Wear 342-343 (2015) 85–91

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

Gamma irradiation effects on thermal, physical and tribological

properties of PEEK under water lubricated conditions
Neelima Khare n, P.K. Limaye, N.L. Soni, R.J. Patel
Refuelling Technology Division, BARC, Trombay, Mumbai 400085, India

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

Article history: Effects of gamma irradiation (upto 3 MGy) on thermal, physical and tribological properties of poly-ether-
Received 3 April 2015 ether ketone (PEEK) were studied. Several studies have presented data on radiation stability of PEEK.
Received in revised form However, none have investigated the effects of gamma irradiation on its tribological properties. This
4 August 2015
work was carried out for applications of precision mechanisms of fuelling machine of Indian Pressurised
Accepted 6 August 2015
Available online 20 August 2015
Heavy Water Reactors (PHWRs). Hence very slow sliding speed and water lubricated environment were
selected.
Keywords: Increase in glass transition temperature, melting temperature, hardness and density was observed
Sliding wear after exposure to gamma irradiation. Highest glass transition temperature and melting temperature were
Wear testing
observed at 0.5 MGy. Tribological properties were also altered after exposure to gamma radiation. Sur-
Hardness
face stresses generated due to crosslinking have resulted into highest coefficient of friction at 0.5 MGy
Steel
Polymers dose. Reduced probability of fracture has resulted into lowest wear rate at same dose.
& 2015 Elsevier B.V. All rights reserved.

1. Introduction
Apart from their good tribological properties, some engineered
polymers have good ductility, formability and light weight. It is
making them an obvious choice for replacing ceramic and metallic
components. Polymeric material for nuclear power plant application
should have high radiation resistance and good mechanical/tribolo-
gical properties. High energy radiation in the plant can bring major
changes in the molecular structure and macroscopic properties of
polymers. Radiation dose required to bring changes in physical
properties of polymers is considerably less than that is required to
cause any significant change in ceramics or metals [1]. The radiation
can bring changes in appearance, chemical/ physical states,
mechanical, tribological, electrical and thermal properties. Poly-
ether-ether-ketone (PEEK) is one of the most promising polymers, a
semi-crystalline thermoplastic with excellent mechanical properties
[2]. It displays high glass transition temperature (143 °C) and high
melting point (335 °C) [3]. It can easily be processed in various
complex shapes and also it possesses high toughness and excellent
wear resistance [4]. It has good stability in both chemically active and
radiation environments [5]. Celina et al. [5] studied about different
polymeric materials components used in acidic-radiation environ-
ment. They concluded that PEEK is stable for radiation and thermal
behaviour under acidic environments. Due to these properties, PEEK
n
Corresponding author.
E-mail address: neelima.khare@gmail.com (N. Khare).
and its composites are widely used for various applications e.g.
aerospace, nuclear and tribological [6,7]. Lawrence et al. [8] studied
the effect of gamma radiation on the thermal properties and mor-
phology of PEEK and PEEK–alumina composites. They concluded that
increase in glass transition temperature (Tg) and decrease in melting
temperature (Tm) take place for both materials. Sasuga et al. [9]
studied effect of gamma radiation in terms of change in mechanical
properties, under oxygen pressure for different aromatic polymers.
Under this study they concluded that aromatic polymers which show
relatively high radiation resistance for non-oxidative irradiation
deteriorate vigorously under oxidative irradiation and this is brought
about mainly by chain scission only. Sharp et al. [10] studied the
effects of radiations on various components of nuclear robot appli-
cation. Remotely operated connectors with PEEK insulation have
been shown to be very resistant, both mechanically and electrically,
up to high total doses (10 MGy) and even under thermal stresses
(120 °C). Hernandez et al. [11] studied the effect of gamma radiation
on water lubricated PEEK components (O-rings, seals etc.) of ITER.
They concluded that PEEK shows excellent mechanical behaviour
after irradiation. Sasuga et al. [12] studied effects of ion irradiation on
thermal and mechanical properties of crystalline and non-crystalline
PEEK. Ash et al. [13] concluded in their work that molecular weight
of polymers increases after exposure to gamma irradiation due to
cross-linking and results into improvement in tribological/ mechan-
ical properties.
Tribological performance of polymer is greatly influenced by
many factors and studied by many researchers in past. Jie et al.
[14] proved in their work that, the friction coefficient is mainly

