode were performed using Elongation at break (e) (ASTM D638) (%) 15 1.97 1.63
Flexural strength (FS) (ASTM D790) (MPa) 185 214 170
a pin on disc configuration on a tribometer, supplied by CETR, USA. A
Flexural modulus (FM) (ASTM D790) (GPa) 4.10 13.85 14.12
pin of 6.4 mm in diameter and length 3.4 mm cut from a tensile bar Impact strength (IS)- Notched (ASTM D256) (J/m) 60 39 39
was fitted in a holder and slid against a mild steel disc (C 0.050, Ni Impact strength- Un-notched (ASTM D256) (J/m) No break 349 181
0.005, Co 0.002, P 0.001, Al 0.03 and rest Fe) (Ra 0.1–0.2 μm) under Thermal conductivity (TC) (ASTM D5930)(W/m K) – 1.26 1.52
constant load of 900 N (pressure 28 MPa) and variable speed (1.6– (i) in plane 0.79 0.83
(ii) through plane
3.5 m/s) till the failure of pin was observed. The total sliding distance
of 12 km in each experiment was manipulated with varying time a
Supplier's data [26]; CNG - Composite with natural graphite NG (10 %); CTG -
with speed and was in the range of 2–0.9 h. Composite with Thermo- graphite-TG (10%);

Fig. 2. SEM micrographs of (a) natural graphite (NG) and (b) thermo-graphite (TG).
90 J.N. Panda et al. / Wear 360-361 (2016) 87–96

Failure of the polymeric/composite material sliding under high
PV conditions can be reflected by noticing critical observations.
 Alteration in the disc color.
 Distortion in a pin shape or melting.
 Disproportionate upsurge in temperature of the disc.
 Excessive elevation in the coefficient of friction.
 Extremely high wear rate.
 Excessive noise or vibration.
values (Table 3) since they lost the load bearing capacity and hence
were deformed and extruded in flake form.
Fig. 4 shows variation in μ with sliding time for both the
composites slid under different speeds but under constant load
(900 N). The figure is split in two parts; the first being for low to
medium speeds and second for higher speeds. The left column is
for CNG while right is for CTG. The CTG showed failure earlier than
the CNG and hence some friction data in the last column are
missing. The major observation was about friction fluctuations

2.3.2. SEM (Scanning electron microscopic) and EDAX (Energy dis- Table 3
persive X-Ray analysis) studies Tribo- performance of CNG and CTG in severe operating conditions.
The surfaces of the transfer films of composites were examined
through a scanning electron microscope (SEM, ZEISS, EVO-MA10). PV (MPa m/ K0 x10-16 (m3/Nm) μ
s)/ V (m/s)
In addition, energy dispersive X-ray spectroscopy (EDAX, Brucker)
CNG CTG CNG CTG
was used for determination of the elemental distribution and
contents in the transfer films. 56 (2) 2.832 3.29 0.046 0.049
63 (2.25) 2.602 4.11 0.049 0.050
70 (2.5) 4.013 4.92 0.050 0.051
77(2.75) 6.406 6.18 0.056 0.057
3. Results and discussion 84 (3) 6.009 7.99 0.051 0.054
91 (3.25) 7.6 9.31 0.053 0.071
As seen from Table 2 inclusion of TG instead of NG has led to 95.2 ( 3.4) 5.45 221 0.050 0.136
Excessive wear and friction
decrease in strength properties (TS, FS, IS un-notched) and elonga-
along with deformation
tion while moduli (tensile and flexural) increased. The TC in plane confirmed failure of CTG
and through plane also increased appreciably due to inclusion of TG. 96.6 (3.45) 5.45 – 0.048 –
98 (3.5) 40 – 0.052 –
Failed-excessive
3.1. Tribological studies wear and
deformed
Fig. 3 shows the deformed specimens under typical velocities.
The pins got melted during shearing action under very high PV

Fig. 3. Photographs of failed samples (900 N) showing excessive deformation and extrusion under shearing forces due to excessive melting (a) and (b) For CNG at 3.5 m/s, and
(c) and (d) CTG at 3.4 m/s.
 J.N. Panda et al. / Wear 360-361 (2016) 87–96 91

