Conductive eco-polymer composites: wear
behaviour of recycled polycarbonate/crushed
rubber microparticles

R. Autay

1

, K. Elleuch

1

, K. Zribi

2,3

and J.-F. Feller*

3

Following an eco-design approach we have investigated the possible formulation of conductive
polymer composite (CPC) from recycled poly(carbonate) (PC) and crushed rubber microparticles
(CR) for tribological applications. Particularly, the abrasive wear behaviour of CPC has been
studied as a function of smooth surface treatments applied to rubber fillers to improve their
adhesion with the PC matrix. The effects of normal load, sliding velocity and treatments applied to
CR on the wear rate and kinetics were investigated. Pin-on-disc tests carried out under water
lubrication show that the wear rate increases with the increase in load and sliding velocity.
Moreover, among all surface treatments, the most effective to improve the interface quality and
thus wear resistance was a stripping of rubber microparticles with methanol whereas flaming was
assumed to degrade filler surface and dichloromethane to swell the matrix. Additionally wear
experiments proved to be effective in evaluating the quality of PC/CR interface.

Keywords: CPC, Abrasive wear, Wear rate, Kinetics of wear, Recycling, Eco-design

Introduction

Owing to environmental issues it is a main concern to
use plastics and composites having the lowest impact on
nature as possible according to eco-design rules.

1

In fact,

analysing the life cycle of such materials evidences that
the use of recycled polymers in composite formulations
allows us to get rid of one of the most impacting step, i.e.
polymerisation. Nevertheless, recycled polymers often
have degraded properties compared to their virgin
homologues as their first processing quite systematically
causes macromolecular chains breakage and conse-
quently molar mass decrease.

2

Thus, two different

strategies can be envisaged to reuse such engineering
polymer wastes: target the same kind of application but
this requires regeneration by addition of a coupling
agent or a chain extender to enhance mechanical
properties, or find a new application that will be less
exigent from this point of view.

3–6

Electrically conduc-

tive polymer composites (CPCs) obtained by blending
an insulating polymer matrix with conductive fillers
like

carbon

nanoparticles,

7–13

carbon

micro

and

nanofibres

11,14–17

or metal micro and nanoparticles

18,19

give a good example of applications which do not need
exceptional mechanical properties; on the other hand,

these materials have been studied by many groups for
their smart functionalities.

9,18,20,21

In fact, they exhibit

several interesting features due to their resistivity vari-
ation with thermal,

22–24

mechanical

12,25

or chemical

solicitations.

23,24,26,27

This versatility of CPC is used for

‘intelligent’ applications such as self-regulated heating
applications such as shielding,

28,29

switching

11,19,23

or

vapour sensors.

14,18,26,27

Some of the last evolutions in the CPC field concern

the use of exclusion volumes to decrease the percol-
ation

threshold

and

control

conductive

pathways

structuring.

30–34

In a recent study, it was shown that CPC

obtained by dispersing crushed tire rubber microparticles
into recycled poly(carbonate) matrix (PC/CR) had very
attractive properties for smart applications

24

owing to their

sensitivity to environmental changes like temperature and
vapour atmosphere. Nevertheless, it was also found that
the development of these composites required taking care
of the quality of PC/CR interface to prevent any
deterioration of their mechanical properties both at micro

35

and macro

36

scales. Among all different strategies experi-

mented to improve adhesion between rubber fillers and PC
matrix solvent washing appeared to better than flaming and
coupling agents.

37

This was explained by a double effect of

solvent: first a removal of oil and dust from particles
surface, and second a desorption of low molar mass
elastomer molecules from the reticulated network which
could act as compatibilising agent. To go further into
interface characterisation and understanding of adhesion
between filler and matrix, we have investigated wear
properties of PC/CR eco-composites.

