Composites: Part B 69 (2015) 145153

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

Effect of crystallite size of zinc oxide on the mechanical, thermal and

flow properties of polypropylene/zinc oxide nanocomposites
Saisy K. Esthappan

a,b

, Ajalesh B. Nair , Rani Joseph

a,

Department of Polymer Science and Rubber Technology, Cochin University of Science & Technology, Cochin 682 022,
b
India Department of Chemistry, Mangalam College of Engineering, Ettumanoor 686 631, India

article info
Article history:
Received 24 September 2012
Received in revised form 9
June 2013 Accepted 12 August
2013
Available online 20 August
2013

A.
B.
B.
E.

Keywords:
Nano-structures
Mechanical properties
Thermal properties
Compression moulding

abstract
ZnO nanoparticles were prepared using zinc chloride and sodium hydroxide in chitosan
medium. Pre-pared ZnO (NZO) and commercial ZnO (CZO) was characterized by scanning
electron microscopic and X-ray diffraction studies. PP/ZnO nanocomposites were prepared
using 05 wt% of zinc oxide by melt mixing. It was then compression moulded into films.
Transparency of the composite films were improved by reducing the crystallite size of ZnO.
Melt flow index studies revealed that NZO increased the flow char-acteristics of PP while CZO
decreased. X-ray diffraction studies indicated a-form of isotactic polypropyl-ene. An increase in
mechanical properties, dynamic mechanical properties and thermal stability of the composites
were observed by the addition of ZnO. Uniform dispersion of the ZnO was observed in the
scanning electron micrographs of the tensile fractured surface of composites.
2013 Published by Elsevier Ltd.

1. Introduction
Polymer nanocomposites have attracted great attention
due to their enhanced mechanical strength and thermal
properties at low filler loadings [13]. Now a days,
nanostructured versions of conventional inorganic fillers
are used in plastic composites. There are many reports on
the enhancement of properties of polymer by adding
inorganic nanofillers [47]. Recently, nanocomposites
based on PP matrix constitute a major challenge for
industry as they represent the route to substantially
improve the mechanical and physical properties of PP. PP
is one of the most widely used thermoplastic polymers due
to its good physical and mechanical properties as well as
the ease of processing at a relatively low cost. There are a
number of investigations on the PP nanocomposites filled
with different types of fillers such as carbon nanotubes [8
10], nanoclay [11,12], talc, mica and fibrous fillers.
The enhanced properties are due to the synergistic
effects of nanoscale structure and interaction of fillers with
polymers. The size and structure of the dispersed phase
significantly influence the properties of polymer
nanocomposites [13]. Recently, there are some studies on
the influence of micro- and nano-sized ZnO on the
properties of PP [14,15]. Morphology of the filler also plays
a major role on the properties of a polymer.

Corresponding author. Tel.: +91 484 2575723; fax: +91 484

2577747. E-mail address: rani@cusat.ac.in (R. Joseph).

http://dx.doi.org/10.1016/j.compositesb.
2013.08.010 1359-8368/ 2013
Published by Elsevier Ltd.

2.2. Methods

In this work, we investigated the effect of crystallite size

and morphology of ZnO on mechanical, dynamic
mechanical, transpar-ency, morphology, thermal and flow
properties of the PP/ZnO com-posites prepared by melt
mixing.
2. Experimental
2.1. Materials
Isotactic PP homopolymer (REPOL H200MA) with melt
flow index of 25 g/min was supplied by M/s. Reliance
Industries limited.

2.2.1. Preparation of zinc oxide

Zinc oxide nanoparticles were prepared by reacting
zinc chlo-ride and sodium hydroxide in chitosan medium.
In this method zinc chloride (5 g in 500 ml 1% acetic acid
in water) was added to chitosan (5 g in 500 ml 1% acetic
acid in water) with vigorous stir-ring using mechanical
stirrer. This was allowed to react for 24 h. During this
period, stabilization of the complex take place. Then
sodium hydroxide (25 g in 500 ml 1% acetic acid in water)
was added drop wise from burette to the above solution
with stirring using mechanical stirrer. The whole mixture
was allowed to digest for 12 h at room temperature. This
was to obtain homogeneous dif-fusion of OH _ and Cl_ to
the matrix. The precipitate formed was washed several
times with distiled water until complete removal