1000 2000 3000 4000 5000 6000 7000 8000 1000 2000 3000 4000 5000 6000 7000 8000

2.75 (m/s)
0.08

2.75 (m/s)
0.08
CNG CTG
µ 0.04 µ
0.04

0.00 0.00
0.08 0.08

2.5 (m/s)
2.5 (m/s)
µ 0.04 µ
0.04

0.00 0.00

2.25 (m/s)
2.25 (m/s)
0.08 0.08

µ 0.04 µ
0.04

0.00 0.00
0.08 0.08

2 (m/s)
2 (m/s)
µ
µ 0.04 0.04

0.00 0.00
0.08 0.08

1.6 (m/s)
1.6 (m/s)
µ 0.04 µ
0.04

0.00 0.00
1000 2000 3000 4000 5000 6000 7000 8000 1000 2000 3000 4000 5000 6000 7000 8000
T (sec) T (sec)

1000 2000 3000 4000 1000 2000 3000 4000

0.24
3.5 (m/s)

Excessive CNG 28.2

3.5 (m/s)
µ 0.16 increase in µ CTG
18.8
0.08
9.4
0.00 0.0
3.45 (m/s)

0.08
28.2

3.45 (m/s)
µ 18.8
0.04
9.4
0.00 0.0
0.08
3.4 (m/s)

0.32

3.4 (m/s)
Excessive
µ 0.24
0.04 increase in
0.16
0.08 µ
0.00 0.00 increase
0.08
3.25 (m/s)

3.25 (m/s)
0.08
in
µ
0.04 0.04

0.00 0.00
0.08 0.08
3 (m/s)

3 (m/s)
µ
0.04 0.04

0.00 0.00
1000 2000 3000 4000 1000 2000 3000 4000
T (sec) T (sec)

Fig. 4. Variation of μ with sliding time at 900 N of CNG and CTG composites; First part – (a) and (b) for 1.6 m/s; (c) and (d) for 2 m/s; (e) and (f) for 2.25 m/s; (g) and (h) for
2.5 m/s; (i) and (j) for 2.75 m/s; (k) and (l) for 3 m/s ; (m) and (n) for 3.25 m/s ; (o) and (p) for 3.40 m/s ; (q) and (r) for 3.45 and 3.5 m/s (for CNG) respectively.

which were higher for CTG as compared to the CNG. For a good
tribo-material, lower μ with minimum fluctuations is preferred
indicating superiority of CNG over CTG.
Figs. 5(a)–(d) are for friction coefficient and specific wear rates
of composites at various speeds and the data are arranged again in
two parts for each; first being for lower speeds and second for
higher speeds. The μ of both the composites mostly was very low
(0.04–0.07). In the case of CNG, however, μ continued to be around
0.04–0.05 even at very high velocity (3.5 m/s) (Fig. 5b).
For both the composites μ showed maxima at 2.75 m/s fol-
lowed by a decrease for next speed. As PV limit reached, the μ
again increased excessively for CTG but not for CNG. The peak value
of μ at 2.75 m/s speed could be because of rheological changes in
the surface of polymer matrix. It was the stage where polymer was
just softened and not melted resulting in stick–slip problem. Once
the top surface layer got partially melted μ decreased for both.
When melting phenomenon became a bulk phenomenon, failure
of a pin was seen since composite lost its load bearing capacity.
CNG showed lower wear rate than the CTG. For both the com-
posites specific wear rates were very low (2–8
10  16 m3/Nm)
and increased with increase in speed because of higher frictional
torque and hence higher generation of frictional heat leading to
more deterioration in fiber–matrix adhesion and hence fiber – pull
out of peeling off was easier due to shearing forces and hence
more wear. This was observed in SEM studies of the surfaces as
discussed in subsequent sections.
When specific wear rates were compared for CNG at 3.45 m/s and
3.5 m/s, it has increased 8 times indicating failure, though μ was still
very low . Figs. 3(a) and (b) have confirmed the failure of CNG at
3.5 m/s. Similarly when specific wear rates of CTG were compared at
92 J.N. Panda et al. / Wear 360-361 (2016) 87–96

