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Leaf Coppin

Sliding Wear Behaviour of PEEK-PTFE Blends

W. Hufenbach, K. Kunze Institutfur Leichtbau und KunststofStechnik, Tech-


nische Universitat Dresden, Germany, and J. Bijwe ITMMEC, Indian
Institute of Technology, New Delhi, India

Abstract

The role of PTFE in tailoring the tribological peflormance of PEEK is not


clear from the literature, and conflicting evidence is reported about its ability
to improve friction, wear, or both. Moreover, little has been reported on the
optimum composition of such blends for the best possible combination of me-
chanical and tribological properties. Hence, in this work various blends of
PEEK with PTFE have been injection moulded and characterised for their
mechanical properties. Their friction and wear behaviour was evaluated
using a pin-on-disc machine. It was observed that the inclusion of PTFE pow-
der not only removed scufJing problems associated with thefriction behaviour
of PEEK, but also improved both friction and wear characteristics. A blend
with 7.5 wt.% PTFE showed the best wear behaviour, while a blend with 30
wt. % PTFE exhibited the best friction pegormance. A concentration of 7.5
wt.% PTFE was thought to be the optimum amount for the best possible
combination of mechanical and tribological properties.

Keywords

friction, wear, PTFE, PEEK, mechanical properties, tribological properties

INTRODUCTION

Poly(ether ether ketone) (PEEK) is a semicrystalline (crystallinity 0-40%),


high-performance engineering thermoplastic with a good combination of
thermal properties (T, = 143"C, T,,, = 338"C, continuous service temperature
= 250"C, heat distortion temperature often in excess of 300°C) and mechanic-
al properties (strength, modulus, toughness, and resistance to creep, abrasion,
and fatigue). It also possesses good resistance to harsh chemicals and environ-
ments and injection processability.' It has been the focus of research of a
number of tribologists seeking to exploit its tribological Review

J. Synthetic Lubricution 20-3, Oct. 2003. (20)227 ISSN 0265-6582$10.00 + $10.00 (242W1003)
228 Hufenbach, Kunze, and Bijwe

Figure 1 Data from the literature: (a) transfer wear rate as a function of
composition (pressure, 6.4 N/m2; speed, 0.45 mm/s; sliding distance, 10 km;
counterface,mild steel; temperature, 20°C);' (b) specific wear rate as a function
of PTFE content (speed, 1 m / s ; pressure, 1 MPa; counterface, 100Cr6, HRC 62,
R, 0.2-0.3 pm)"

10

8
I Wear rate of 100% PTFE: 60 x lod

0
0 20 40 60 80 100 PTFE
Composition (wt.%)
100 80 60 40 20 0 PEEK

lo-" h

E
z
2
E
v

10-13 L"
6
c
F
10-14
ki
0)
%
.-
0
c0
a,
10-l~ g
0 20 40 60 80 100
PTFE content (vol.%)

articles on the current state of PEEK tribology have also appeared.''.'' This is
possibly the tribo-polymer most investigated in recent years.
In spite of its excellent resistance to adhesive wear, it has some serious
drawbacks. It is known to exhibit a coefficient of friction as high as 0.7, which
limits its use as an antifriction material in applications such as slideways and
linkage bearings. Another potential problem with this material is its scuffing

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Sliding wear behaviour of PEEK-PTFE blends 229