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S.K. Esthappan et al. / Composites: Part B 69 (2015) 145153

of sodium chloride and dried at 100 LC. Then

it was calcined at 550 LC for 4 h.
2.2.2. Preparation of PP/ZnO composites:
compression moulding
The melt compounding was performed
using a Thermo Haake Polylab system
operating with counter rotating screws at 40
rpm for 8 min at 170 LC with a capacity of 60
3

cm . Composites of differ-ent concentrations

(05 wt%) of ZnO were prepared. The hot mix
immediately pressed after mixing using a
hydraulic press. The samples were then made
into films using compression moulding at 180
LC for 6 min in an electrically heated hydraulic
press.
2.2.3. Mechanical properties of PP/ZnO
composites
Mechanical properties of the compression
moulded samples of PP and PP/ZnO
composites were studied using a Universal
testing machine (UTM, Shimadzu, modelAG1) with a load cell of 10 kN capacity. The
specimens used were rectangular strips of
dimen-sions 10 _ 1 cm. The gauge length
between the jaws at the start of each test was
adjusted to 40 mm and the measurements
were carried out at a cross-head speed of 50
mm/min (ASTM D 882).
2.2.4. Dynamic mechanical analysis (DMA)
DMA studies were carried out on
rectangular shaped specimens of dimensions
3 _ 1 cm by temperature sweep (temperature
ramp from 30 LC to 150 LC at 3 LC/min)
method at a constant frequency of 1 Hz. The
dynamic storage modulus, loss modulus and
tan d were measured.
2.2.5. Scanning electron microscopy
The morphology of the tensile fractured
surface of PP and com-posites was studied
using scanning electron microscope (JOEL
model JSM 6390 LV).
2.2.6. Thermogravimetric analysis
Thermogravimetric analyzer (TGA Q-50,
TA instruments) was used to study the effect
of ZnO on the thermal stability of PP.
Approximately 10 mg of the samples were
heated at the rate of 20 LC/min from ambient
to 800 LC in nitrogen atmosphere.
2.2.7. Melt flow index (MFI) measurements
MFI of the composites were studied using
CEAST melt flow modular line indexer (ITALY)
at 190 LC and 2.16 and 5 kg wt. A pre-heating
time of 6 min is given before each experiment.
The weight of the substance extruded in 10
min in grams is then measured.
2.2.8. X-ray diffraction studies
X-ray diffraction studies were carried out
using Rigaku Geiger-flex at wavelength Cu Ka

= 1.54 . Crystallite size of ZnO was calculated using Debye Sherrer equation:

CS 0:9k=b cos h
where CS is the crystallite size, b is the full
width at half-maximum of an hkl peak at h
value, h is the half of the scattering angle.
3. Results and discussion
3.1. X-ray diffraction studies of zinc oxide
XDD pattern of NZO and CZO is shown in
Figs. 1a and 1b respec-tively. The figures
show the characteristics peaks of hexagonal
crystal structure. The peaks obtained
correspond to (100), (002), (101), (102), (110),
(103), (112), (201), (004), (202), (104) planes.
The (101) plane is most prominent. The
crystallite size of

41.2 N/mm

at 1.5 wt% CZO and tensile

2

modulus from 1105.75 to 1422.9 N/mm at 0.5

wt% of CZO. The increase in properties may
be due to the interface inter-action between
nanoparticles and a polymer matrix that can
trans-fer stress, which is beneficial for the
improvement of the tensile strength of
composite films. However, with increasing
content of nanoparticles, aggregation occurs,
which leads to a decrease in the contact area
between the nanoparticles and polymer matrix
and results in the formation of defects in the
composites.
Fig. 1a. XRD pattern of ZnO prepared in
chitosan medium.

Fig. 1b. XRD pattern of commercial

ZnO.

ZnO are calculated using Debye Sherrer

equation is 13.4 nm for NZO and 29.2 nm for
CZO.
3.2. Scanning electron micrographs of zinc
oxide
Scanning electron micrographs of two ZnO
which is taken for the study are shown in Fig.
2. Similar morphologies and different particle
sizes are seen in SEM. ZnO shown in Fig. 2a
depicted as NZO and Fig. 2b is denoted as
CZO. Both show sphere like morphol-ogy and
small particles are observed in the scanning
electron micrographs of NZO when compared
to CZO.
3.3. Mechanical properties of PP/ZnO
composites
Figs. 3 and 4 show variation in tensile
strength and modulus of PP with ZnO content.
The incorporation of ZnO in the PP matrix
result in an increase in the tensile strength
and modulus. It reaches maximum at 1.5 wt%
concentration of ZnO and then decreases. In
the case of PP with NZO the tensile strength
2

gets increased from 31.75 to 44.37 N/mm

and tensile modulus from 1105.35 to 1897.02
2

N/mm at 1.5 wt% NZO. CZO filled PP shows

an increase in tensile strength from 31.8 to

S.K. Esthappan et al. / Composites: Part B 69 (2015) 145153

147

Fig. 2. Scanning electron micrographs of (a) NZO and (b) CZO.

