Composites: Part B 43 (2012) 44–49

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Composites: Part B
journal homepage: www.elsevier.com/locate/compositesb

Hybrid effect of nanoparticles with carbon fibers on the mechanical and wear
properties of polymer composites
Guo-ming Lin, Guang-you Xie, Guo-xin Sui ⇑, Rui Yang
Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016, China

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

Article history: Polyetheretherketone (PEEK) composites reinforced with carbon fibers (CFs) and nano-ZrO2 particles
Received 25 December 2010 were prepared by incorporating nanoparticles into PEEK/CF composites via twin-screw extrusion. The
Received in revised form 20 March 2011 effects of nanoparticles on the mechanical and wear properties of the PEEK/CF composites were studied.
Accepted 20 March 2011
The results showed that the incorporation of nano-ZrO2 particles with carbon fiber could effectively
Available online 28 April 2011
enhance the tensile properties of the composites. The tensile strength and Young’s modulus of the com-
posites increased with the increasing nano-ZrO2 content. The enhancement effect of the particle was
Keywords:
more significant in the hybrid reinforced composites. The compounding of the two fillers also remarkably
A. Polymer-matrix composites (PMCs)
B. Wear
improved the wear resistance of the composites under water condition especially under high pressures. It
was revealed that the excellent wear resistance of the PEEK/CF/ZrO2 composites was due to a synergy
effect between the nano-ZrO2 particles and CF. CF carried the majority of load during sliding process
and prevented severe wear to the matrix. The incorporation of nano-ZrO2 effectively inhibited the CF fail-
ures through reducing the stress concentration on the carbon fibers interface and the shear stress
between two sliding surfaces. It was also indicated that the wear rates of the hybrid composites
decreased with the increasing applied load and sliding distance under water lubrication. And low friction
coefficient and low wear rate could be achieved at high sliding velocity.
Ó 2011 Elsevier Ltd. All rights reserved.

1. Introduction ness. SCFs also increase the creep resistance, hardness, compres-
sive strength of the PEEK composites; reduce their adhesion to
As a typical high performance thermoplastic polymer with high the counterpart and the frictional heat in the contact area. Further-
mechanical properties, chemical inertness, high wear resistance more, the fiber carries the main load between the contacting sur-
and easy processing, polyetheretherketone (PEEK) has been widely faces during the sliding process, so the PEEK composites
used as matrix material for high performance composites [1–6]. reinforced by the CFs show excellent wear resistance under water
However, in order to facilitate more applications under some se- lubrication [8] .
vere conditions, various micro or nanosized fillers are incorporated Nanoparticles reinforced polymer composites have attracted
into PEEK. more and more attentions [9–11]. The extremely high specific sur-
Fibers are thought to be the most effective reinforcement face area facilitates creating a great amount of interphase in com-
phases for polymer materials, and the fiber-reinforced composite posite and a strong interaction between the fillers and the matrix.
materials always show high mechanical performance. Especially, Thus, the nanocomposites always have unique properties resulting
carbon fibers (CFs) show superior properties such as higher from the nano-scale structures. Some nanometer inorganic fillers
Young’s modulus, better strength, better thermal conductivity, are demonstrated to have the ability in reducing the friction and
and more excellent electrical properties than other fibers [7]. enhancing the wear resistance of polymers. The inclusion of nano-
Therefore, CFs are currently the most extensively used reinforce- particles, such as Si3N4, SiO2, SiC and ZrO2, in PEEK is also for the
ments for composites because of their availability and reliability. purposes of processing ability and mechanical enhancement
The incorporation of CFs greatly improves the mechanical perfor- [10,12,13].
mances of PEEK composites [4,5,8]. It is well known that short car- Recently, some sub-micro/nanoinorganic particles were mixed
bon fibers (SCFs) reinforced PEEK composites are characterized by with SCFs to reinforce the polymer matrix. Hussain et al. [14] re-
reasonably high tensile modulus, strength and high fracture tough- ported the improvement of the mechanical properties of CFRPs
by the addition of nano- and micro-sized Al2O3. The incorporation
of the particles resulted in a higher fracture toughness by improv-
⇑ Corresponding author. Tel./fax: +86 24 83978040.
ing significantly the toughness of the matrix. According to Gilbert
E-mail address: [email protected] (G.-x. Sui).