3.25 m/s and 3.4 m/s, wear rate has suddenly increased 25 times
along with excessive increase in μ indicating gross failure. Figs. 3
(c) and (d) have confirmed the failure at 3.4 m/s.
Thus, the overall μ of CTG was higher than the CNG because of
treated graphite (thermo-graphite). Though the technology of
treatment/coating on graphite is patented [21], it appears that gra-
phite is in exfoliated form. The distortion (Fig. 1(b)) in a perfect layer
lattice structure (Fig. 1(a)) along with some coating has resulted in
increased conductivity but at the cost of deterioration in friction
behavior and hence consequently in wear behavior. In literature also
similar behavior is reported for PTFE [27]. Hunke et.al [27] treated
PTFE powder with two types of plasma to grow functional groups on
PTFE and hence to increase its adhesion with polyether sulfone
(PESU) matrix and carbon fibers. The composite with treated parti-
cles led to reduced wear almost by 50% at the cost of increase in m. It
was argued that due to the presence of the functional groups on the
plasma treated PTFE, the thin film formation capability of PTFE was
possibly hindered resulting in high m. Thus, the distortion in typical
chain structure of PTFE or a layer lattice structure of graphite may
lead to deterioration in tribo-properties.
In the present work, it was observed that in spite of increase in
the heat exaction capacity of graphite due to treatment, it could
not lead to better performance than the natural graphite. Finally
contribution due to layer lattice structure in controlling tribo-
performance dominated.
Time related depth wear rates (Wt) against PV is presented in
Fig.6. The composites showed almost linear increase in wear rate
till 91 MPa m/s. At low PV values (i.e., o 77 MPa m/s), the differ-
ence in tribo-performance of composites was not so significant.
However, for higher PV values, it was substantial. When failure
limit approached for CTG (95.5 MPa m/s), Wt increased abruptly to
2103 nm/s from 80 while CNG showed a very low value of 52 nm/s.

PV (MPa m/s) PV (MPa m/s)

56 63 70 77 84 91 95.2 96.6 98
0.075
C NG µ max 0.14
0.070 CTG C NG
0.12 CTG
0.065
P= 28 MPa 0.10 P= 28 MPa
0.060
0.08
µ

µ
0.055 0.06
0.050 0.04
0.045 0.02
0.040 0.00
2 2.25 2.5 2.75 3 3.25 3.40 3.45 3.50
Velocity (m/s) Velocity (m/s)

PV (MPa m/s) PV (MPa m/s)

56 63 70 77 84 91 95.2 96.6 98
10 250
CNG 221
9 CTG 200 CNG
CTG
K0*10-16(m3/Nm)

8 150
K0*10 -16(m3/Nm)

7 P= 28 MPa 100 P= 28 MPa

50 40
6
5 6
4 4
3 2
2 0
2.00 2.25 2.50 2.75 3.00 3.25 3.40 3.45 3.50
Velocity (m/s) Velocity (m/s)
Fig. 5. Coefficient of friction as a function of velocity under constant load 900 N- (a) 1.6 m/s, 2.0 m/s, 2.25 m/s, 2.5 m/s, 2.75 m/s, 3.0 m/s, 3.25 m/s, (b) 3.4 m/s, 3.45 m/s,
3.5 m/s.

100 2500
CNG
CNG 2000
CTG
CTG
1500
80
1000
500
wt (nm/s)
wt (nm/s)

60

40
50
20

0 0
56 63 70 77 84 91 95.5 96.6 98
PV (MPa m/s) PV (MPa m/s)