Fig. 3. Effect of particle size of ZnO on tensile strength

of PP/ZnO composites.

Fig. 5. Effect of particle size of ZnO on elongation at

break of PP/ZnO composites.

and crystallite size of filler. ZnO with smaller

crystallite size shows better properties than
ZnO with higher crys-tallite size. Sphere like
morphology of NZO results in the uniform
distribution of ZnO particles in the PP and thus
improve the mechanical properties of PP.
Elongation at break (Fig. 5) of PP is
decreased by the addition of low concentration
of ZnO, at a higher concentration it is
increased.

Fig. 4. Effect of particle size of ZnO on modulus of

PP/ZnO composites.

Therefore, the effective interfacial interaction

is reduced, and the tensile strength of the
films gets decreased [6]. The mechanical
properties also depend on the dispersion of
nanoparticles in the matrix. The improvement
of tensile modulus and strength of PP/ ZnO
nanocomposites is related to the inherent
stiffness and quality of the dispersion of ZnO
[16,17]. NZO filled PP shows higher
mechanical properties than CZO filled PP.
This is due to the differ-ence in morphology

3.4. Dynamical mechanical analysis of

PP/ZnO composites
Dynamic storage modulus is the most
important property to assess the load-bearing
capability of a material. The storage mod-ulus
of neat PP and PP/ZnO nanocomposites as a
function of tem-perature at 1 Hz are shown in
Fig. 6. Storage modulus of the PP is increased
with the addition of ZnO. The increase in
storage mod-ulus is significant at low
temperature like 40 LC. The increase may be
due to the stiffening effects of ZnO and
efficient stress transfer between the polymer
matrix and nano ZnO.
The loss modulus of the PP and
composites are given in Fig. 7. The loss
modulus also increase substantially with the
ZnO concen-tration. Maximum improvement is
shown by PP with 1.5 wt% NZO. Composite of
PP with NZO shows significant improvement

com-pared to CZO. Reinforcing effect of ZnO

increases with decrease in crystallite size of
ZnO.

Fig. 6. Effect of ZnO on storage modulus of

PP/ZnO composites.

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S.K. Esthappan et al. / Composites: Part B 69 (2015) 145153

initial mixing and then dropped to stabilize a

line with higher mixing time.
This indicates a good level of mixing at the
specified conditions. Also the torque value of
the PP/NZO composites are higher than that
of neat PP and PP/CZO composites. This is
mainly due to the increase in interfacial
interaction between the nanoparticles and
polymer [18].

3.6. X-ray diffraction analysis of composites

Fig. 7. Effect of ZnO on loss modulus of

PP/ZnO composites.

XRD plots of neat PP and PP/ZnO

composites are given in Fig. 10. The peaks
obtained are corresponding to the planes
(110), (040), (130) represents a form of
isotactic PP. Gopinath et al. observed the
similar peaks in the XRD pattern of isotactic
PP [19]. X-ray dif-fraction pattern of
nanocomposites show sharp and highly
intense peaks whereas neat PP shows less
intense peaks. This may due to the
development of crystallinity in the polymer. In
both neat PP and PP with ZnO, the crystal
plane of PP is monoclinic.
3.7. Scanning electron micrographs (SEM) of
the nanocomposites

Fig. 8. Effect of ZnO on tan d values of

PP/ZnO composites.

The tan d curves of PP and composites are

shown in Fig. 8. It is evident from the figure
that there is an increase in tan d value on
addition of ZnO. This indicates an increase in
damping characteris-tics of the composites. It
is obtained in many cases that the
improvement of stiffness markedly decreases
the ductility. But PP/ZnO composite showed
increased stiffness without reduction in
ductility.

3.5. Torque studies

Fig. 9 indicates the variation of torque with
mixing time for neat PP and PP/ZnO
composites. Torque is increased rapidly during

Fig.
11ac
represents
the
SEM
photographs of fractured surfaces of neat PP,
composites of PP with NZO and CZO at 1.5 wt
% respec-tively. The SEM of PP with 1.5 wt%
NZO shows formation of fibre like structure
which results increase in mechanical
properties. Uni-form distribution of ZnO is
observed in the SEM photographs. Fig. 11d
and e shows SEM photographs of PP with
NZO and PP with CZO at 5 wt% respectively.
At higher percentage large particles are
observed due to the agglomeration of the zinc
oxide particles. This may be the reason for the
decrease in mechanical properties at higher
concentration.

