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INTRODUCTION
More and more requirements in nearly all applications
address the need for high temperature resistance and high
strength. Polymers that can fulll these requirements are
grouped together as high temperature resins. Polyetheretherketone (PEEK) and polyethersulphone (PES) are two
representative members of this group of polymers. PES is a
high temperature amorphous thermoplastic polymer having
all the strengths and weaknesses of an amorphous polymer.
PEEK on the other hand is a high temperature semicrystal-
POLYMER COMPOSITES2007
TABLE 1.
Grade
Source
Density
(g/cm3)
Melting temperature
(C)
Tg (C)
Victrex
BASF
1.3
1.37
340
340390
143
225
Material
Polyether-ether-ketone (PEEK)
Polyether-sulphone (PES)
here. Two different matrices and one ller were used in this
work. So the article provides a comparative study on how
matrix morphology can change the properties of the composites. Composites were analyzed by DMA (dynamic mechanical analysis), DSC (differential scanning calorimetry),
TGA (thermogravimetric analysis), and for their electrical
as well as thermal conductivity properties. The bulk properties of all the composites are very much dependant upon
the matrix, reinforcement, interface, surface properties of
the llers and matrix, crystallinity, size of the spherulites,
and transcrytallinity, etc. [8]. Mechanical properties were
analyzed by monitoring property changes in material with
respect to the temperature by DMA. Thermal analysis was
used to study the effects of ber content and bermatrix
adhesion in the composite. The interaction and adhesion
between the ber and matrix has a signicant effect in
determining the mechanical and physical behavior of the
ber composites [9].
EXPERIMENTAL
Materials
Two polymers were used in this work as matrix material.
Table 1 lists the characteristics of these polymers.
PEEK is a Victrex PEEK 450G and was provided by
Victrex. PEEK is a semicrystalline polymer and the repeat
unit is
TABLE 2.
Material
Carbon bers (CF)
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Grade
Source
Form
Density
(g/cm3)
Diameter
(m)
Length
(mm)
Aspect
ratio
HTA5131
TOHO Tenax
Fiber
1.76
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Xc
Qm Qc
100
mQx
(1)
In this equation, Xc is the degree of crystallinity in percentage, Qm and Qc are the experimentally obtained endothermic melting and exothermic crystallization enthalpies, respectively, m is the experimental weight content of the
PEEK matrix in the composite, and Qx is equal to 130 J/g is
the melting enthalpy value deduced for fully crystallized
PEEK [10].
Electrical Resistivity.
Electrical resistivity was measured by the instrument, Agilent 4339B High Resistance
Meter. This model is designed for measuring very high
resistance and related parameters of insulation materials. All
the measurements were made at 100 mV. The instrument
was calibrated according to manufacturers recommendations before use.
Thermal Conductivity. The thermal conductivity was
measured by an instrument, NETZSCH TCA 200-LT-A as
a function of temperature. This model is a computer-controlled instrument used to measure the thermal conductivity
of materials by the guarded heat ow meter method. The
test sample is placed between two heated surfaces controlled at different temperatures with a heat ow from the
hotter to the colder. The thermal resistance of the interfaces
between the sample and adjacent surfaces is reduced by
applying a coupling agent i.e. silicone heat sink compound.
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FIG. 2. (a) Storage modulus of pure PEEK and the composites with CF. (b) Storage modulus of CF-reinforced
PEEK composites after heating above Tg.
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FIG. 3.
The loss moduli represent the energy lost during deformation of the polymer. It is related to the viscous portion
of the elastomer. It provides information about the overall
exibility and the interactions between the components of
composite material.
Figure 4 shows the loss modulus for PEEK and PEEK/CF
where relaxation peak is located between 140 and
160C while a peak is located between 165 and 180C
representing cold crystallization. With the increase of the
CF in the matrix, the peaks of loss moduli are becoming
narrow and extended to the higher temperature side. The
FIG. 4.
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FIG. 5.
FIG. 6.
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FIG. 7.
FIG. 8.
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FIG. 9.
Thermal Properties
Figure 9 shows the DSC thermograms of PEEK and
PEEK/CF. These curves are the rst heating scans of the
matrix and the composites. At 140C plots shift upward.
This indicates the approach of the glass transition point of
the polymer and composites. Figure also shows one exothermic peak between 150 and 175C, and an endothermic
peak between 300 and 350C [17]. The exothermic peaks
appear due to the cold crystallization. In semicrystalline
polymers, above Tg, when chains have a lot of mobility,
they wiggle and squirm and try to gain enough energy to
move into very ordered arrangements. When chains are in
these crystalline arrangements they give off heat and an
exotherm can be seen in the DSC curve. Temperature at the
lowest point of this exothermic dip is called crystallization
temperature Tc and it is an indication that the material can
crystallize. For PEEK/CF this temperature lies between 150
and 160C. When heating is continued past Tc then an
endothermic peak can be seen. This peak indicates the
disappearance of the crystals [18]. Chains come out of their
ordered arrangement and begin to move around freely. The
peak temperature is the melting temperature (Tm) of the
material. For PEEK and PEEK/CF this temperature lies
between 340 and 350C. Both crystallization and melting
peaks are decreasing by the addition of bers, indicating an
effective association between ller and matrix. The percent
crystallinity calculated for pure PEEK, PEEK with 10% CF,
and PEEK with 35% CF is 10, 16, and 17%, respectively, by
DSC. It seems percentage of crystallinity is increasing by
the addition of bers. However, from rst heating scans of
the composites, it is not possible to have some nal statement about the effect of bers on crystallinity. But the
previous work of several authors has been reported that the
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POLYMER COMPOSITES2007
Electrical Resistivity
Presence of CFs render the polymers electrically conductive. Figure 13 shows the electrical resistivity, which is the
inverse of conductivity, of pure PEEK, PES, and their
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FIG. 10.
CF-reinforced composites. For PEEK composites a percolation threshold is observed near 35 wt% CF loading. A
sudden decrease in resistivity is observed at this point. For
PES composites a percolation threshold is observed near 10
wt% ller loading.
At lower ller loadings, ller particles act like conductive islands in a sea of electrically insulating polymer. As
more particles are introduced, the conductive particles become more crowded and are more likely to come in contact
with each other. At percolation threshold, a majority of ller
FIG. 11.
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FIG. 12.
FIG. 13.
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Electrical resistivity of the composites of PEEK and PES with CF at room temperature.
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FIG. 14.
FIG. 15.
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