behaviour, which has always been a matter of concern to tribologists. High


frictional work often generates high interfacial temperatures and PEEK-
ferrous metal contacts undergo a rather unusual type of failure which re-
sembles the scuffing failure commonly observed in lubricated or unlubricated
metal contacts." Continuing efforts are being made to enhance the utility of
PEEK as a more versatile tribological material for a wide range of applica-
tions. This has mostly been achieved by fabricating composites with fillers
and solid lubricant^*^^-^^ or fibrous reinforcements, or with combinations of
both.4,5,12,19,20 Other approaches have been based on plasma treatment2'or ion
implantation.**The development and tribological evaluation of various blends
of PEEK to enhance its T value with some high-temperature polymers, such
as polyetherimide (PEI)" and thermotropic liquid crystal polymer^?^ have
also been attempted. Very low coefficients of friction (down to 0.1) without
scuffing at high pressure-velocity (pv) values and very low wear rates in the
region of m3/Nmhave been achieved.
Compared to fibrous reinforcements in polymers, particulate fillers are
favoured through perceived benefits associated with easy mixing and process-
ing. In the case of PEEK tribology, composites with fillers, such as
polytetrafluoroethylene (PTFE)and CuS and nanometre-size fillers such as
ZrO,, Si3N4,and SiC,2,9-i7 have been investigated in depth. The role of PTFE
in controlling friction, wear, or both in polymer compositeshlends has been
one of the most-investigated aspects of polymer tribology. Briscoe et a1.* in-
vestigated a series of composites of PEEK-PTFE with an increasing amount
of PTFE in the PEEK (0, 10,20,30, ...loo%) along with studies on their me-
chanical properties, such as micro-hardness, compressive strength, and elastic
modulus. It was concluded that the inclusion of PTFE in PEEK extended its
load-carrying capacity and reduced the coefficient of friction drastically, but
at the cost of a modest loss in wear resistance (Figure l(a)). A composition
with 10%PTFE proved to be close to the optimum for the friction and wear
properties. It is important to note that the minimum coefficient of friction and
minimum wear do not occur at the same composition. Interestingly,in a paper
by Lu and Friedrichi2on blends with PTFE (5, 15,40, 60, 85, 95, 100%) in
PEEK (prepared by injection moulding) it was concluded that PTFE not only
reduced the coefficient of friction of PEEK drastically but improved the wear
performance (Figure l(b)). In this study too, the minimum coefficients of
friction and wear did not occur at the same composition. The minima of the
coefficient of friction and wear were recorded for a blend with 15 and 5 vol.%
PTFE,respectively. A composition with PTFE in the range 10-20% was

J. Synthetic Lubrication 20-3, Oct. 2003. (20) 229 ISSN 0265-6582 $10.00 + $10.00
230 Hufenbach, Kunze, and Bijwe

Table 1 Details of PEEK-PTFE blends2’


Material designation All ,475 4 5 A22 5 A,
PTFE (wt.%) 0 7.5 15 22.5 30
PTFE (vo~.%) - 3.26 6.52 9.78 13.04
Density, ASTM D 792 1.28 1.32 1.36 1.41 1.43

Hardness (Shore D) 94 90 85 83 80

Tensile strength at break (MPa), 87 84 77 70.5 64.6


ASTM D 638 Type 1

Tensile modulus (GPa) 3.9 1.5 1.43 1.32 1.23


Elongation at break (%) 21 11.2 10.49 10.42 8.87
Flexural strength (MPa), 139 122.66 100.7 98.53 92.62
ASTM D 790

Flexural modulus (GPa) 3.7 2.98 2.62 2.57 2.4

Impact strength (Jim), 60 97.32 102.2 1 1 6.34 126.42


ASTM D 256 (Charpy impact)

observed to be the optimum for the best tribological behaviour. The authors of
these studies, however, focused only on the tribological behaviour of blends,
and the influence of PTFE on mechanical properties was not studied. It is an
accepted fact that for material selection for any application, mechanical prop-
erties also play an important role. Although these two papers focused on
similar series of compositeshlends prepared by different moulding
techniques and the operating conditions, testing devices, and counterface
materials were also different, the role of PTFE in PEEK in influencing wear
appeared to be conflicting. Moreover, the optimum range of PTFE
composition for the best properties also differed widely.
The present paper reports a study of the role of PTFE in both the friction
and wear behaviour of PEEK and the determination of the optimum composi-
tion for the best properties. Simultaneous studies on the influence of PTFE on
the mechanical properties of PEEK composites were also carried out. To this
end, a series of blends containing PTFE in PEEK was investigated for their
tribological and mechanical strength behaviour and the results are presented
in this paper.