http://dx.doi.org/10.1016/j.wear.2015.08.005
0043-1648/& 2015 Elsevier B.V. All rights reserved.
86 N. Khare et al. / Wear 342-343 (2015) 85–91

influenced by the PV factor (mechanical factor), and the weight Table 1

loss was mainly influenced by the contact temperature (thermal Properties of PEEK, aluminium bronze and 17-4 PH stainless steel.
factor). Effects of reinforcement on tribological performance were
Property Values
investigated by Davim et al. [15] under dry condition and by Khare
et al. [16] under water lubricated conditions. They concluded that Name PEEK 17-4 PH SS Aluminium bronze
carbon fibre reinforcement is very effective for improved tribolo- Composition (wt%) No fillers Cr¼ 17%, Ni¼ 4%, Al ¼8.5–11%, Fe¼ 2.0–
gical performances of PEEK. Tribological performance of PEEK was Cu ¼ 4%, % 5.0%, Ni ¼ 4.0–6.0%,
Fe¼ balance Mn ¼0.0–1.5 %
nicely evaluated by statistical and other methods by researchers Cu ¼balance
[14,17]. Several studies have presented data on radiation stability Density (gm/cc) 1.31 7.8 7.58
of PEEK. However, none have investigated the effects of gamma Water absorption (%) 0.1 – –
irradiation on its tribological properties. (immersion after
24 h)
In fuelling machine head of Pressurised Heavy Water Reactors
Thermal conductivity 0.252 22.6 39.1
(PHWRs), present design employs components of aluminium (W/m K)
bronze and phosphor bronze rubbing against moving components Tensile strength (MPa) 110 1400 690
of precipitation hardened stainless steels (e.g. 17-4 PH SS, 13-08 Hardness 105 36 96
MO SS) at slow sliding speeds (0.005–0.05 m/s). Some examples of
these components are piston-cylinder, ram drives, latch gear-
0.5–3 MGy (50 -300 MRad) at a dose rate of 12.5 kGy/h, as mea-
spline shaft etc. These all components are sliding at very low speed
sured by Fricke dosimetry.
and always submerged under water lubrication. To determine
tribological performance of these components, it is required to
carry out test on pin-on-disc setup for simulated operated condi- 2.3. Thermal characterisation
tions. Operating environment is high purity de-mineralised water
at moderate temperature and 10 MPa operating pressure. In these Samples of dimensions approx. 2
2 mm2 were cut from irra-
operating conditions, wear mechanism of aluminium bronze is diated PEEK samples. Subsequent thermal characterisation was
adhesive in nature, which produces large size wear debris and carried out using a differential scanning calorimeter (DSC; Model:
causes significant damage to mating part. These wear debris DSC 131) supplied by M/s. SETARAM Instrumentations, France.
accumulate at other sliding joints and cause further damage to the Samples were kept in aluminium crucible and heated from 30 to
surfaces. Hence for long term solution, new materials are needed 450 °C at 10 °C/min. Subsequent cooling was carried out from melt
to study as a replacement for bronze components. In this work, the to 30 °C. Graphs were recorded online and values of glass transi-
effects of gamma radiation on the tribological and thermal beha- tion and melting temperatures extracted for various doses.
viour of natural PEEK under water lubricated condition were
investigated. 17-4 PH SS counterface was used because it is com- 2.4. Density measurement
monly used material for nuclear applications. Comparison
between tribological properties of conventional material pair The determination of the density was carried out by water
(aluminium bronze and 17-4 PH SS) and selected material pair
displacement, which consists in evaluating the specific gravity of a
(PEEK and 17-4 PH SS) was carried out. Accumulated dose for 10
specimen. The specific gravity of PEEK samples (unirradiated and
years operating life for fuelling machine components is of the
irradiated) was determined with a Mettler H35 AR scale, a con-
order of 2–2.5 MGy. Thermal, physical, and tribological properties
tainer filled with distilled water and attachment for suspending
evaluation of PEEK was carried out up to 3 MGy.
the specimens following the procedures laid out in ASTM D792-A.
Tribological performance of a system can be improved by
First, the samples of about 10 g weights were conditioned for 48 h
replacing conventional metallic materials with high performance
at 237 1 °C. Samples were weighted first in air, then in water. Five
polymers. However for nuclear applications careful selection of
samples were measured three times each, which provided for a
material is required due to the presence of radiation. Purpose of
low standard deviation on the mean value of the density at any
this work is to establish the effect of gamma irradiation on prop-
erties of PEEK and to compare the performance with conventional given dose. Specific gravity was calculated using the following
material. equation:
a
Specific gravity, ρ =
a−b
2. Experimental where a is the apparent mass of specimen in air and b is the
apparent mass of specimen completely immersed in water.
2.1. Materials