Fig. 6. (a) and (b) Dependence of time related depth wear rate (Wt) on the PV factor.
 J.N. Panda et al. / Wear 360-361 (2016) 87–96
For CNG, at 98 MPa m/s, enhancement in Wt was nearly eight times
i.e. 400 nm/s than the previous value at 96.6 MPa m/s.
Table 3 compiles the data for both the composites about spe-
cific wear rates and μ at various PV levels. The μ and wear rates of
both in identical conditions for both the composites can be seen.
CNG excelled CTG in all the tribo-features such as μ, wear rate and
PVlimit value. The difference in performance properties of CNG and
CTG composites surfaced out clearly under severe operating con-
ditions. In literature so high values along with low friction and
wear performance are not reported [13–15]. PVsafe value achieved
was 10 MPa m/s (wear rate 4
10  7 mm3/Nm and m 0.1) for PEEK
composite containing short carbon fibers /PTFE/graphite sliding
against steel ring in dry condition [14]. In earlier work in authors'
laboratory [10] on a composite based on blend of PBI and PAEK
containing short carbon fibers/hBN/graphite sliding against mild
steel on the same facility and in similar conditions, PVsafe value of
63 MPa m/s (m 0.06 and K0 2.4
10  16 m3/Nm) was reported. The
composites in present work have excelled in all the parameters. It
was clear that these composites may be ideal materials for dry
bearings operating under severe conditions of P, V and T.
3.2. Worn surface analysis
3.2.1. Pin surfaces
Fig. 7 shows the worn surfaces of pins (a) and (c) under max.
safe values of PV (for CNG-Vmax safe 3.45 m/s and PVmax safe
CNG 3.45 m/s
20µm 1000 X
CTG 3.25 m/s
20µm
1000 X
CNG 3.5 m/s
20µm 1000 X
Fig. 7. SEM (
1000) and corresponding Fe dot mappings of micrographs for worn pin surfaces of CNG and CTG under PVmax
values (e) and (f) CNG (3.5 m/s) and CTG (3.4 m/s).
93
98 MPa m/s) and (for CTG-Vmax safe 3.25 m/s and PVmax safe
95.2 MPa m/s) and corresponding Fe dot maps based on EDAX
studies (b) and (d). Fig. 7(e) and (f) are for micrographs of failed
pin surfaces. Overall, topography of both the surfaces is quite
different. CNG shows smoother topography compared to the CTG.
CTG, on the other hand, clearly shows thicker patches of back
transferred material from the disc, more pulverized fibers com-
paratively easily released from the composite during shearing
indicating influence of modified surface of graphite in filler–matrix
bonding and increased fiber–fiber–matrix debonding leading to
higher wear. Thus, modified surface of graphite has resulted in
deterioration in quality of bonding with matrix and fibers, which
could be one of the reasons for its higher wear. The Fe dot maps
indicate back-transferred Fe particles on the pin surface. Fe par-
ticles are due to wear of the disc and get embedded on the sof-
tened surface of a polymeric pin. The locations where dot density
is intense, correspond exactly to the back-transferred layers of
polymer composites indicating that the Fe is due to disc wear and
not as an integral ingredient of pin. Overall, higher wear of CTG
could be well correlated with the surface topography.
3.2.2. Worn surfaces of the disks
Figs. 8 and 9 are for disc surfaces under various magnifications
worn against CNG and CTG under various PV values; mainly under
PVlimit values. Fig. 8 (under PVlimit) shows overall surface topo-
graphy of the disc and material transfer from the pin. The
b Fe dot mapping
Fe dot mapping
Large sized Fe-debris
C TG 3.4 m/s Thick polymer melt
20µm
1000 X
