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Susceptibility to scratch damage of high

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 Materials Science and Engineering A 492 (2008) 400406

Contents lists available at ScienceDirect

Materials Science and Engineering A

journal homepage: www.elsevier.com/locate/msea

Susceptibility to scratch damage of high density polyethylene coating

N. Guermazi a , K. Elleuch b, , H.F. Ayedi a , H. Zahouani c , Ph. Kapsa c
a
Unit de Recherche de Chimie Industrielle et Matriaux, URCIM-ENIS, BP W 3038, Sfax, Tunisia
b
Laboratoire des Systmes lectro-Mcaniques, LASEM-ENIS, BP W 3038, Sfax, Tunisia
c
Laboratoire de Tribologie et Dynamique des Systmes, LTDS-ECL, 69134, Ecully, France

a r t i c l e i n f o a b s t r a c t

Article history: The scratch behaviour of a polymeric coating, based on high density polyethylene (HDPE), used for pipeline
Received 26 December 2007 application was investigated in this work. Instrumented scratch testing was used for the characterization
Received in revised form 26 March 2008 of the friction and wear behaviour of such materials. Static contact of a diamond conical indenter against
Accepted 14 May 2008
the polyethylene (PE) coating was experimentally studied. Normal and tangential forces are measured
during the scratch experiments using various scratch parameters (such as sliding velocity, attack angle,
Keywords:
applied normal load). All the experiments were performed under unlubricated conditions and at room
Polymeric coating
temperature. Moreover, some hygrothermally aged coating samples were considered in order to analyze
Scratch
Friction
the effect of immersion aging on their scratch behaviour. Before being subjected to scratch experiments,
Wear resistance these samples were immersed in synthetic sea water at a set temperature of 70 C and for 6 months. The
Wear mechanisms scratch behaviour of the polymeric coating was discussed in terms of friction coefcient, wear resistance
Hygrothermal aging impact and wear mechanisms. Thus, scratch tracks were analyzed qualitatively and quantitatively. To characterize
the scratch process, three-dimensional topography of the scratched surfaces was measured. In fact, wear
morphologies of the PE coating were observed after scratching by tactile prolometer and laser interfer-
ometer. Friction response was correlated to wear mechanisms. Wear volume can be considered relevant
responses to describe the materials scratch resistance. It was found that friction and wear behaviours are
signicantly affected by scratch parameters. Hygrothermal aging considerably affects the wear resistance
of the studied coating. In terms of wear mechanisms, the ploughing controls the wear of such PE coating
whole the retained test conditions.
2008 Elsevier B.V. All rights reserved.

1. Introduction
The scratch test is a very old experimental procedure used
to study the surface mechanical properties and the tribological
performances of materials. The scratching technique has gained
interest in recent times due to its varied applications to a num-
ber of engineering materials, especially for the evaluation of the
mechanical properties of materials under various contact condi-
tions [16].
Scratch testing is applied to polymers for about 10 years [715]
because polymers are more often used to increase the scratch and
wear resistance in many applications, in particular, in petroleum
and gases industries as a pipe coatings [1619]. Moderate friction
coefcient and high abrasion resistance are required in this appli-
cation. Scratch behaviour of polymers is generally quite different
from metals; and wear of polymers is more complicated than that
of metals. The analysis and the interpretation of scratch test is far
Corresponding author.
E-mail address: khaled.elleuch@enis.rnu.tn (K. Elleuch).
more difcult than for metals because of the large elastic recovery
of polymers and their complex rheological behaviour [10]. Felder
and Bucaille [6] have provided a mechanical analysis of the scratch-
ing of metals and polymers with conical indenters at low and large
strains. They have related the differences in their scratch resistance
to their rheological properties.
Recently, Hadal and Misra [20] have studied the scratch defor-
mation behaviour of thermoplastic materials with signicant
differences in ductility. They have discussed their susceptibil-
ity to scratch deformation in terms of modulus, elastic recovery,
scratch hardness, and entanglement density. Koch and Machl
[21] have provided an evaluation of scratch resistance in mul-
tiphase PP blends. They have investigated the inuence of
addition of different polyethylenes (PEs) to these blends on the
scratch behaviour in terms of wear mechanism and elastic recov-
ery.
In 1996, Briscoe et al. [22] have constructed a number of defor-
mation maps for a range of polymers subjected to various scratch
contact conditions (strain, sliding velocity, and applied normal
load). Friction maps have also been generated in order to cor-
relate the surface deformation mechanisms with the energetic