PEEK in extruded rod form was purchased from a reputed
supplier. Flat ended cylindrical pins with 4.0 mm diameter at
contact were machined from rods. The 17-4 pH stainless steel discs
of 10 mm thickness and 110 mm diameter were machined from a
forged rod. Discs were heat treated to achieve hardness value of 36
HRC. Discs and pins were ground to achieve surface roughness (Ra)
of 0.96 mm. For detailed materials properties refer Table 1.
2.2. Radiation aging
Sealed samples of PEEK were kept in ice temperature bath and
irradiated with gamma rays from a 60Co source in a gamma
chamber (Model no.: GC-5000, supplied by M/s BRIT India). The
irradiation was carried out by delivering radiation doses of
2.5. Hardness measurement
Rockwell hardness is a measure of the net increase in depth of
the indenter. The Rockwell hardness test was conducted at room
temperature as per ASTMD785. Samples of PEEK having 8 mm
diameter and 10 mm length were prepared. Three samples at each
dose of 0.5, 0.75, 1, 2, 3 MGy were irradiated. Testing was per-
formed by first forcing a steel ball indenter (diameter 6.35 mm)
into the surface of a sample using a specified minor load (10 kg).
The load is then increased to a specified major load (100 kg) and
then decreased back to the original minor load. Rockwell hardness
number was obtained from direct reading on M scale. To find
accurate results, at least three readings at different locations of
samples were determined and average value was reported.
 N. Khare et al. / Wear 342-343 (2015) 85–91
2.6. Tribological evaluation
The friction and wear tests were conducted on a pin-on-disc
test rig. Test rig was specially designed for under water lubricated
testing. Proper sealing arrangements were provided to prevent any
leakage of water. PEEK pin sample was held by a pin holder against
the rotating disc mounted on disc holder. Before each test, poly-
mer pins and 17-4 PH stainless steel discs were thoroughly
cleaned with alcohol/acetone in an ultrasonic bath. Lubrication
was applied on wear track (wear track diameter is 90 mm) using
20 drops of de-mineralised water (having 9.5 pH) every minute,
keeping it flooded to achieve testing in submerged condition. The
tribological tests were carried out at sliding speeds of 0.005,
0.05 m/s and contact pressures 3, 6, 12 MPa. Diameter of pin at the
contact was 4 mm and it was constant for all the tests. Variable
contact pressure was achieved by varying normal load and keep-
ing area of contact constant. Ambient temperature around 25 °C
and sliding distance of 1000 m were kept constant for all tests.
During the test, friction force was recorded continuously
throughout the test using a load cell. Plot of variation of coefficient
of friction with varying sliding distance was displaced online
during the test. After stabilisation of plot average value of COF was
reported. Wear of the pin was evaluated by measuring weight loss
after completing the test using a precision weight balance
(AFCOSET ER-182 A).
Each test was repeated three times and their average values
were presented. The specific wear rate Ws was calculated from the
following relationship
Δm ⎡ 3 ⎤
Ws = ⎣ mm /Nm⎦
ρF N L
where ∆m is the mass loss, ρ is the density of the irradiated/
unirradiated specimen, L is total sliding distance and FN is the
applied load. Aluminium bronze (Pin) and 17-4 pH stainless steel
(Disc) material pair was also tested similarly under water lubri-
cated condition. Sliding speed of 0.5 m/s and contact pressures 3,
6 and 12 MPa were used. The worn surfaces of PEEK and alumi-
nium bronze were observed under a scanning electron microscope
(SEM) (CT/100 Cam Scan MV2300, UK). Before SEM examination
the worn surfaces of PEEK were sputtered coated with a thin layer
of gold.
3. Results and discussion
3.1. Thermal properties
Fig. 1 shows the variation of glass transition temperature (Tg)
and melting temperature (Tm) with absorbed radiation doses.
Fig. 1. Variation of glass transition temperature, Tg, and melting temperature, Tm,
with radiation dose.
87
Glass transition and melting temperatures started from their
lowest value for unirradiated condition and reached to highest
value for 0.50 MGy irradiated condition. These started decreasing
after 0.50 MGy and reached to some value (still greater than uni-
rradiated condition) for 3 MGy irradiated condition. Glass transi-
tion temperature at all radiation doses was higher than that for
un-irradiated conditions. It indicated radiation stability of PEEK
upto 3 MGy. Melting temperature and glass transition temperature
are directly related to the molecular weight of the polymer.
Melting point reached to its highest value at 0.50 MGy irradiated
conditions signifies that molecular weight of PEEK is maximum at
0.50 MGy condition. Ash et al. [13] concluded in his work that
molecular weight of polymers increases after exposure to gamma
irradiation due to cross-linking and results into improvement in