In fact, abrasive wear behaviour of polymer compo-

sites has attracted lots of scientists due to its simple

1

Unit of Research Industrial Chemistry & Materials, National School of

Engineers, Sfax, Tunisia

2

Laboratory of Water, Energy & Environment, National School of

Engineers, Sfax, Tunisia

3

Smart Plastics Group, European University of Brittany (UEB), LIMAT

B

-

UBS, Lorient, France

*

Corresponding author, email [e-mail]

ß

Institute of Materials, Minerals and Mining 2011

Published by Maney on behalf of the Institute
Received 29 June 2010; accepted 30 October 2010
DOI 10.1179/1743289811X12988633927952

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139

approach and ability to study surface characteristics in
severe friction conditions in relation with the different
mechanical characteristics of the material.

38–42

Many

models, which attempted to relate the abrasive wear
resistance of polymers to other mechanical properties,
have been examined

43–45

and it was shown that the wear

behaviour

14,46

differed depending upon the polymer

type.

Numerous studies have been carried out to investigate

the influence of test conditions on wear properties.

47–58

Some authors observed a decrease in wear rate with
increasing load in a number of materials and it was
associated to the formation of ridges within the wear
scar.

46

Others showed that its value will increase when the

load increases to the limit load value because of the
critical surface energy of the polymer.

59

The effect of

sliding speed and load, on the friction and wear of glass-
fibre-reinforced poly(ether imide), (20%) composite has
been studied,

38

it was reported that no unique trend

between wear rate and speed can be expected. The same
authors showed that the friction coefficient of unfilled
PEI and PEI/PTFE composite decreased with increasing
load; however, in the case of glass-fibre-reinforced PEI,
the effect of load on wear differed with counterface
roughness and no clear trend emerged. Liu et al.

41

reported that load is the most important factor in the
wear of unfilled UHMWPE specimens; however, for the
wear of filler reinforced UHMWPE composites, the role
of the load abates and the role of abrasive particle size
increases with the increase in filler particle size. On the
other hand, sliding speed seems to have little effect on the
total wear volume. Abrasive wear studies

60

of poly(aryl

ether ketone) PAEK and their composites, against silicon
carbide (SiC) abrasive paper, showed that wear volume
increases with the increase in load and sliding distance.
Liu et al.

61

observed that wear loss of PA and UHMWPE

blend is higher under dry-sliding conditions than
lubricated test conditions, and increases with load in-
crease. Li and Bell,

62

showed that the mechanical

properties and wear resistance of UHMWPE can be
improved by surface treatment with the active screen
plasma nitriding technique. Zhang et al.

63

reported that

tribological behaviour of plasma-treated PEEK and its
composites was improved. Indumathi et al.

64

found that

comparison of wear rates of treated and untreated
samples under various loads revealed that cryo-treatment
technique has potential to increase the wear resistance of
some polymers and their composites. Finally, Blanchet
and Peng

65

reported that wear resistance of fluorinated

ethylene propylene can be increased through electron
irradiation treatment.

The present paper investigates the ability of tribological

experiments to discriminate between different treatments
applied to crushed rubber microparticles to improve their
adhesion with a poly(carbonate) matrix. Additionally, it is
of interest to produce information on wear behaviour,
under variable normal load and sliding velocity, of such
new polymer composites having low impact on environ-
ment which proved to be suitable for smart applications.

Experimental

Materials

The material used in this study is a blend of poly
(carbonate) engineering wastes (rPC) from signalisation

panel cuttings by Self-Signal company (derived from
Makrolon 3103 commercial grade of Bayer company)
and of crushed tire rubber particles (CRs) from Delta-
Gom company. PC wastes were just ground at room
temperature to obtain millimetric pellets without any
additional treatment whereas rubber millimetric particles
were milled in liquid nitrogen to reduce their diameter
range down to 140 mm,w,315 mm after sieving. The fine
micrometric CR particles were then melt-mixed with
millimetric PC crushed pellets. The density of CR
measured with a pycnometre was d50?840. Two types
of surface treatments were carried out:

(i) firstly, a flame treatment proceeded to oxidise the

CR surface and obtain satisfactory level of
adhesion with poly(carbonate). This treatment
was performed with a propane blowtorch. The
flame temperature was about 800

uC and particles

were flamed during 1 min at a distance of
20 cm.