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Sliding wear behaviour of PEEK-PTFE blends 231

Figure 2 Image and schematic of the pin-on-discmachine

Pin

EXPERIMENTAL

Materials

Neat (unfilled) PEEK (Gatone PEEK 5400) and its various blends with PTFE
were supplied by Gharda Chemicals Ltd., India, in the form of dumbbells. The
PEEK and PTFE (Grade MP 1000 by Dupont) were powder mixed before
melt blending using a Berstorff twin-screw extruder in the temperature range
330-350°C. The extruded strands were quenched in water and then chopped
into granules. They were dried for 4 h at 150°C prior to injection moulding
using an LMT Demag 60 N4K injection moulding machine. The details of the
blends are given in Table 1, as are their mechanical properties, characterised
in the 1aborato1-y.~~

Adhesive wear studies

Adhesive wear studies were carried out using a pin-on-disc machine (Figure
2) fabricated at ILK India (a diagram of the configuration is also shown in
Figure 2). A polymer pin of 5 mm diameter and 15 mm length was slid against
a steel (16Mn Cr5) disc of diameter 46 mm, hardness HRC56, and surface
roughness R,=3.2 pm in a vertical configuration. The pin was slid in a track of
36 mm in diameter with a speed of 0.35 d s . The sliding duration and loading
conditions depended on the selected testing mode. The frictional torque was
continuously recorded by an attached microprocessor while wear was deter-
mined by measuring the reduction in the length of the pin after cleaning and

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232 Hufenbach, Kunze, and Bijwe

Figure 3 Friction testing mode - coefficient of friction (average) as a function of


sliding duration (speed, 0.35 m / s ; counterface, steel (16Mn Cr5) disc) for
various blends: (a) A,, (b) A,,5, (c) A,5, (d) and (e) A,,

0.8
-
I
Y

c 0.6
0
._
c
._
0
c
L

Z
c
0.4
C
.-a
0
fj 0.2
s
0
0 0.25 0.5 0.75 1 1.25
Sliding duration (h)

Normal force, FN
F ~ = 2 0 0 NFN=250N FN=300N FN=350N FN=400N
0.4
0.4 I I I I
1 I

Y
I
5
._
0.3
c
0
c
L

Z 0.2

0
0 0.5 1 1.5 2 2.5
Sliding duration (h)

- Regression
Average value (in interval of force)

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Sliding wear behaviour of PEEK-PTFE blends 233

Figure 3 Friction testing mode - coefficient of friction (average) as a function of


sliding duration (speed, 0.35 d s ; counterface, steel (16Mn Cr5) disc) for
various blends: (a) Ao, (b) A,.5, (c) A,5, (d) A22.5,and (e) A,,

Normal force, FN
FN= 200 N FN= 250 N FN = 300 N FN= 350 N FN= 400 N
0.3

5 0.25
v

*
L

c
C
.z.-
0

c
a,
0.2

0.15
- 8

I
I
8
I
I
1
9

1
'U 0.1
5
6 0.05 i

0
0 0.5 1 1.5 2 2.5
Sliding duration (h)

Normal force, FN
FN= 200 N FN= 250 N FN= 300 N FN= 350 N FN= 400 N
04 I I I I
I 1 ,
h
1
i I 1
v I
c 0.3 1 I
0
1
0
i ' 8 1

-
c
L

5 02
C
a,
f 01 I I I
s I
0
0 05 1 15 2 25
Sliding duration (h)

__ Regression
Average value (in interval of force)

J. Synthetic Lubrication 20-3, Oct. 2003. (20)233 ISSN 0265-6582 $10.00 + $10.00
234 Hufenbach, Kunze, and Bijwe

Figure 3 Friction testing mode - coefficient of friction (average) as a function of


sliding duration (speed, 0.35 m/s; counterface, steel (16Mn Cr5) disc) for
various blends: (a) A,, (b) A,.,, (c) A,,, (d) A,,,,, and (e) A,,

Normal force, FN
FN= 200 N FN = 250 N FN= 300 N FN= 350 N FN= 400 N
0.2 I I I

-
v
I
~

c 0.15
--c
0
0
.-
v-
L

5
I
0.1 L
C
a,
.-
V
$ 0.05
6
0
0 0.5 1 1.5 2 2.5
Sliding duration (h)

~ Regression
Average value (in interval of force)

cooling to ambient temperature. The specific wear rate, KO,was calculated


from the following equation:

KO= A V1LD (m3/Nm)

where A V is the wear volume in m3,L is the load in N, and D is the distance
slid in m. Investigations were performed in two types of test mode, as outlined
below.