tribological/mechanical properties. This signifies that highest
crosslinking has occurred at 0.5 MGy irradiation dose among the
other selected doses. Shift of Tg to high temperature because of
radiation may arise from restriction of three dimensional mole-
cular motions by the newly formed crystallites during cooling run
of DSC at given crystallisation temperatures. In terms of degree of
crosslinking it can be stated that highest and lowest degree of
crosslinking is indicated at 0.5 MGy and 3 MGy respectively.
3.2. Density measurement
The specific gravity or density of a solid is a property that can
be an indicative of physical changes in a sample. Changes in
density of the material may be due to changes in crystallinity,
molecular weight, crosslinking, molecular configuration etc. The
measured densities as a function of the irradiation dose are pre-
sented in Fig. 2. As expected, the densities of the irradiated PEEK
grades are different, a fact explained by the difference in the
molecular weight. The density increase is an indicative of mor-
phological changes in the polymer structure, consisting mostly in
crosslinking occurring. Thermal evaluation displayed the highest
crosslinking at 0.5 MGy dose, however density has not confirmed
the same. Density is almost same at all the irradiation doses.
3.3. Hardness evaluation
Exposure of radiation resulted into increased hardness of PEEK
as displayed in Fig. 3. Once increased, hardness is stabilized for
further increase in irradiation dose upto 3 MGy. Although
increased hardness attributed to crosslinking of PEEK however it is
not confirmed that crosslinking is maximum at 0.5 MGy dose.
High hardness generally produces wear resistant surfaces however
other factors also influence this.
Fig. 2. Variation of density with radiation dose.
88 N. Khare et al. / Wear 342-343 (2015) 85–91
3.4. Tribological properties
Friction and wear are serious causes of energy dissipation and
material dissipation respectively. Fig. 4 presents typical variation
of coefficient of friction (COF) with sliding distance. Once the
graph is stabilized, average value of COF was calculated and
reported. Fig. 5(a) and (b) presents the variation of coefficient of
friction with change in contact pressure and irradiation doses.
General trend is COF reducing to a certain extent then stabilized
with increase in contact pressure. This is a typical behaviour due to
elastic deformation of asperities. Highest COF was depicted by
samples irradiated for 0.50 MGy and 0.75 MGy (only at high slid-
ing speed) irradiation dose. The junctions sheared under the
applied tangential force results in the friction force. In general, the
interfacial junctions are influenced by the nature of the mated
Fig. 3. Variation of hardness with radiation dose.
Fig. 4. Variation of coefficient of friction with sliding distance at 0.75 MGy, 12 MPa,
0.05 m/s.
Fig. 5. Variation of coefficient of friction with contact pressure and radiation dose (a) 0.005 m/s and (b) 0.05 m/s.
surfaces as well as by the surface chemistry and the stresses in the
surface layers. Irisawa et al. [18,19] showed in their work that
coefficient of friction can be represented by following equation:
gσ
μ=
kH
where H is the microhardness of softer material, s is the stress
required to slide the abrasive particle, g is the shape factor of the
abrasive particle (or asperity), and k is a constant. In current work,
difference in hardness of both the surfaces is very high. Asperities
of hard metallic counterface are sliding on soft polymer material,
hence abrasion is talking place. Here g is constant because same
counterface is being used for all the PEEK surfaces; however H is
different for irradiated and unirradiated material. Coefficient of
friction decreases with either increase in hardness or decrease in
surface stresses. Results showed that hardness of irradiated
material at all the selected doses is approximately the same. This
indicated that surface stress generated due to crosslinking of
polymer is responsible for change in COF. Highly cross linked
material at 0.5 MGy and 0.75 MGy is indicating maximum COF in
most of the conditions. These results also indicate that with
increase in contact pressure effect of surface stresses is reduced.
Due to much difference in the hardness of PEEK and 17-4 PH SS,
negligible wear of 17-4 PH SS was observed. Wear rate of PEEK was
calculated and reported here. Fig. 6(a) and (b) presents variation of
wear rate of PEEK with contact pressure and sliding speed for
different radiation doses. Wear rate is different at different irra-
diation doses and lowest for samples irradiated at 0.5 and
0.75 MGy. However order of wear is same for all the conditions.
Sample irradiated at 0.5 MGy indicated sharp decrease in wear
rate with increase in contact pressure. This phenomenon was
observed only at high speed. Contact pressure and sliding speed