0921-5093/$ see front matter 2008 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2008.05.035
 N. Guermazi et al. / Materials Science and Engineering A 492 (2008) 400406 401

Table 1
Some properties of the studied polymeric coating [29]

Density 0.93 0.01

Vicat softening point ( C) 114 2
Melting point ( C) 131 2
Hardness (shore A) 90 2
Elastic modulus (MPa) 358 4
Tensile strength (MPa) 19.2 0.5
Percent elongation (%) Over 500

Fig. 1. Position of the scratch test samples from the pipe coating.

response. In particular, the effect of sliding velocity was consid-

ered. In addition, indenter geometry plays an important role in
scratch behaviour of polymers [11,2224]. It was found that wear
mechanisms depend on attack angle of the indenter at a given tem-
perature.
Furthermore, effect of the applied normal load on scratch
behaviour was largely considered [11,2227]. However, the con-
clusions related to variation of this parameter present some
contradictions. In fact, Ducret et al. [23] have shown that the appar-
ent friction coefcient is not dependent upon the applied normal
load when studying scratch behaviour of ultra high molecular
weight polyethylene (UHMWPE). Whereas, Barquins [26] has found
that the friction coefcient varies according to the applied normal
load, Sinha and Lim [27] have studied the effects of applied normal
load and the resulting scratch depth on scratch force prole and
the mechanisms of deformation for a number of industrial poly-
mers. They have found that deformation mechanism is insensitive
to both applied normal load and scratch depth. However, material
removal and debris formation process depend strongly upon the
scratch depth.
Almost all scratch studies were considered without lubrication,
i.e. under dry conditions. In contrast, the scratch of some plasticized
polymers (in the presence of a plasticizing agent) was investigated
by Stuart and Briscoe [28]. Hence, as the hygrothermal aging pro-
vokes plasticization phenomena in polymer coatings [29], scratch
of aged polymers may be simulated by scratching plasticized poly-
mers.
The aim of this study is to investigate the scratch behaviour of
pipe coatings based on high density polyethylene (HDPE). An exper-
imental analysis was carried out to simulate the damages which
occurred and observed in service conditions of this material. More-
over, some hygrothermally aged coating samples were considered
in order to analyze the effect of immersion aging on their scratch
behaviour.
2. Experimental procedure
2.1. Materials
The material used for this work was already described in pre-
vious study [29]. It consists of a polymeric coating based on
HDPE and it was cut from pipeline coatings (Fig. 1). Paralleli-
Fig. 2. Scratch test device.
of arithmetic roughness (Ra ) for all sample surfaces was given by
both tactile prolometer and laser interferometer and it was around
0.62 m.
The maximum penetration depth of the scratch experiment is
less than 200 m so that the mechanical properties of the underly-
ing layer should not affect the results. Some properties of the main
coating are reported in Table 1.
2.2. Scratch test device
The apparatus used for the characterization of the scratch
behaviour of the polymeric coating was the sclerometer which
is already described in the literature [12,23]. Also, its principle is
shown schematically in Fig. 2. The indenter was held on a pivoted
beam so that it could be positioned orthogonally to the at sample.
The sample surface is positioned so that it is parallel to the inden-
ter motion by a specic, automatically, controlled process. The unit
is controlled by a computer, which also controls the various test
parameters. The indenter used in this study has a diamond conical
tip with a spherical end of 5 m radius.
2.3. Test conditions and procedure
Scratch experiments were performed at room temperature
under dry conditions. The retained test conditions were detailed in
Table 2. During the machining procedure, a normal load was applied
and maintained constant over the length of the scratch. Both the
tangential force (Ft ) and the normal load (Fn ) were continuously
recorded using a piezo-electric transducer located underneath
Table 2
Experimental conditions for the scratch test

pedic samples 30 mm 15 mm 3.3 mm of PE coating were used Applied normal load, Fn (N) 1, 5, 10, 15 and 20
as samples for scratch tests. At the rst, the coating samples were Sliding velocity, v (mm s1 ) 0.1, 0.5, 1, 5, 10, 50 and 100
mechanically ground to P2500 grade paper (grit size 6 m) under Indenter attack angle,  ( ) 10, 30 and 45
Scratching length (mm) 5
water-lubricated condition. After polishing operation, the average
402 N. Guermazi et al. / Materials Science and Engineering A 492 (2008) 400406

Fig. 3. Illustration of scratch sections: w, scratching width; d, scratching depth; S(),

negative section; S(+), positive section or the material piled up next to the scratch.