Friction testing mode A pin was slid (sliding speed 0.35 d s ) against a disc
for the selected duration (for PEEK, 1.25 h; for the blends, 2.5 h), increasing
the load in steps of 50 N with a preset programme (the interval for PEEK was
15 min and for blends, 30 min). The loads selected were 100, 150, 200, 250,
and 300 N for PEEK, and 200,250,300,350, and 400 N for the blends (PEEK
could not be tested at higher loads because stick-slip was observed).

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Sliding wear behaviour of PEEK-PTFE blends 235

Figure 4 Wear testing mode (speed, 0.35 d s ; counterface, steel (16Mn Cr5)
disc; sliding distance, 10 km): (a) coefficient of friction (average) as a function
of pressure; (b) coefficient of friction (average) as a function of PTFE content

(4 06
h

v
I 0.5
C
0.4
0

-
w
L
u-
0 03
C
; 02
f
6 01

0
10 125 15 17.5 20 22.5 25
Pressure, p (MPa)

(b) 0.6
h

v
I 0.5
C
.z
0
.-
0.4
c
L

5 0.3
c
t
aY
'5 0.2

6 0.1

0
0 5 10 15 20 25 30
PTFE content (wt.%)

Wear testing mode A pin of measured thickness was slid against the disc
(sliding speed 0.35 m / s ) under the selected loads for 8 h; the selected loads
were 150, 200, and 250 N (corresponding pressures 15, 20, and 25 MPa) for
the blends. In the case of PEEK, only one load, 150 N (pressure 15 MPa), was
used because at higher loads scuffing was observed. After the wear experi-
ment (sliding distance 10 km) the reduction in the thickness of the pin was
measured after cooling.

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236 Hufenbach, Kunze, und Bijwe

Figure 5 Specific wear rates of the blends at various pressures (speed, 0.35 m/s;
counterface, steel (16Mn Cr5) disc; sliding distance, 10 km)

E
z
2
10-14

E
v

X0
6
c
e
;ir 10-15

I
0
c
0
a
Q
10-16
0 7.5 15 22.5 30
PTFE content (vd %)

RESULTS AND DISCUSSION

The coefficient of friction for thc selected blends as a function of sliding time
in the friction testing mode is shown in Figure 3 (pp. 232-234). Figure 4
above shows the friction data in the wear mode. The specific wear rate at
different pressures as a function of PTFE content is shown in Figure 5 while
Figures 6 and 7 (see p. 238) summarise respectively the tribological
performance and mechanical properties of the blends.
As seen from Figure 3, a high coefficient of friction (0.55) and stick-slip
behaviour were observed for unfilled PEEK which is in agreement with the
literature. Wang et ~ 1 . reported
' ~ a very high coefficient of friction (0.7) while
Mens and Gee' reported a value of 0.5 for different materials and under
different conditions.
The important features emerging from the studies are as follows. Inclu-
sion of PTFE drastically improved the friction behaviour of PEEK. Not only
was the magnitude of p reduced due to the inclusion of PTFE, but no scuffing
behaviour was observed for any composition. The coefficient of friction de-
creased continuously with increasing PTFE content. For the 30% blend, there
was a significant reduction, from 0.55 to 0.12.
The wear behaviour was also substantially improved due to PTFE inclu-
sion. KOwas a minimum at 7.5 wt.% loading, followed by a slow increase with
increasing PTFE content. At the 7.5% level, KOwas reduced by 30 times,

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Sliding wear behaviour of PEEK-PTFE blends 237

Figure 6 Specific wear rate and coefficient of friction as a function of PTFE


content (pressure, 20 MPa)