1359-8368/$ - see front matter Ó 2011 Elsevier Ltd. All rights reserved.
doi:10.1016/j.compositesb.2011.04.029
 G.-m. Lin et al. / Composites: Part B 43 (2012) 44–49 45

et al. [15], rubber particle interlayer toughened composites exhib- 2.3. Mechanical properties
ited enhanced mode I and II fracture toughness and reduced water
sensitivity. Timmerman et al. [16] modified the matrices of CFRPs Tensile tests are carried out on a universal testing machine with
with nanoclays resulting in reduction of transverse cracking as re- a crosshead speed of 5.0 mm/min. A load cell of 20 kN and an
sponse to cryogenic cycling. Tanimoto and co-workers [17] found extensometer with a gage length of 25 mm are used. The parallel
that the damping properties and fatigue life of CFRPs were en- segment of the dumbbell-shaped specimens for tensile tests is
hanced by spreading PZT particles between their interlayers. This 30  5  4 mm3. For each specimen, the data reported here repre-
concept is attractive because the mixing multiple constituents sents the averaged result of at least five successful tests.
would enable the creation of higher performance materials.
It is believed that there is a synergistic effect of SCFs with fine 2.4. Wear test
particles on the enhancement of the wear resistance. The protec-
tion of SCF/matrix interface from the nanoparticles is supposed Wear tests are conducted on a MM-W1A universal wear testing
to be the main reason for the enhancement of the wear resistance machine (Jinan Shijin Co. Ltd.) using a three-pin-on-disk configura-
and a rolling effect of the nanoparticles between the counterpart tion. Both the cylindrical specimen pins (4.8 mm diameter and
pairs is also proposed. The wear properties and mechanism of 12.8 mm length) and the stainless steel counterpart disk (4Cr13,
the carbon fiber reinforced PEEK composite has been well studied HV476) are polished with 1500 grit SiC water-abrasive paper.
in some others reports [18,19]. However, the tribological behaviors The average roughness of the counterface (Ra) is 0.038 lm. All
and the wear mechanism of sub-micro/nanoinorganic particles the tests are carried out under ambient temperature over a period
compounding with the carbon fibers composites under water of 2 h at the sliding velocity of 2.0 m/s. The applied load is arranged
lubricated condition are still unclear and there is no report on it from 1 MPa to 8 MPa. The polymer–metal interface is immerged in
until now. tap water. Before and after the test, the pins are ultrasonically
The present work focuses on the wear behavior and mechanical cleaned and dried at 150 °C for 3 h for weighing. Then the mass loss
performance of CFs and nano-ZrO2 particles reinforced PEEK com- of the composite pins is measured by electronic balance (Mettler
posites. The effects of nanoparticles on the mechanical properties AE240, accuracy 0.01 mg) for the specific wear rate calculation.
of the PEEK/CF composites are studied. The specific wear rate is calculated after the test using the follow-
ing equation:
2. Experimental Dm
K¼ ð1Þ
qF N L
2.1. Materials
where Dm is the mass loss of the pins (mg), q is the density of the
The commercially available PEEK and PEEK/30%CF used in this pins (g/cm3), FN is the applied load (N) and L is the total sliding dis-