Fig. 4. The initial indentation and recovered scratch depths as a function of sliding
the sample. Therefore, the apparent friction coefcient, app , was distance. The arrow indicates the scratch direction.
dened as
Ft
app = (1)
Fn
The experimentally measured friction coefcient was compared to
the theoretical friction coefcient suggested by Bowden and Tabor
[30]. This model was developed in order to predict the friction coef-
cient of a conical indenter for material having a constant yield
stress. This model supposes that the apparent friction coefcient,
app , is given by [28]:
2 tan 
app = (2)

where  is the indenter attack angle. This expression suggests that
the scratch friction coefcient due to plastic ploughing is inde-
pendent of any material parameter and depends entirely on the
geometry of the indenter. For the ideal case of plastic ploughing
the relationship between the friction coefcient and tan  is linear. Fig. 5. Friction coefcient as function of sliding velocity, v (mm s1 ) (in terms of
Variations from this linear relationship, in the experimental val- logarithm (Ln v)) (unaged sample, Fn = 10 N, and  = 30 ).
ues, may be used to determine the type of material response for
the polymer [28].
The estimation of wear volume produced by the scratch tests on Finally, it should be noted that each of the presented results is
PE coating is, however, extremely challenging because of the very the average of three values measured under the same conditions.
small quantity of wear debris particles involved. For this reason,
the scratch cross-section area, S(), was measured using a tactile 3. Results and discussion
prolometer (see Fig. 3). The volume of removed material was esti-
mated as the negative section, S(), multiplied by the scratching The effect of several parameters such as the sliding velocity,
length: applied normal load and attack angle on the scratch behaviour of
the studied polymeric coating is discussed in the following sections.
Volume of removal material=negative section scratching length A tactile prolometer was used to estimate the scratch cross-
In addition, the scratches were also observed using laser interfer- section and the removed material. Laser interferometer was also
ometer as explained below. Toposurf 3D, as a commercial software used for studying the deformation and wear mechanisms. There-
package for the treatment of surface morphological images, has fore, various scratch responses, such as friction coefcient, wear
been successfully used to estimate the wear parameters. From the resistance and wear mechanisms, were investigated (Figs. 512).
scratch morphology lots of quantitative and qualitative informa-
tions or explanations were extracted. The following parameters 3.1. Effect of the sliding velocity on scratch behaviour
may be considered: the initial indentation depth, d1 (this penetra-
tion corresponds to the transition between the initial indentation In this section, only the frictional response of the polymeric coat-
step and the beginning of the scratch test and it must be measured ing was studied. Fig. 5 shows the variation of the friction coefcient
during the test in steady conditions), the recovered scratch depth, as function of sliding velocity for an unaged sample, under applied
d2 (scratch depth after unloading), width of the scratch, w, and normal load of 10 N and attack angle of 30 .
the pile-up height, hp (see Fig. 4). In addition to the above mea- As it can be seen, when the sliding velocity increases the appar-
sured parameters to characterize scratch deformation resistance, ent friction coefcient signicantly decreases. This variation can
the recovery parameter can be estimated, from the cross proles of be due to the viscoplasticity of the polymer coating: an increase in
the scratches (Fig. 4), using the following way [21]: sliding velocity produces an increase in the strain rate and the yield