0
- - __ z _ 0
'c
u
0 (I)
a

while at the 30% level, it was reduced by 10 times. Thus, the best friction be-
haviour was shown by A,, and the best wear performance was exhibited by
A7,5(Figure 6). As seen in Figure 7, except for the impact behaviour, all the
mechanical properties of the blend deteriorated with increasing PTFE content
in PEEK. Hardness, tensile strength, flexural strength, and modulus decreased
above 7.5%. Tensile modulus, however, showed an excessive reduction even
at this level of PTFE. Thus PEEK with no PTFE exhibited the best mechanical
properties, except for impact strength. The tribological properties, however,
were the lowest. A,, was best in terms of impact and friction properties but
poorest in terms of mechanical properties. A,.' was best in terms of wearprop-
erties, showing very good friction behaviour with a good combination of
mechanical properties. In fact, a number of blends in this narrow range of
composition should be evaluated for still greater optimisation of the
properties.
In the case of the role of PTFE in PEEK, conflicting evidence is reported
in the literature. Mens and de Gee' reported an improvement in both friction
and wear performance of PEEK due to the inclusion of 15% PTFE. Wang et
aZ.I7 reported a reduction in p (from 0.38 to 0.26) and KO(almost two times)
due to 5 vol.% (approximately 1 1 % by weight) content of PTFE. The extent
of the reduction in friction, however, decreased slowly with further addition
of PTFE,as in the present case. The minimum K, was recorded at 20 vol.%
(approximately 45% by weight) loading of PTFE. Briscoe et aL2studied various

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238 Hufenbach, Kunze, and Bijwe

Figure 7 Influence of PTFE on the mechanical properties of the blends

Hardness Tensile strength at Tensile modulus Elongationat break


(Shore D) break (GPa) (”/)
(MPa)

Flexural strength Flexural modulus Impact strength


(MP4 (GW (JW

tribological and mechanical properties of several composites of PEEK with


PTFE. Although their findings on the friction behaviour of the composites are
in agreement with the literature and the present investigation (large reduction
in p due to PTFE), their observations on wear aspects are very different. A
continuous increase in the wear rate with increasing PTFE content (Figure
l(b)) was recorded. In the case of mechanical properties similar trends were
observed. An absolute comparison of the observations, however, should not
be done in the case of composites since the moulding conditions and testing
conditions were significantly different. Lu and Friedrich’*also studied the tri-
bological performance of similar compositions. Their findings also are
different from those of Briscoe et d 2Lu and Friedrich reported a significant

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Sliding wear behaviour of PEEK-PTFE blends 239

improvement in both friction and wear behaviour due to PTFE inclusion. Both
p and the specific wear rate showed minima at some concentration of PTFE.
An almost 200 times enhancement in the wear performance due to 5 vol.% (1 1
wt.%) PTFE inclusion was observed (in the present work a 30-times improve-
ment at 7.5 wt.% PTFE inclusion was recorded). For PEEK-PTFE
combinations, p was a minimum at 15 vol.% (35 wt.%). The optimum com-
position suggested for the best possible combination of friction and wear was
in the range 10-20 vol.% (23-45 wt.%). The range suggested by Lu and
Friedrich did not exactly match with the range observed in the present inves-
tigation (7.5 wt.%) which could be due to differences in the moulding and
testing processes. Moreover, the PEEK material and PTFE filler selected in
this work were also of different grades.

CONCLUSIONS

It was concluded from the investigations that the inclusion of PTFE in PEEK
definitely and significantly improved the performance of the PEEK. The
blends did not show any scuffing problems. A wear rate as low as m3/Nm
was recorded in the case of the blends. An improvement of 30 times in the
wear rate and 5 times in the friction coefficient was observed due to blending.
For the composition at which p was a minimum, the wear rate was not at the
minimum; where the wear was at a minimum, p was not at its minimum. For
the best combination of tribological and mechanical properties, inclusion of
PTFE in the region of 7.5 wt.% was recommended from these investigations.

Acknowledgement

The authors are grateful to Dr. P.D. Trivedi, Gharda Chemicals Ltd. India, for
providing samples for the research.

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