study is supplied by Degussa Co. Ltd. ZrO2 nanoparticles are sup- tance (m). Three replicate friction and wear tests are performed for
plied by Tianraoshiye Co. Ltd. The nanoparticles have an average each specimen to minimize data scattering and the average of the
size of 80 nm; the average diameter of SCFs is about 7 lm. three replicate test results is reported as the specific wear rate in
this work.
2.2. Specimen preparation
2.5. Morphological observation
The compounding of different fillers with PEEK is achieved by
using twin-screw extruder with a screw speed of 360 rpm under After the test, the tensile fracture surfaces, the worn surfaces of
processing temperature of 390 °C. All the materials are dried in the composites and the counterfaces are coated with a thin layer of
an oven at 150 °C for 6 h prior to melt processing. The extrudate gold and then examined using a JSM-6301F Scanning Electron
is continuously cooled by water and pelletized. The pellets are Microscope (SEM).
dried in oven at 150 °C for 6 h ready for injection molding. Stan-
dard test bars are injection molded with mold temperature at 3. Results and discussions
180 °C.
The compositions of the PEEK composites groups are listed in 3.1. Effect of the ZrO2 nanoparticles on mechanical properties
Table 1. For the purpose of comparison, neat PEEK, PEEK compos-
ites filled individually with 10, 15, 20 wt%CF and 10, 15, Table 1 shows the results of mechanical properties of PEEK and
20 wt%ZrO2 are also injection molded. PEEK composites. It can be seen that the tensile strength and the
Young’s modulus are evidently enhanced by the addition of the
Table 1 two fillers. The ascending trend with the increasing filler loading
Mechanical properties of PEEK and PEEK composites. of tensile strength and Young’s modulus can be found. It is evident
that CFs are the main reason for the increased tensile strength. The
PEEK/CF/ZrO2 Tensile strength Young’s modulus Fracture strain
(wt%) (MPa) (GPa) (%) addition of the ZrO2 nanoparticles also increases the tensile
strength and Young’s modulus of the composite. The incorporation
100/0/0 98 ± 1 3.7 ± 0.1 21.6 ± 0.9
90/0/10 103 ± 1 3.9 ± 0.1 19.9 ± 4.3 of 20% ZrO2 leads to a rise of 7.82% in the tensile strength com-
85/0/15 104 ± 1 4.2 ± 0.1 16.0 ± 2.6 pared with neat PEEK.
80/0/20 106 ± 1 4.3 ± 0.1 10.5 ± 3.7 However, the reinforced effect of ZrO2 is more effective for the
90/10/0 145 ± 2 9.4 ± 0.3 2.9 ± 0.1 hybrid composites. The PEEK/10CF/10ZrO2 composites show an in-
80/10/10 161 ± 2 10.4 ± 0.6 3.1 ± 0.2
crease of 16.50% and 28.19% in tensile strength and Young’s mod-
85/15/0 157 ± 1 11.9 ± 0.4 2.3 ± 0.1
80/15/5 186 ± 2 12.8 ± 0.8 2.4 ± 0.3 ulus, respectively, with comparison to that of PEEK/10CF
75/15/10 191 ± 1 13.7 ± 0.7 2.2 ± 0.4 composite. Meanwhile, adding of 10% ZrO2 into neat PEEK can only
70/15/15 195 ± 7 15.1 ± 0.6 2.2 ± 0.8 increase 4.82% and 5.90% in strength and modulus compared with
80/20/0 175 ± 3 14.1 ± 0.3 1.8 ± 0.1
neat PEEK. Obviously, there is a synergistic effect of ZrO2 and CFs
70/20/10 216 ± 1 17.8 ± 0.6 2.0 ± 0.3
on the enhancement of the mechanical properties. This could be
46 G.-m. Lin et al. / Composites: Part B 43 (2012) 44–49