d d  stress of the polymer; so the plastic deformation decreases and the
1 2
Elastic recovery (%) = 100 (3) recovery at the rear part of the indenter increases: the apparent
d1
friction coefcient decreases as the elastic part of the deformation
where d1 is the initial indentation depth and d2 is the recovered increases [7,9]. Also in the literature, many studies [22,24,3134]
scratch depth. have shown the same result, i.e. the apparent friction coefcient
 N. Guermazi et al. / Materials Science and Engineering A 492 (2008) 400406
Fig. 6. Friction coefcient as function of attack angle (unaged sample, Fn = 10 N, and
v = 0.1 mm s1 ).
decreases as the sliding velocity increases, in the case of viscoelas-
tic, viscoplastic and viscoelastoplastic contacts.
3.2. Effect of the attack angle on scratch behaviour
In this section, the scratch experiments were conducted under
an applied normal load of 10 N and sliding velocity of 0.1 mm s1
using various attack angles.
The variation of the frictional response as function of attack
angle is plotted in Fig. 6. It was found that the friction coefcient
increases signicantly with increase in attack angle. The predicted
friction coefcient due to the plastic ploughing, calculated using
Eq. (2), is also shown in Fig. 6. There is poor agreement between
the measured and theoretical ploughing values, especially for rel-
atively small attack angle. In fact, for an attack angle below 30 ,
this poor agreement is probably due to the contribution of adhe-
sive component [28]. However, for an attack angle over 30 , the
Fig. 7. Laser interferometer images of (a) scratch produced by a constant-force scratch method: 2D intensity projection (left); (b) 3D scratch morphology measured by laser
interferometer on PE coating, imaged by Toposurf 3D; (c) line prole; (d) elastic recovery of the scratch groove. Attack angle  = 10 , Fn = 10 N and v = 0.1 mm s1 .
403
Table 3
Scratch deformation parameters for the polymeric coating determined from pro-
lometry measurements (using various attack angles)
Scratch parameters (Fn = 10 N Attack angle
and v = 0.1 mm s1 )
 = 10  = 30  = 45
Scratch depth (m) 41 2 104 3 162 4
Scratch width (m) 267 4 359 4 399 4
Pile-up height (m) 6.3 0.2 13.8 0.5 30 1
theoretical model correlates well the experimental curve. So the
adhesive component can be neglected and there is only a ploughing
component.
In addition, increase in the friction coefcient may be explained
by that, when the attack angle increases the contact area between
the indenter and the sample decreases, which causes a deeper
indentation at higher angle (see Table 3). Consequently, the dis-
placement of the indenter becomes more and more difcult during
the scratch. Such results are in great accordance with those found
in the literature [11,22,23].
Qualitatively, in order to identify the wear mechanisms under-
gone by PE coating with various attack angles, the morphology
of the scratches made under the same applied normal load was
analyzed and examined using the tactile prolometer (Figs. 79).
These gures mainly show two kinds of deformation during
the experiments: plastic or permanent deformation and an elas-
tic recovery of the scratch groove. Moreover, it was observed that
there is a material piled up at the lateral edge of the scratch. These
results are in good agreement with those found by Jardret et al.
[12] in the study of the scratch behaviours of some polymers. How-
ever, the transition of the wear mechanism from microploughing
to microcutting, which widely depends on the nature of materials
in contact, was not clearly observed under the considered scratch
conditions, which is probably due to the ductile character of the
studied coating.
404 N. Guermazi et al. / Materials Science and Engineering A 492 (2008) 400406