3.8. EDAX of the composites

EDAX is used for identifying the chemical
composition of a specimen. Fig. 12 represents
the EDAX of neat PP, 1.5 wt% NZO filled PP
and 1.5 wt% CZO filled PP.
EDAX shows the presence of ZnO in the
PP matrix. EDAX of the composites shows the
peak compared to zinc and oxygen indicat-ing
the presence of ZnO in the composites.
Lighter elements such as hydrogen cannot be
observed in EDAX due to the beryllium window that isolates the cooled detector from the
vacuum system. So the peak of hydrogen is
not seen in the spectrum.
3.9. Thermogravimetric analysis (TGA)
Fig. 13 represents the thermogram of neat
PP and composites. The values are tabulated
in Table 1. Thermal stability of PP/ZnO

Fig. 9. Variation of torque with time during mixing.

neat PP and ZnO filled composites.

Fig. 10. X-ray diffraction pattern of

S.K. Esthappan et al. / Composites: Part B 69 (2015) 145153

Fig. 11. SEM images of fractured surface of (a) neat PP, (b) PP + 1.5 wt% NZO, (c) PP + 1.5 wt% CZO, (d) PP + 5 wt%
NZO, and (e) PP + 5 wt% CZO filled composites.

composites are greater than neat PP. The

properties studied by TGA indicate an
improvement in thermal stability of PP by the

addition of ZnO. Onset of degradation

(temperature at which degradation starts) is
increased by the addition of ZnO. The
increase is signifi-cant when the particle size
of ZnO decreases. Onset of degradation of
neat PP is 391 LC where as 1 wt% NZO

149

added PP is 422.7 LC. The temperature at

which maximum degradation takes place is
increased by the addition of ZnO. Rate of
degradation is decreased with filler loading.
The increase in thermal stability of the
compos-ites may be due to the strong
interaction between the ZnO and PP. TGA
studies show that inorganic fillers, which are
widely used industrially to improve the
mechanical properties of polymer materials,
have various effects on the thermal oxidation
of PP. Gilman [20] suggested that the thermal
stability of polymers in presence of fillers is
due to the hindered thermal motion of polymer chains.

3.10. Kinetic analysis of thermal

decomposition
CoatsRedfern method was used to study
the kinetics of thermal degradation of PP and
PP/ZnO composites [21]. This

method is an integral method and thermal

degradation functions for the CoatsRedfern
method are given in Table 2.
Thermogravimetric function g(a) and
activation energy (E) is obtained from the
equation:

lnga=T2& lnAR=UE1 _ 2RT=E

_ E=RT
1

where a is the decomposed fraction at any

temperature and is given as:

a Ci _ C=Ci _ Cf
where C is the weight at the chosen
temperature, Ci is the weight at initial
temperature, Cf is the weight at final
temperature, a is the heating rate, and E is the
activation energy for decomposition. Activation energy (E) can be calculated from the
slope of the curve and pre-exponential factor
(A) using the intercept value of the plot of ln
2
[g(a)/T ] against the reciprocal of absolute
temperature (1/T). The order of decomposition
reaction was measured using the best linear fit
of the kinetic curve and that gives the
maximum correlation coefficient. The form of
g(a), which best represents the experimen-tal
data gives the proper mechanism. From these
calculations it is observed that the Mampel
equation (_ln(1 _ a)) fits in well. The

150

S.K. Esthappan et al. / Composites: Part B 69 (2015) 145153

Fig. 12. EDAX of (a) neat PP, (b) PP + 5 wt% NZO, and (c) PP + 5 wt% CZO composites.

linear correlation coefficients suggest that the F1

model is the most appropriate to describe the
experimental results (Table 2).
From Table 3 it is clear that the activation energy
of PP increased with the addition of ZnO
nanoparticles. Activation energy (E) obtained for
neat PP is 126.52 kJ/mol, 1.5 wt% NZO added PP
is 136.84 kJ/mol. Significant increase in activation
energy
indicates
high
thermal
stability.
Representative plot of CoatsRed-fern equation for
neat PP, PP/1.5 wt% NZO and PP/3 wt% NZO is
shown in Fig. 14.