(ii) Second, a solvent washing with dichloromethane

or methanol was done to eliminate oil residues.
Particles were dispersed in solution under sonica-
tion and stirred at room temperature for 25 min.
Then the particles were filtered and dried under
vacuum at 40

uC for 30 min to remove remaining

solvent.

Main properties of PC can be found in Table 1,
additional data concerning recycled polymers are given
elsewhere.

1,24,35,36

Blend processing

PC/CR blends were melt-mixed in a BRABENDER 50
EHT internal mixer with contra rotating blades driven
by WINMIX software. Polymers were dried under
vacuum for 24 h at 90

uC before processing. PC matrix

and CR particles were mixed with a rotor speed of
V540 rev min

2

1

at a temperature of T5240

uC for

10 min. These optimised blending conditions allowed
a good dispersion of CR into PC. Just after mixing,
blends were hot pressed T

mould.

5

240

uC, p

mould.

5

50 bar,

t

mould.

5

5 min to provide 4 mm thick plates which were

cooled down to room temperature in approximately
15 min. Normalised samples of 10610 mm were cut out
of plates with a small numerical milling machine. The
formulations used in this study were composed of 80%
PC/20% untreated CR, 80% PC/20% flame treated CR,
80% rPC/20% solvent treated CR.

Wear tests

Abrasion tests were conducted by the use of a
METKON Instruments machine that simulates a pin-
on-disc configuration. The schematic illustration of the
wear test apparatus is shown in Fig. 1 and described
elsewhere.

61,60,66

During abrasion experiments, polymer

samples

with

dimensions

of

1061064 mm

were

Table 1

Characteristics

of

virgin

and

recycled

poly

(carbonate)

vPC

rPC

Glass transition temperature T

g

/

uC

148

149

Young modulus E/GPa

2.3

1.95

Strain at breake

r

/%

100

5

Stress at breaks

r

/MPa

65–70

72

Thermal conductivity l/W m

2

1

K

2

1

0.21

…

Density (at 23

uC) d

1.2

…

Autay et al.

Wear behaviour of conductive eco-polymer composites

140

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abraded against waterproof (grit grade 600) SiC paper,
fixed on the rotating disc surface. The tests were carried
out at ambient temperature under water lubricating
condition. A constant lubricant flow was used in order
to avoid rip of the abrasive paper especially in the
beginning of the wear test. Samples were brought into
contact with abrasive paper under constant normal load.
The abrasive paper was changed before each test. Wear
rate, computed from weight loss of sample and averaged
on three separate tests, was measured at different times
by stopping the test. The wear rate (%) is calculated by
equation (1)

T ~

m

0

{m

t

m

0

(1)

where m

0

and m

t

are respectively mass of the sample

before and after a time t of wear.

An electronic scale with an accuracy of 10

2

3

g was

used to weigh samples. The abrasive wear test conditions
are detailed in Table 2.

Microstructure characterisation

Microstructures of worn surfaces, for the various CPCs,
were observed with different microscopes. Scanning
electronic microscopy observations were performed with
a JEOL JSM-6031 after fracture of samples in liquid
nitrogen and spray deposition onto the surface of a thin
gold layer. A LEICA DMLP optical microscope with
LIDA software in episcopy mode and non-polarised
light was used to observe worn surfaces of both paper
and composite.

Results and discussion

Effect of test conditions on wear properties

The effect of normal load on wear rate of a CPC with
untreated CR is shown in Fig. 2. It can be seen that the
wear rate increases linearly with sliding time (proportional

to sliding distance through equation (2)). These results are
in agreement with those found by Shipway and Ngao

46

for

poly(methyl methacrylate) samples

d~

2pRvt

60

(2)

where R55 cm, t is the time (s) and v is the rotation speed
(rev min

2

1

).