Fig. 8. Laser interferometer images of (a) scratch produced by a constant-force scratch method: 2D intensity projection; (b) 3D topological presentation; (c) line prole; (d)
elastic recovery of the scratch groove. Attack angle  = 30 , Fn = 10 N and v = 0.1 mm s1 .

In addition, a signicant elastic recovery was clearly
observed for the PE coating under the retained attack angles
(Figs. 7d, 8d and 9d). Such elastic recovery proves the viscoelastic
behaviour of the studied material and explains the dependence of
friction coefcient with the sliding velocity.
On the other hand, Fig. 10 shows the variation of the wear vol-
ume as function of the attack angle under the same conditions.
It was demonstrated that the wear volume is proportional to the
attack angle. Similarly, Table 3 shows that the penetration depth
increases with the attack angle. This increase is a pure geometrical

Fig. 9. Laser interferometer images of (a) scratch produced by a constant-force scratch method: 2D intensity projection; (b) 3D topological presentation; (c) line prole; (d)
elastic recovery of the scratch groove. Attack angle  = 45 , Fn = 10 N and v = 0.1 mm s1 .
 N. Guermazi et al. / Materials Science and Engineering A 492 (2008) 400406
Fig. 10. The variation of the wear volume as function of attack angle (unaged sample,
Fn = 10 N and v = 0.1 mm s1 ).
effect: in rst approximation, the load determines the width
of the groove and the contact area, and for a given contact
area, the penetration depth increases as function of the attack
angle. Consequently, one can conclude that the increase in attack
angle increases the deformation and so the damage of the mate-
rial.
3.3. Effect of the normal load on scratch behaviour
To investigate the effect of the normal load on the scratch
response, a xed attack angle of 10 and a sliding velocity
of 0.1 mm s1 were considered. The corresponding results were
shown in Figs. 11 and 12.
Many authors have demonstrated that friction coefcient
slightly increases with increase in applied normal load [25,26,35].
However, Fig. 11 shows that the apparent friction coefcient does
not depend upon the applied normal load. This observation con-
rms that the contact geometry is self-similar under the considered
loads, and that the rounding at the extremity of the conical inden-
ter (5 m) can be neglected [23]. Furthermore, it can be noted
that increasing applied normal load does not change the deforma-
tion mechanism. A ductile deformation was often occurred. It was
deduced from the elastic recovery behaviour of the studied coating.
This result is in good agreement with those found by Sinha and Lim
[27].
In terms of wear resistance, it was found that the wear volume
varies according to the applied normal load (Fig. 12). In fact, when
Fig. 11. Friction coefcient as function of applied normal load for both unaged and
aged samples ( = 10 and v = 0.1 mm s1 ).
405
Fig. 12. Wear volume as function of applied normal load for both unaged and aged
samples ( = 10 and v = 0.1 mm s1 ).
the applied normal load increases, the penetration of the inden-
ter into the scratched sample becomes more and more deeper.
Consequently, the volume of the removed material increases. The
observed trends are consistent with the wear model of Rabinow-
icz [36] which states that the wear volume is proportional to the
applied normal load.
3.4. Effect of the immersion aging on scratch behaviour
In previous work, it was found that wear resistance of PE
coating was considerably affected by hygrothermal aging under
a pin-on disk conguration [29]. This is due to the plasti-
cization phenomena occurred when the coating samples were
subjected to immersion aging. So it will be interesting to study
the effect of hygrothermal aging throughout scratch test. All the
scratch experiments were conducted using an attack angle of 10
and sliding velocity of 0.1 mm s1 under various applied normal
loads.
Variation of the frictional responses and wear volume responses
versus the applied normal load for aged and unaged samples were
reported in Figs. 11 and 12.
It was observed in Fig. 11 that the friction coefcient remains
constant versus the applied normal load under aging conditions,
however there is a decrease in friction coefcient compared to the
values corresponding to the unaged samples. Such difference may
be related to the solvent effect in the coating surface. In fact, the
solvent can play the role of lubricant such as relative humidity
(RH), which explains the decrease of the friction coefcient for the
immersed samples. This result is in agreement with the works of Da
Silva et al. [37]. In fact, they have found that the friction coefcient
is inversely proportional to the RH variation.
In terms of wear resistance, Fig. 12 shows that, wear volume of
the aging samples increases versus the applied normal load as well
as the unaged case. In contrast, aging induces increase of wear vol-
ume compared to the unaged coating. Similarly, Table 4 shows that
Table 4
Scratch deformation parameters for the polymeric coating determined from pro-
lometry measurements (for both unaged and aged samples)
Scratch parameters (Fn = 10 N,  = 10 and v = 0.1 mm s1 ) Studied sample
Unaged Aged
Scratch depth (m) 41 2 47 2
Scratch width, w (m) 267 4 305 4
Pile-up height (m) 6.3 0.2 6.8 0.2
Scratch hardness, Hs a (MPa) 178 4 137 4
a
Scratch hardness was calculated as follows [20,32]: Hs = 4Fn /w2 .
406 N. Guermazi et al. / Materials Science and Engineering A 492 (2008) 400406
aging process has a harmful effect on scratch response, in particu-
lar, scratch hardness. Synthetic sea water acts as a plasticizer and
the softening of the PE coating allows the indenter to penetrate the
polymer to a great depth, which explains the decrease of the wear
resistance of the aged samples.
4. Conclusions
The purpose of this work is to determine the susceptibility of
PE coating to scratch damage. Scratch testing was used to study its
tribological properties (in terms of friction and wear). Both unaged
and hygrothermal aged samples are considered. Aged samples were
immersed in synthetic sea water at a set temperature of 70 C for 6
months.
It was found that the friction coefcient as an energetic response
widely depends on the scratch parameters. There is a dramatic
decrease of friction coefcient with sliding velocity, however, it
increases when increasing the attack angle of the indenter. No sig-
nicant effect was noted on the friction coefcient when varying
the applied normal load.
Independently of the imposed normal load or the depth of
scratching, two kinds of deformation were discerned during the
scratch experiments: plastic or permanent deformation and an
elastic recovery of the scratch groove. The observed recoverable
deformation clearly reveals the viscoelastic behaviour of the PE
coating.
From quantitative viewpoint, wear resistance of such coating
has been found enormously depending on test parameters. Wear
volume varies with both the indenter attack angle and the applied
normal load. Material removal widely depends upon the scratch
depth. Hygrothermal aging signicantly affects the wear resistance
of the studied coating. Scratch test can thus be seen to be a quick
and sensitive measure of the degradation of this material following
aging process. Finally, the ploughing remains the main wear mech-
anisms controlling the wear of such PE coating whole the retained
test conditions.
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