safe values; (a)–(d) and failed surfaces at PVlimit
94 J.N. Panda et al. / Wear 360-361 (2016) 87–96
C NG3.45 m/s
1000 X
CTG 3.25 m/s
Wear debris
1000 X
Si dot mapping
Fig. 8. SEM of discs slid against CNG (a) and (b) (v- 3.45 m/s) and CTG (c)–(f) (V 3.25 m/s)and corresponding dot mappings of Carbon (indicating PEK/TG or both) and Si.
micrographs in Fig. 8(a) and (b) are for disc against CNG while Fig. 8
(c)–(d) are for disc against CTG. Comparison of micrographs in
Fig. 8(a) and (c) clearly indicates difference in quality of film
transfer. For Fig. 8(a) it is smooth and more uniform, while for
Fig. 8(c) it is more heterogeneous and showing lumpy transfer.
This was the basic reason for difference in tribo-performance of
both the composites. The most important observation is about
molten glass transfer on the disc confirmed by Si dot mapping
Fig. 8(b) and (d). In our earlier work [5] such molten glass transfer
was observed for PEK composites with different compositions and
slid under different conditions, which acted as a third solid
lubricant reducing the friction further. The transfer of molten glass
on the disc is comparatively lower in case of disc against CTG. This
was because of higher TC of TG which was effective in conduction
of heat from the tribo-interface. Though it is very much desired for
a tribo-composite and tribo-surface, in this case it has hindered
transfer of molten glass, which was beneficial. This was one of the
reasons for slightly higher m and wear of CTG. Comparison of
micrograph C and corresponding carbon dot mapping for CTG
indicates transferred lumps (marked) are due to polymer and
graphite. Fe dot mapping (micrograh Fig. 7(f)) shows minimal
density of Fe confirming heavy transfer of fiber, polymer and fillers
from the pin.
Fig. 9 is also for discs slid against CNG and CTG under PV limit
values. The overall disc surface in Fig. 9(a) (against CNG) is covered
with thin film while Fig. 9(b) (against CTG) shows thicker transfer.
Si dot mapping
20µm
Molten glass fiber layer
C dot mapping
20µm
Fe dot mapping
The typical location where bulk of material is transferred was
focused. Micrographs Fig. 9(a) and (b) shows the difference in
gross transfer of material when composites showed failure. It was
a continuous narrow stream probably from the central portion of
the pin on both the surfaces Fig. 9(a) and (b), which gets max-
imum heated due to poorest heat conduction. These decisively led
to failure of pins. The magnified views of these tunnels show
interesting features. For disc against CNG the scenario was not so
chaotic. A few fibers also got on the disc during gross failure of pin.
Si and Carbon dot mappings Fig. 9(d) and (e) indicated locations of
fibers (empty spaces in Fig. 9(e)). The narrow streak also shows
molten polymer (Carbon dot density). In case of disc against CTG,
the molten material transfer was so sudden and heavy that one
can easily see the bunches of fibers transferred on the disc. Thus,
during failure, surface of composite got molten as a whole and
hence all ingredients were transferred simultaneously. Markers in
micrographs Fig. 9(g), (h) and (i) indicate some transfer appearing
similar to fibers is not due to fibers but due to carbonaceous (PAEK
and graphite).
Thus, the SEM and EDAX studies proved very helpful in
understanding failure reasons and mechanisms.
4. Conclusions
Based on the philosophy that the enhanced capacity of heat
extraction from the surface of a polymer composite sliding under
 J.N. Panda et al. / Wear 360-361 (2016) 87–96 95