The application of a normal load of 40 N generates a

significant increase in the wear rate compared to a
loading of 20 and 10 N; this evolution can be explained
by the heavy damage of PC matrix by ploughing and
cutting action of abrasive particles at higher load. It was
noticed that curves do not start from zero, then two
slopes are distinguished: the one with higher value,
indicating a maximum speed of wear, located in the
interval of time (0–1 min) and the other lower value
(thus a low wear speed) spread out over the remaining
wear time. This phenomenon can be explained by the
fact that the first contact of the material with virgin
abrasive paper (Fig. 3a) will generate necessarily a
maximum tearing off of the material during the first
minute, then the active surface of the paper will be
covered by an adherent layer (formed by wear debris,
the area outlined in Fig. 3b) whose thickness increases
with wear time. Moreover, most grains lose their
sharpness by crushing, some of them being torn off.
This supports the reduction of wear speed and explains
the decrease in wear kinetics with wear time, whatever
the loading.

Figure 4 illustrates the effect of sliding velocity on the

wear rate of CPC with untreated CR. It shows a linear
increase in wear rate with the increase in sliding velocity
and a decrease in the kinetics of wear is noticed, in the
course of the wear time, for all speeds. It should be
noted that the heat accumulated in the wear process
causes thermal softening of the polymer, and repeated
sliding causes massive tearing and rupture of the surface
layer. Indeed, the variation of the wear rate is more
marked for high sliding velocity values (220 or
270 rev min

2

1

), which is in agreement with the results

found by Wang and Sliding

54

describing the effect of

sliding velocity on wear loss.

Effect of CR treatment on CPC wear behaviour

Preliminary tests were carried out under 5 N and
50 rev min

2

1

(mild conditions) for four CPC only

differing by CR particles treatment.

1

Pin-on-disc wear test configuration

Table 2

Experimental conditions for abrasive wear tests

Load/N

5, 10, 20, 40

Sliding velocity of disc/rev min

2

1

50, 170, 220, 270

Sliding velocity of disc/m s

2

1

0.26, 0.89, 1.15, 1.41

Testing time/min

1 to 6

Testing length/m

15.7 to 508.9

Lubricant flowrate/m

3

s

2

1

2.16610

2

5

Abrasive paper roughness R

a

/mm

30

Abrasive paper grit grade

600

2

Evolution of wear rate with normal load

Autay et al.

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As shown in Fig. 5, the CPC with CR washed by

CH

2

Cl

2

wears very quickly (wear rate equals to 100% at

the end of less than 2 min) and it presents the highest
kinetics of wear. This fast degradation of the material
can be explained by the absence of the adherent layer
formed by wear debris on the counter face, unlike other
CPCs, which leads to the specimen being directly in
contact with a clean abrasive surface; then the mechan-
ism of wear changes and the wear loss increases
significantly. Moreover, it is likely the dichloromethane
washing has partially swollen PC matrix changing
surface roughness and probably also degrading it. The
fast degradation of the CPC with CR washed by CH

2

Cl

2

makes the study reserved exclusively for the CPC that
showed an abrasion resistance (CPC with CR flamed
and washed with methanol).

It should be noted that the results found for the

evolution of wear properties with test conditions in the
case of the CPC with CR flamed or washed by methanol
are similar to those found for CPC with untreated CR.
Thus it can be concluded that 5 N load only makes it
possible to evidence the effect of washing solvent but not
to compare the influence of other treatments.