have little effect on wear rate of irradiated/unirradiated samples.
Wear and friction are surface phenomena, modification of
surfaces leads to change in wear and friction mechanisms. Wear
rate may change with either change in hardness or in surface
conditions. In general increased hardness is responsible for
increased wear resistance of a material. In current work, hardness
of irradiated material at all the selected doses is approximately
same however wear rate is different. Reason behind this may be
that, as degree of crosslinking is changing, surface condition is also
changing. Formation of three dimensional networks due to
crosslinking and resulting surfaces stresses caused improved sur-
face conditions. Highest degree crosslinking at 0.5 MGy indicated
lowest wear rate.
Coefficient of friction (COF) and wear rates of unirradiated and
irradiated PEEK were compared with aluminium bronze. Fig. 7(a)
and (b) shows COF and wear rate respectively for irradiated/uni-
rradiated PEEK and aluminium bronze, under water lubricated
environment. For most of the conditions, all materials exhibited
 N. Khare et al. / Wear 342-343 (2015) 85–91
Fig. 6. Variation of wear rate with contact pressure and radiation dose (a) 0.005 m/s and (b) 0.05 m/s.
Fig. 7. The relationship with contact pressure for PEEK materials and aluminium bronze at 0.05 m/s (a) coefficient of friction and (b) wear rate.
lower COF than that of aluminium bronze. However, at 3 MPa
contact pressure, 0.5 and 0.75 MGy condition showed higher COF
than aluminium bronze. COF for metallic material pairs comprises
two components namely adhesion and ploughing. At higher con-
tact pressure, adhesion component of friction might be dominat-
ing for aluminium bronze and 17-4 PH SS material pair, which
results into high COF. All materials exhibit lower wear rate than
aluminium bronze except at 3 MPa contact pressure. Increased
contact pressure resulted into high wear rate of aluminium bronze
may be due to change in wear mechanism from abrasive to
adhesive.
Replacement of aluminium bronze with PEEK may result into
reduction in wear rate. However it all depends on value of irra-
diation dose.
3.5. Wear mechanisms of irradiated and unirradiated PEEK
Surface topographies of worn surfaces clearly supported wear
performance trends of unirradiated and irradiated PEEK. The worn
surface of unirradiated PEEK as shown in Fig. 8(a) exhibited wear
marks in the form of continuous narrow cutting grooves. Grooves
are formed due to ploughing of soft material by hard asperities of
counterface material. In addition, some chip like large size wear
debris formed during the sliding process was also visible. Wear
debris might have originated due to detachment of soften plasti-
cized surface from bulk material. Fig. 8(b) indicates more entrap-
ment of wear debris on the surface which might have resulted into
decreasing coefficient of friction and wear rate with increase in
contact pressure. Main wear mechanism of unirradiated PEEK is
abrasive wear caused by hard asperities of the counterface. Fig. 8
(c) indicates worn surface of PEEK irradiated at 0.50 MGy. It
showed comparatively smooth topography, sliding marks were not
much visible. Entrapped wear debris was clearly visible on the
89
surface. Main wear mechanisms for this condition can be stated as
very mild wear. Fig. 8(d) indicates worn surface of PEEK irradiated
at 0.75 MGy. It also showed smooth topography however sliding
marks are much visible than sample irradiated at 0.50 MGy. Back
transferred PEEK and embedded wear debris are clearly visible on
the surface. Fig. 8(e) and (f) indicates worn surfaces of samples
irradiated at 3 MGy conditions, as wear performances indicated
that 3 MGy exhibited very high wear rate. Micrographs are
showing back transferred, entrapped wear debris. Presence of
wear particles supports its wear performance.
Fig. 8(g) and (h) shows increased surface distress and delami-
nation due to increasing contact pressure from 3 MPa to 6 MPa.
This has resulted into sudden transition in wear rate of aluminium
bronze. Fig. 8(i) shows large extent of adhesive wear and severe
plastic deformation of aluminium bronze in sliding direction,
resulting surface delamination. Surface was covered with plasti-
cally deformed wear debris and surface pits due to material pull
out at many locations. This tendency of plastic deformation and
adhesion increased the probability of formation of asperity junc-
tions, resulting in much higher friction coefficient.
4. Conclusions
Natural PEEK samples were irradiated up to 3 MGy for gamma
radiation dose. Thermal, physical and tribological properties were
evaluated at various radiation doses. Following conclusions were
drawn:
 Exposure to gamma irradiation caused crosslinking of PEEK and
resulted into increase in glass transition temperature, melting
temperature, density and hardness.
90 N. Khare et al. / Wear 342-343 (2015) 85–91

