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Experimental investigation on thermal electric and dielectric characterization for polypropylene
- 1. INTERNATIONAL JOURNAL OF Issue 2, March – April (2013), ©ISSN 0976 –
International Journal of Electrical Engineering and Technology (IJEET),
6545(Print), ISSN 0976 – 6553(Online) Volume 4,
ELECTRICAL ENGINEERING IAEME
& TECHNOLOGY (IJEET)
ISSN 0976 – 6545(Print)
ISSN 0976 – 6553(Online)
Volume 4, Issue 2, March – April (2013), pp. 01-12 IJEET
© IAEME: www.iaeme.com/ijeet.asp
Journal Impact Factor (2012): 3.2031 (Calculated by GISI)
www.jifactor.com ©IAEME
EXPERIMENTAL INVESTIGATION ON THERMAL ELECTRIC AND
DIELECTRIC CHARACTERIZATION FOR POLYPROPYLENE
NANOCOMPOSITES USING COST-FEWER NANOPARTICLES
Ahmed Thabet
Nano-Technology Research Centre, Faculty of Energy Engineering, Aswan University,
Aswan, Egypt
athm@hotmail.com
ABSTRACT
Cost-fewer nanoparticles (clay and fumed silica) have very poor cost and high ability
for changing polymer matrix characterization, therefore, an experimental investigation on
thermal effects of cost-fewer nanoparticles on electric and dielectric properties of
Polypropylene Nanocomposites is presented in this research. This is an experimental study
that has been carried out to characterize and state the effect of type’s concentration of
nanoparticles on the electric and dielectric nanocomposites materials. Namely, dielectric
spectroscopy has measured the relative permittivity and the loss tangent of Polypropylene
with and without nano-fillers. All measurements were carried out at variant frequencies and
temperatures (20°C, 40°C and 60°C). Different dielectric behavior was observed depending
on nanofiller type, nanofiller concentration and nanocomposite temperature.
Keywords: Polypropylene, Dielectric properties, Nano-composite, Nanoparticles, Polymers
1. INTRODUCTION
Nanotechnologies are present in a lot of domain since they are a great source of
innovation. They may have a powerful impact on development of advanced electrical and
electronic device. In the last decade many research teams from all over the world have
focused their energies toward studies on polymer nanocomposites as effective materials for
electrical insulation. These materials, also called nanodielectrics, are usually made of
polymers uniformly filled, from 1 to 10 wt. %, with particles with at least one dimension
from 1 to 100 nm. The increasing interest in the behaviour of these newly born dielectrics is
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mainly due to the fact that these materials possess huge filler – polymer matrix interface
which has a major influence on the electrical, thermal and mechanical properties [1-6].
Dielectric materials of nanoscale dimensions have aroused considerable interest. It has been
mentioned two examples. First, in the semiconductor industry, in order to keep pace with
Moore’s law scaling, the thickness of the gate oxide dielectric material is reaching nanoscale
dimensions. Second, the high energy density capacitor industry is currently considering
dielectric composites with a polymer host matrix filled with inorganic dielectric nanoparticles
or polarizable organic molecules. The driving force for the former application is high
dielectric constants (or high-k), and those for the latter are high-k and/or high dielectric
breakdown strengths. [7-10].Recently, preliminary work has been already done to investigate
the capability of nanocomposite polymeric materials for electrical insulation to show
improved electrical performances with respect to the corresponding conventional materials,
possibly filled by micrograins or chemical additives. Very interesting properties, such as
reduction of space charge, variation of conductivity and increase of electric strength have
been detected in polyethylene-based materials and epoxy resin, doped with nano or
microfillers. It has been clarified already that nanomaterials, which have an average
crystalline size at least in one dimension between 1 and 100 nm, can interact with the
polymeric structure of an insulating material so as to achieve significant modifications with
respect to unfilled material properties. Such modifications are attributed, besides to the
presence of filler, to the much higher surface area to volume ratio associated with the
presence of nanoparticles with respect to micrometric-size fillers. However, there is some
published literature available on the use of nano-sized in insulating composites for dielectric
applications. Thus an investigation on the nanometric dielectric materials would find
usefulness in electrical insulation, electronics, MEMS, batteries etc. Electrical diagnostic
insulation testing is important from the point of low frequency applications. Several
investigations done by others on the nanocomposites for dielectric properties have reported
varied responses of frequency[11-16]. The use of polymers as electrical insulating materials
has been growing rapidly in recent decades. The base polymer properties have been
developed by adding small amounts of different fillers but they are expensive to the polymer
material. Recently, great expectations have focused on cost-less nanofillers, however, there
are few papers concerning the effect of types of cost-less nanofillers on electrical properties
of polymeric nanocomposite. With a continual progress in polymer nanocomposites, this
research depicts the effects of types and concentration of costless nanoparticles in electrical
properties of industrial polymer material [13-17]. Thisresearch is an experimental studythat
has been investigated the effects ofnanofiller types (clay, and fumed silica), nanofiller
concentration (1%wt, 5%wt, and 10%wt) and nanocomposite temperature(20oC, 40oC, and
60oC) on the dielectric properties of nanocomposite materials.