3.11. Melt flow index (MFI)

MFI gives an idea about the flow characteristics
of the ther-moplastics. It depends on the molecular

properties such as molecular weight and structure of

polymers [22]. Fig. 15a and b shows the effect of
ZnO on the MFI of PP at 5 kg and 2.16 kg
respectively. MFI of PP is decreased by the addition
of

the structure of nanoparticles was interconnected to

hinder the molecular motion of polymer chains [24].
CZO indicate a decrease in flow characteristics of
the polymers. In NZO filled PP, MFI is increased by
the addition of low concen-tration of NZO indicates
an increase in the flow properties of the polymers.
Adding the low concentration of nanoparticles may
provide a flow favouring orientation due to the small
size of NZO as depicted in Fig. 16. An increase in
MFI is reported when adding multi walled carbon
nanotube to PP [23]. After adding 1 wt% NZO to the
PP the MFI value decreases gradually. It indi-cates

3.12. Transparency of the films

The percentage transmittance of neat PP and
composites is given in Fig. 17. By the addition of
ZnO the transmittance of the film is decreased. NZO
filled PP films show higher

S.K. Esthappan et al. / Composites: Part B 69 (2015) 145153

151

Fig. 13 (continued)

Table 2
The mechanisms of solid-state thermal degradation reaction and
corresponding thermal degradation functions g(a).
g(a) = kt

Symbol

Deceleratory at curves
(a) Based on diffusion mechanism
D
2

a + (1 _ a)
[1 _ (1 _ a)

ln(1
1/3

1 _ (2/

2_

D
2

2/3

D4

3)a _ (1 _ a)
(b) Based on geometrical models
1/n
1 _ (1 _ a)
Rn

Rate controlling process

One-dimensional diffusion
Two-dimensional diffusion
Three-dimensional diffusion
Three-dimensional diffusion
(GistlingBrounshtein equation)
Phase-boundary reaction; n = 1, 2 and 3
(one, two and three dimensional,
respectively

(c) Based on order of reaction

_ln(1 _ a)

First order (Mampel equation)

Fig. 13. Thermogram of PP and PP/ZnO

composites.

Table 3
Apparent activation energy (E) and correlation coefficients (R)
for neat PP and PP/ZnO composites by CoatsRedfern method.

Table 1
Effect of ZnO particle size on the thermal stability of PP.
Concentration Temperature
of ZnO (%)
at which
maximum
degradation
take place
(LC)

0
0.5
1
1.5
2
3

Onset of
degradation
(LC)

End set of
degradation
(LC)

Residue
(%)

Sample name

Neat PP
PP + 0.5% NZO
PP + 1.5% NZO
PP + 3% NZO

0.999
0.999
0.999
0.999

126.52
134.73
136.84
133.61

NZO

CZO

NZO

CZO NZO

CZO NZO CZO NZO CZO

471.6
472.9
474.4
475.4
475.3
473.9

471.6
471.8
472.4
472.9
475.4
471.6

391.0
409.8
422.7
416.3
412.7
406.3

391.0
390.1
392.9
396.6
401.7
402.6

500.7
492.9
498.9
498.5
498.6
494.6

500.7
500.1
499.9
499.8
497.2
499.1

1.4
0.8
1.6
2.6
3.5
3.9

transparency when compared to CZO filled PP

films. As the crys-tallite size of ZnO decreases the
transparency of the composite film increases.

152

Fig. 14. Representative plot of CoatsRedfern equation for

neat PP and PP/ZnO nanocomposites.

S.K. Esthappan et al. / Composites: Part B 69 (2015) 145153

Fig. 17. Visible-IR transmittance of neat PP and

PP/ZnO composites.
(a) PP/NZO and (b) PP/CZO composites.

Fig. 15. Effect of ZnO particle size on the melt flow index
of PP using (a) 2.16 kg and
(b) 5 kg weight.

Fig. 16. Schematic representation of flow behaviour of

2006;66:88694.

4. Conclusion
NZO shows smaller crystallite size
compared to CZO. PP/ZnO composites are
prepared by melt mixing method. Mechanical
and dynamic mechanical properties of PP are
improved by the addition of ZnO. PP shows
better thermal stability in presence of ZnO.
NZO filled PP shows higher mechanical and
thermal properties than CZO filled PP and
neat polymer. X-ray diffraction studies of neat
PP and composites indicate the presence of a
phase of monoclinic PP. Melt flow index
increases by adding low concentration of NZO
whereas CZO added PP shows a decrease in
MFI. Transparency of the PP films is
decreased by the addition of ZnO. PP with
NZO filled film shows higher transparency
when compared to CZO filled PP films.

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