CNG 3.5 m/s C TG 3.4 m/s

Molten material transfer

100 µm
150 X 100 µm 150 X

CNG 3.5 m/s C dot mapping

1000 X 60µ

B dot Si dot mapping

CTG (3.4 m/s C dot mapping

PAEK & graphite transfer

1000 X 60µ

B dot mapping
Si dot mapping

Fig. 9. SEM and EDAX studies done on the discs slid against CTG and CNG in PVlimit conditions- (failed CNG at 3.5 m/s and CTG at 3.4 m/s); (a) and (b) at low magnification
150
showing lumpy transfer of molten material; (c)–(j) high magnification- 1000
focused on the lumps.
96 J.N. Panda et al. / Wear 360-361 (2016) 87–96
dry condition will help to minimize the thermal damage of a
polymer, and hence will improve the tribo-performance; a special
composite was designed containing graphite with higher con-
ductivity (thermographite-TG) (10%) along with PAEK (50%), short
glass fibers (30%) and hBN (10%). Another composite (NG) con-
taining identical ingredients but differing only in the type of gra-
phite was also developed using natural graphite. Based on obser-
vations on tribo-studies against mild steel discs under a wide
range of velocities (1.6–3.5 m/s) and under constant load 900 N,
following major conclusions were drawn.
Both the composites showed very low friction coefficient in the
range of 0.04–0.07 and specific wear rates in the range of 2–
7
10  16 m3/Nm under very high pressure 28 MPa and range of
speed (1.6–3.5 m/s). Overall CNG exhibited lower m than the CNG
(approx. 2% depending on selected speeds) and lower specific
wear rate (approx. 20%) in general. The PVlimit values and PVsafe
values for CNG and CNG were 98 and 96.6 MPa m/s, 95.2 and
91 MPa m/s.
Such values indicate the possibility of using these materials
reliably under harsh operating conditions and for polymeric
materials such combination of tribo-properties is first time
reported.
It was concluded that the natural graphite proved better per-
former than the thermographite, which was not anticipated. The
distorted layer lattice structure due to exfoliation as a result of
patented coating/treatment could be the reason for such behavior.
The efficient thin film transfer on the counterface was hindered
resulting in poorer performance by TG. This was evident from the
SEM and EDAX studies.
It was finally concluded that any treatment/coating to the filler/
fiber for attaining typical performance property (in this case
thermal conductivity) cannot be extended to the derived perfor-
mance properties such as tribo-behavior under very high PV
values as in the present case. It has to be validated in desired
situation.
Acknowledgment
Authors are grateful to Department of Science & Technology,
Delhi India (Sanction no. SR/S3/MERC/0088/2011) for financial
assistance for carrying out the research work in the sponsored
project.
Authors gratefully acknowledge the help offered by Mr T Parida
and Dr P Trivedi for injection molding the composites.
The authors confirm that this article content has no conflicts of
interest that could any way bias this work.
References
[1] K. Friedrich, A.K. Schlarb, Tribology of Polymeric Nanocomposites: Friction and
Wear of Bulk Materials and Coatings, Elsevier, United Kingdom, 2013,
ISBN:13:978-0-444-59455-6.
[2] D.L. Burris, W.G. Sawyer, Tribological behavior of PEEK components with
compositionally graded PEEK/PTFE surfaces, Wear 262 (2007) 220–224, http:
//dx.doi.org/10.1016/j.wear.2006.03.045.
[3] A.C. Greco, R. Erck, O. Ajayi, G. Fenske, Effect of reinforcement morphology on
high-speed sliding friction and wear of PEEK polymers, Wear 271 (2011)
2222–2229, http://dx.doi.org/10.1016/j.wear.2011.01.065.
[4] M. Kalin, M. Zalaznik, S. Novak, Wear and friction behaviour of poly-ether-
ether-ketone (PEEK) filled with graphene , WS2 and CNT nanoparticles, Wear
332–333 (2015) 855–862, http://dx.doi.org/10.1016/j.wear.2014.12.036.
[5] J. Bijwe, S. Sharma, M. Sharma, T. Parida, P. Trivedi, Exploration of potential of
solid lubricants and short fibers in Polyetherketone (PEK) composites, Wear
301 (2013) 810–819, http://dx.doi.org/10.1016/j.wear.2013.01.059.
[6] J. Bijwe, Nidhi, Potential of fibers and solid lubricants to enhance the tribo-