convinced by the relationship of tensile strength and Young’s mod-

ulus versus the ZrO2 content for the PEEK/CF composites with var-
(a) 225
PEEK/ ZrO2/ 15CF
ious CF loading, as shown in Fig. 1. It is clear that the increasing

Tensile strength MPa

trend is sharper as the CF content increasing from 0% to 20%. The 210
reinforcing effect of ZrO2 particles is more effective with higher
content of CFs. 195
The adding of 5% ZrO2 into PEEK/CF composites always leads to
a large enhancement in the mechanical properties. Taking PEEK/ 180
15CF series as an example (as shown in Fig. 2), the compounding
of 5% ZrO2 into PEEK/15CF leads to a sharp increase of the tensile
165
strength from 156.74 MPa to 185.67 MPa. However, the enhance-
ment of the composite is not so effective for a high ZrO2 loading
composite. Although the ascending trend does not change, the ten- 150
sile strength only increases by 3.31 MPa with ZrO2 increasing form 0 5 10 15 20
10% to 15%. ZrO2 content wt%

3.2. Effect of filler on the tribological properties (b)

18 PEEK/ ZrO2/ 15CF

Tables 2 and 3 show the coefficients of friction and wear rate of

Young's modulus GPa

PEEK/CF/10ZrO2 composites with various amounts of CF under dif- 16
ferent applied load in water condition. It is evident that the coeffi-
cient of friction and wear rate of the PEEK/10ZrO2 increase as the
14
load increasing. Contrarily, the incorporation of CF significantly im-
proves the tribological performances of the composites. Both coef-
ficient of friction and wear rate decrease dramatically with the load 12
increasing. This implies that the tribological properties of the
PEEK/10ZrO2 composites severely deteriorate at high load due to
10
lack of the protection of CFs. It should be noted that the friction test
for the PEEK/10ZrO2 composite could not be carried out at the load
0 5 10 15 20
ZrO2 content wt%

(a) 220 PEEK/ ZrO2 Fig. 2. Variation of (a) tensile strength, and (b) Young’s modulus of the 15%CF
PEEK/ ZrO2/ 10CF composites as a function of the ZrO2 content.

200 PEEK/ ZrO2/ 15CF

Tensile strength MPa

PEEK/ ZrO2/ 20CF

180 Table 2
The coefficient of friction of PEEK/CF/10ZrO2 composites (103).

160 PEEK/CF/ZrO2 1 MPa 2 MPa 4 MPa 8 MPa

90/0/10 7.2 ± 4.2 78 ± 13 316 ± 88
140 80/10/10 13.3 ± 6.1 10.4 ± 1.4 4.4 ± 2.0 11.7 ± 0.7
75/15/10 13.2 ± 7.6 3.8 ± 1.2 4.8 ± 3.9 6.0 ± 2.7
120 70/20/10 4.9 ± 2.6 11.4 ± 5.7 4.3 ± 2.9 4.2 ± 1.7

100
0 5 10 15 20 Table 3
ZrO2 content wt% The wear rate of PEEK/CF/10ZrO2 composites (106 mm3 N1 m1).

PEEK/CF/ZrO2 1 MPa 2 MPa 4 MPa 8 MPa

(b) 18 PEEK/ ZrO2 90/0/10 0.47 ± 0.08 3.56 ± 2.08 43.5 ± 20.7
PEEK/ ZrO2/ 10CF 80/10/10 0.20 ± 0.07 0.12 ± 0.04 0.06 ± 0.01 0.030 ± 0.004
75/15/10 0.21 ± 0.07 0.12 ± 0.04 0.07 ± 0.02 0.029 ± 0.008
PEEK/ ZrO2/ 15CF
Young's modulus GPa

15 70/20/10 0.12 ± 0.06 0.08 ± 0.04 0.04 ± 0.01 0.02 ± 0.01

PEEK/ ZrO2/ 20CF

12

higher than 4 MPa due to severe vibration of the test machine

9
caused by the high frictional force, so no wear test date under
8 MPa is given. It is apparent that the PEEK composites containing
6 CFs exhibit better wear resistance, especially under high pressures
in water.
3 In order to identify the wear mechanism of PEEK composites
0 5 10 15 20 and the effect of CFs and load on the wear rate, the morphologies
ZrO2 content wt% of the worn surfaces of PEEK/10ZrO2 and PEEK/10CF/10ZrO2 com-
posite at 1 MPa and 4 MPa are observed by the SEM, as shown in
Fig. 1. Variation of (a) tensile strength, and (b) Young’s modulus of the composites Fig. 3. It can be seen that the worn surfaces of PEEK/10CF/10ZrO2
as a function of the ZrO2 content with different CF level. composite for both conditions are characterized with mild plowing
 G.-m. Lin et al. / Composites: Part B 43 (2012) 44–49 47

Fig. 3. The typical morphology of the worn surfaces for PEEK/10CF/10ZrO2 (a and b) and PEEK/10ZrO2 (c and d) composite under 1 MPa (a and c) and 4 MPa (b and d). Test
conditions: water lubricated; sliding velocity, 2 m/s; sliding duration, 2 h.