Fig. 8. Worn surfaces of PEEK pins (a) unirradiated (V¼ 0.005 m/s, P¼ 6 MPa), (b) unirradiated (V ¼ 0.05 m/s, P¼ 12 MPa), (c) irradiated at 0.50 MGy (V ¼ 0.005 m/s,
P¼ 12 MPa), (d) irradiated at 0.75 MGy (V ¼0.05 m/s, P ¼12 MPa), (e) irradiated at 3 MGy (V ¼ 0.005 m/s, P¼ 12 MPa), (f) irradiated at 3 MGy (V¼ 0. 05 m/s, P ¼12 MPa),
(g) aluminium bronze (V ¼ 0.05 m/s, P¼ 3 MPa), (h) aluminium bronze (V ¼0.05 m/s, P ¼6 MPa) and (i) aluminium bronze (V¼ 0.05 m/s, P¼ 12 MPa).
 N. Khare et al. / Wear 342-343 (2015) 85–91
 Thermal evaluation indicated highest degree of crosslinking at
0.5 MGy radiation dose, although it was not supported by
hardness and density evaluation.
 Degree of crosslinking was correlated with the tribological
properties. Highest COF was observed at 0.5 MGy conditions
due to increase in surface stresses. Lowest wear was observed at
0.5 MGy conditions due to improved surface conditions by for-
mation of three dimensional networks.
 Abrasion associated with the ploughing marks and the presence
of wear particles were dominant wear phenomenon for irra-
diated/unirradiated PEEK.
 Adhesive wear, severe plastic deformation and delamination
were the main wear mechanisms of aluminium bronze.
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