utility of PEEK in adverse operating conditions, Ind. Lubr. Tribol. 59 (2007)
156–165, http://dx.doi.org/10.1108/003687907107535451.
[7] X. Pei, K. Friedrich, Sliding wear properties of PEEK, PBI and PPP, Wear 274–
275 (2012) 452–455, http://dx.doi.org/10.1016/j.wear.2011.09.009.
[8] J. Geringer, W. Tatkiewicz, G. Rouchouse, Wear behavior of PAEK, poly(aryl-
ether-ketone), under physiological condit ions, outlooks for performing these
materials in the field of hip prosthesis, Wear 271 (2011) 2793–2803, http://dx.
doi.org/10.1016/j.wear.2011.05.034.
[9] M. Sharma, J. Bijwe, P. Mitschang, Wear performance of PEEK–carbon fabric
composites with strengthened fiber–matrix interface, Wear 271 (2011)
2261–2268, http://dx.doi.org/10.1016/j.wear.2010.11.055.
[10] J. Bijwe, M.K. Gupta, T. Parida, P. Trivedi, Design and development of advanced
polymer composites as high performance tribo-materials based on blends of
PEK and ABPBI, Wear 342–343 (2015) 65–76, http://dx.doi.org/10.1016/j.
wear.2015.07.018.
[11] R. Schroeder, F.W. Torres, C. Binder, A.N. Klein, J.D.B. de Mello, Failure mode in
sliding wear of PEEK based composites, Wear 301 (2013) 717–726, http://dx.
doi.org/10.1016/j.wear.2012.11.055.
[12] L. Chang, Z. Zhang, H. Zhang, K. Friedrich, Effect of nanoparticles on the tri-
bological behaviour of short carbon fibre reinforced poly(etherimide) com-
posites, Tribol. Int. 38 (2005) 966–973, http://dx.doi.org/10.1016/j.
triboint.2005.07.026.
[13] Z. Zhang, C. Breidt, L. Chang, F. Haupert, K. Friedrich, Enhancement of the wear
resistance of epoxy: short carbon fibres, graphite, PTFE and nano-TiO2, Com-
pos. Part A Appl. Sci. Manuf. 35 (2004) 1385–1392, http://dx.doi.org/10.1016/j.
compositesa.2004.05.005.
[14] G. Zhang, L. Chang, A.K. Schlarb, The role of nano-SiO2 particles on the tri-
bological behavior of short carbon fiber reinforced PEEK, Compos. Sci. Technol.
69 (2009) 1029–1035, http://dx.doi.org/10.1016/j.compscitech.2009.01.023.
[15] L. Chang, Z. Zhang, H. Zhang, A.K. Schlarb, On the sliding wear of nanoparticle
filled polyamide 66 composites, Compos. Sci. Technol. 66 (2006) 3188–3198,
http://dx.doi.org/10.1016/j.compscitech.2005.02.021.
[16] 〈http://en.wikipedia.org/wiki/Boron_nitride〉 (15th October 2015).
[17] Properties and Characteristics of Graphite, 1996. doi:10.1016/S0022-3913(12)
00047-9.
[18] J. Drobny, Fluoroplastics, Ismithers Rapra Publishing, Rapra technology, United
Kingdom, 2006, ISSN: 0889-3144, 16(4).
[19] A.A. Balandin, Thermal properties of graphene and nanostructured carbon
materials, Nat. Mater. 10 (2011) 569–581, http://dx.doi.org/10.1038/nmat3064.
[20] R. Gilardi, L. Alzati, M. Thiam, J.F. Brunel, Y. Desplanques, P. Dufrénoy, et al.,
Copper substitution and noise reduction in brake pads: Graphite type selection,
Materials 5 (2012) 2258–2269, http://dx.doi.org/10.3390/ma5112258 (Basel).
[21] E. Grivei, F. Rota, J.C. Rietsch, S. Zuercher, R. Gilardi, M. Spahr, Ground
Expanded Graphite Agglomerates, Methods of Making, and Applications of the
Same, Patent No. WO 2012020099A1, 16 February 2012.
[22] 〈http://www.imerys–graphite–and–carbon.com〉(15th October 2015).
[23] N. Aranganathan, J. Bijwe, Special grade of graphite in NAO friction materials
for possible replacement of copper, Wear 330 (2015) 515–523, http://dx.doi.
org/10.1016/j.wear.2014.12.037.
[24] J. Bijwe, K. Kumar, J. Panda, T. Parida, P. Trivedi, Design and development of high
performance tribo-composites based on synergism in two solid lubricants,
Compos. Part B (2016), http://dx.doi.org/10.1016/j.compositesb.2016.03.034.
[25] J. Bijwe, A. Kadiyala, K. Kumar, D. Puhan, T. Parida, Development of high per-
formance poly (ether-ketone) composites based on novel processing technique,
Mater. Des. 73 (2015) 50–59, http://dx.doi.org/10.1016/j.matdes.2015.02.007.
[26] 〈http://www.ghardaplastics.com〉 (15th October 2015).
[27] H. Hunke, N. Soin, T. Shah, E. Kramer, K. Witan, E. Siores, Influence of plasma
pre-treatment of polytetrafluoroethylene (PTFE) micropowders on the
mechanical and tribological performance of Polyethersulfone (PESU)–PTFE
composites, Wear 328–329 (2015) 480–487, http://dx.doi.org/10.1016/j.
wear.2015.03.004.