and microsurface damage caused by mild fatigue wear. This indi- particles into the composites increases the coefficient of friction
cates that the main wear mechanism of the hybrid PEEK compos- slightly. The increase of the pressure leads to evident decline of
ites is mild abrasive and fatigue wear. From Fig. 3, it could also the wear rate. Moreover, the wear rates of the composites are obvi-
be found that there are only mild plowing and microcrack on the ously influenced by the nano-ZrO2 content. The incorporation of
worn surface of PEEK/10ZrO2 composite at 1 MPa. However, obvi- 5 wt% nano-ZrO2 leads to the decrease in the specific wear rates
ous scuffing and plastic deformation, along with wear debris on of the PEEK/10CF composites. Then the wear rates slightly rise with
the worn surface of PEEK/10ZrO2 composite at 4 MPa indicates a nano-ZrO2 content increasing to 10 wt% and keep nearly un-
severe wear at high load without CFs. This is consistent with the changed until 15 wt%. With further addition of the nano-ZrO2,
high wear rate for the PEEK/10ZrO2 composite under 4 MPa. Those the wear rate drops remarkably and reaches the lowest value. It
observations imply that CFs support most stress during the sliding looks like that the ZrO2 nanoparticles and CFs worked synergisti-
process, so that the hybrid composites show outstanding wear cally on the wear behavior of the hybrid composites, since the hy-
resistance. brid composites with the proper ZrO2 content achieves a lower
Tables 4 and 5 show the coefficients of friction and wear rates of wear rate.
PEEK/10CF/ZrO2 composites with different content of ZrO2 nano- The worn surfaces of PEEK/10CF composite and PEEK/10CF/
particles. It can be seen that the coefficients of friction of PEEK/ 5ZrO2 composite at 8 MPa are illustrated in Fig. 4 to confirm the
10CF composites are all below 0.01. The incorporation of the nano- above description. Fiber thinning, debonding and breakage could
be found on both worn surfaces. However, with the incorporation
Table 4 of nanoparticles, less fiber removal could be observed on the worn
The coefficient of friction of PEEK/10CF/ZrO2 composites(103). surface for the hybrid composite. It is well known that the wear
PEEK/CF/ZrO2 1 MPa 2 MPa 4 MPa 8 MPa performance of the SCFs reinforced polymer composites are gov-
90/10/0 3.5 ± 1.3 3.7 ± 2.1 5.5 ± 3.4 5.7 ± 1.6 erned mainly by the process of fiber thinning, fiber breaking and
85/10/5 30.5 ± 10.2 5.2 ± 0.8 6.5 ± 1.2 6.3 ± 3.4 fiber peeling off under dry sliding. The fiber removal plays an
80/10/10 16.1 ± 5.2 10.4 ± 1.4 4.4 ± 2.0 9.3 ± 4.2 important role in the wear mechanism. Because the matrix would
75/10/15 11.8 ± 2.4 7.1 ± 3.5 6.4 ± 1.4 10.1 ± 7.4 be subjected to more intensive micro-ploughing and micro-cutting
70/10/20 19.2 ± 0.1 10.1 ± 1.3 12.2 ± 0.2 5.2 ± 2.5
and more wear of the matrix could occur after the fiber peeling-off
from the surface. It could be seen that the worn surfaces with
nanoparticles are much smoother and the CFs breakage, debonding
Table 5 and peeling-off are greatly restricted with the addition of 5% nano-
The wear rate of PEEK/10CF/ZrO2 composites (106 mm3 N1 m1). ZrO2 at 8 MPa. This should be the main reason for the superior
PEEK/CF/ZrO2 1 MPa 2 MPa 4 MPa 8 MPa wear resistance of the PEEK/10CF/ZrO2 composite in present condi-
tion. Similar results were also reported for the wear behavior of
90/10/0 0.19 ± 0.08 0.11 ± 0.01 0.047 ± 0.007 0.025 ± 0.003
85/10/5 0.15 ± 0.03 0.07 ± 0.03 0.034 ± 0.009 0.018 ± 0.002 polymer composite reinforced by short carbon fibers and fine par-
80/10/10 0.20 ± 0.07 0.14 ± 0.01 0.06 ± 0.01 0.030 ± 0.004 ticles under dry sliding condition [20], where a synergistic effect of
75/10/15 0.26 ± 0.02 0.12 ± 0.01 0.06 ± 0.02 0.03 ± 0.01 short carbon fibers with fine particles on the enhancement of the
70/10/20 0.08 ± 0.01 0.04 ± 0.01 0.022 ± 0.006 0.017 ± 0.007 dry sliding wear resistance was proposed.
48 G.-m. Lin et al. / Composites: Part B 43 (2012) 44–49

Fig. 4. The morphology of the worn surfaces of PEEK/10CF/ZrO2 (a) and PEEK/10CF (b) composite at 8 MPa. Test conditions: water lubricated; sliding velocity, 2 m/s; sliding
duration, 2 h.