Figures 6 and 7 show that the CPC with flamed CR

has the lowest resistance to abrasive wear. However, the
CPC with CR washed with methanol has always the
lowest wear rate. It should be noted that washing with
methanol eliminates the residues of grease and any trace
of moisture being able to generate chains breakage by
hydrolysis for example or appearance of air bubbles in
the composite. This treatment was also found to
improve adhesion between PC and CR in another

study,

36

in the same way flaming contributes although

less importantly to the improvement of the interface
quality. Scanning electron and optical micrographs of
abraded surfaces under 10 N load and 50 rev min

2

1

sliding velocity (Figs. 8 and 9) show the presence of
porosities or internal cavities due probably to the
imprisonment of air bubbles in the mixture and the
presence of a phenomenon of wrenching of CR particles
which proves that treatments have no significant
influence on the reduction of these phenomena. In
addition, deep furrows in the abrading direction due to
the ploughing action by sharp abrasive particles are
illustrated. It is pointed out that the furrows appear only
under severe tribological conditions and they are
characteristics of abrasive wear.

Figure 10 represents the evolution of the wear rate as

a function of the applied loading for wear duration of

3

a

non-worn and b worn surface of abrasive paper (2006)

4

Wear rate as a function of sliding velocity of abrasive
disc

5

Wear rate of CPC as a function of type of applied
treatment

6

Wear rate of CPC as a function of applied treatment
under high speed

Autay et al.

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6 min. It is noted that the wear rate of various materials
makes a remarkable jump at a loading of 40 N and more
particularly the wear rate of CPC with flamed CR
increased more than those of others. Moreover, the
curves of kinetics of wear for the various materials
(Fig. 11) show an abrupt increase in the kinetics of wear
of the CPC with flamed CR while passing to a loading of
40 N. The low wear resistance of flamed CR filled CPC
is thought to result from its higher rigidity, i.e. Young
modulus determined by tensile tests.

36

In fact, hetero-

geneous materials with high rigidity can less easily
accommodate slip, which will weaken their wear
resistance. Additionally

nanoindentation tests have

shown that CPC filled with flamed CR presented the

lowest hardness and the weakest resistance to diamond
indenter depression, which can be compared to the
action of silica grains on paper surface during wear
tests.

35

As the abrasive wear resistance is an increasing

linear function of the material’s hardness,

67

the wear

rate increase was considered to be acceptable for flamed
CR CPC, and then mechanical and wear rate results are
in good agreement.

Conclusion

In this study, wear experiments have been carried out
(with a pin-on-disc test under water lubrication) to
investigate the tribological behaviour of CPC obtained

a CPC with untreated CR; b CPC with CR washed with
methanol; c CPC with flamed CR

8

Optical micrograph of surfaces of wear after wear test
under

10 N

load

and

50 rev min

2

1

sliding

velocity

(6200)

a CPC with untreated CR; b CPC with CR washed with
methanol; c CPC with flamed CR

9

Scanning electron micrograph of surfaces of wear after
wear test under 10 N load and 50 rev min

2

1

sliding

velocity (6200)

10

Wear rate of CPC as a function of applied treatment
for t56 min (V550 rev min

2

1

)

7

Wear rate of CPC as a function of applied treatment
under high load

Autay et al.

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by the dispersion of crushed CRs into a recycled PC
matrix. In an eco-design approach, these plastic wastes
could be valued as smart materials for sensing

24

but their

further development could be limited by insufficient
mechanical properties

35

due to a poor interface between

CR and PC.

36

Tribological tests appear to be a good

(and cheap) alternative to qualify PC/CR interface as it
was able to discriminate between all surface treatments
applied to CR. As expected wear rate increases with load
and sliding velocity whatever the type of treatment
applied for rubber microparticles. The CH

2

Cl

2

treat-

ment led to very bad wear resistance, probably due to
the swelling of CR low mass macromolecules whereas
the flaming treatment was found to decrease CPC wear
properties

certainly

because

of

surface

damage.

Methanol treatment of CR provided the best compro-
mise between surface activation/degradation allowing us
to develop CPC with the best wear resistance for all
loading and sliding velocities. It is also noticed that the
kinetics of wear depends primarily on the nature of the
treatment applied to the CR particles. The examination
of micrographies showed that all CPC present almost
identical wear scars characterised by the presence of
internal

cavities,

wear

furrows and

CR

particles

wrenching.

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