Table 6 0.08 0.12

The mass loss of PEEK/CF/ZrO2 composites under different loads (mg).
coefficient of friction of composite
Mass loss/ 90/ 85/ 80/10/ 75/10/ 70/10/ 75/15/ 70/20/ wear rate of composite 0.10

-1
Wear rate,10 mm (Nm)
mg 10/0 10/5 10 15 20 10 10

Coefficient of friction
0.06
1 MPa 0.19 0.16 0.22 0.22 0.08 0.23 0.13 0.08

3
2 MPa 0.22 0.15 0.25 0.22 0.10 0.26 0.19
4 MPa 0.19 0.14 0.28 0.26 0.11 0.28 0.17

-6
8 MPa 0.21 0.12 0.27 0.28 0.16 0.27 0.16 0.04 0.06

0.04
0.02
3.3. Effect of sliding condition on the tribological properties 0.02

The weight losses of hybrid composites at the load from 1 MPa 0.00 0.00
to 8 MPa are almost at the same level less than 0.3 mg, as shown in 0.0 0.5 1.0 1.5 2.0 2.5
-1
Table 6. Commonly, the applied load affected the wear behaviors in Sliding velocity, ms
many ways. The sliding between materials would result in heat
generation and hence increased the temperature of two frictional Fig. 5. Effect of sliding velocity on the tribological properties of the PEEK/20CF/
10ZrO2 composite.
surfaces. A high applied load always led to high temperature rise
at the rubbing surfaces under dry sliding condition. Thus the poly-
mer surface might be plasticized and followed by a decrease in the
carrying capacity, which facilitate the polymer to be detached eas- The coefficient of friction and wear rate of PEEK/20CF/10ZrO2
ily and resulted in severe wear. However, for the case of reinforced composite as a function of sliding distance are shown in Fig. 6. It
composites, the wear rate is almost not affected by the load until a indicates that the wear rates of the hybrid composites decrease
critical value. Besides, water could act as a cooling agent at present with the increasing sliding distance under water lubrication.
case, which means that the friction induced thermal and mechan- Although the mechanism is still unclear, it is apparent that the hy-
ical effects might be inhibited in the aqueous environment. Actu- brid composites are suitable for the long duration application in
ally, the temperature rises of the water at various loads are all water condition.
less than 10 °C in present condition for all hybrid composites,
which denoted that the heat could be efficiently dissipated out of
the sliding surface by water. Furthermore, since the mass losses
of the composites at different applied loads are all at the same le- 0.05 10
vel, the specific wear rates of the composites show a decreasing coefficient of friction of composite
Wear rate,10-6 mm3(Nm)-1

trend with the pressure increasing. wear rate of composite

0.04
Coefficient of friction

The coefficients of friction and wear rates of PEEK/20CF/10ZrO2

1
composite at high and low speed are shown in Fig. 5. It is clear that
a low coefficient of friction and low wear rate could be achieved at 0.03
high sliding velocity. Basically, the presence of water in the friction
surface could result in fluid film lubrication, boundary lubrication, 0.1
or a mixture of the two [21]. Speed is important not only because 0.02
of its major role in both the viscoelastic response to stress and the
generation of friction heat, but also because the lubricated model is 0.01 0.01
partly determined by the sliding speed [8]. A hydrodynamic lubri-
cating film could be formed at high speed. In fact, at very low
speed, the lubricated wear rates of some polymers are approaching 0.00
1000 10000
the values characteristic of unlubricated sliding and thus lubrica-
Sliding distance, m
tion is becoming almost ineffective [22]. The low coefficient of fric-
tion and wear rate might result from the effective lubrication came Fig. 6. Effect of sliding distance on the coefficient of friction and wear rate of the
from the high speed. PEEK/20CF/10ZrO2 composite.
 G.-m. Lin et al. / Composites: Part B 43 (2012) 44–49 49

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