2. EXPERIMENTAL SETUP AND PREPARATION NANOCOMPOSITE
INDUSTRIAL MATERIALS
Nanoparticles: Nanoclay is nanomer 1.30E, clay surface modified with 25-30wt. %
octadecylamine. Spherical particle shape is the most important characteristic of nanoclay for
polymer applications. Nano fumed silica is a fluffy white powder with an extremely low
density, marketed under trade names. Fumed silica powders used in paints and coatings,
silicone rubber and silicone sealants, adhesives, cable compounds and gels, printing inks and
toner, and plant protection.
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Polypropylene Materials: Polypropylene is one of the most common and versatile
thermoplastics in the plastics industry. Filling polypropylene with a certain nanoparticles
greatly increases electrical, dielectrically, and mechanical properties, tensile strength, impact
strength, flexural modulus, and deflection temperature under load with a corresponding
reduction in elongation according to type and percentages of nanofillers. The industrial
materials studied here is Polypropylene which has been formulated utilizing variant
percentages of nano-particulates of clay and fumed silica.
Measurement Setup: HIOKI 3522-50 LCR Hi-tester device has been measured electrical
parameters of nano-metric solid dielectric insulation specimens at various frequencies.
Specification of LCR is Power supply: 100, 120, 220 or 240 V (±10%) AC (selectable), 50/60
Hz, and Frequency: DC, 1 mHz to 100 kHz, Display Screen: LCD with backlight / 99999
(full 5 digits), Basic Accuracy: Z: ± 0.08% rdg. θ: ± 0.05˚, and External DC bias ± 40 V
max.(option) (3522-50 used alone ± 10 V max./ using 9268 ± 40 V max.). It can be measured
all dielectric properties for pure and nanocomposite industrial materials by using HIOKI
3522-50 LCR Hi-tester device.Figure (1) shows HIOKI 3522-50 LCR Hi-tester device for
measuring characterization of nanocomposite insulation industrial materials.
Fig. 1 HIOKI 3522-50 LCR Hi-tester device
The base of all these polymer materials is a commercially available material already in use in
the manufacturing of high-voltage (HV) industrial products and their properties detailed in
table (1).
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Table (1) Electric and Dielectric Properties of Pure and Nano-Composite Materials
Materials Dielectric Resistivity
Constantat ( .m)
1kHz
Pure PP 2.28 108
PP + 1%wt Clay 2.21 109
PP + 5%wt Clay 1.97 109-1010
PP + 10%wt Clay 1.75 1010-1012
PP + 1%wt Fumed Silica 2.29 107
PP + 5%wt Fumed Silica 2.37 107-105
PP + 10%wt Fumed Silica 2.47 105-104
Preparation Nanocomposite: Preparation of studied Polypropylene nanocomposites have
been used SOL-GEL method by Additives of clay nanoparticles to the base industrial
polymers that has been fabricated by using mixing, ultrasonic, and heating processes. The
sol-gel processing of the nanoparticles inside the polymer dissolved in non-aqueous or
aqueous solution is the ideal procedure for the formation of interpenetrating networks
between inorganic and organic moieties at the milder temperature in improving good
compatibility and building strong interfacial interaction between two phases. This process has
been used successfully to prepare nanocomposites with nanoparticles in a range of polymer
matrices. Several strategies for the sol-gel process are applied for formation of the hybrid
materials. One method involves the polymerization of organic functional groups from a
preformed sol–gel network. The sol- gel process is a rich chemistry which has been reviewed
elsewhere on the processing of materials from glass to polymers. The organic–inorganic
hybrid nanocomposites comprising of polymer, and nanoparticles were synthesized through
sol–gel technique at ambient temperature. The inorganic phase was generated in situ by
hydrolysis–condensation of tetraethoxysilane (TEOS) in different concentrations, under acid
catalysis, in presence of the organic phase, polymer, dissolved in formic acid [17].
3. RESULTS AND DISCUSSION
Dielectric Spectroscopy is a powerful experimental method to investigate the dynamical
behavior of a sample through the analysis of its frequency dependent dielectric response. This
technique is based on the measurement of the capacitance as a function of frequency for a
sample sandwiched between two electrodes. The tan δ, and capacitance (C) were measured as
a function of frequency in the range 10 Hz to 50 kHz at 25°C for all the test samples. The
measurements were made using high resolution dielectric spectroscopy.
3.1 Effect of Cost-fewer Nanoparticles on Nanocomposite Polypropylene Characterization at
Room Temperature (25oC)
Figure 2.a shows loss tangent as a function of frequency for Clay/Polypropylene
nanocomposites at room temperature (25oC). The loss tangent of polypropylene decreases
with increasing clay nanoparticles percentage up to 1%wt, specially, at low frequencies but, it
increases with increasing clay nanoparticles percentage up to 10%wt, specially, at high
frequencies.Whatever, Figure 2.b shows the measured loss tangent with rising percentage of
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fumed silica nanofillers in the nanocomposite at room temperature (25oC). It is cleared that, the loss
tangent of Fumed silica/Polypropylene nanocomposite increases with increasing fumed silica
percentage nanofillers up to 10%wt, specially, at high frequencies.
0.005 0.005
PP+0%wt clay
0.004 PP+1%wt clay 0.004
PP+5%wt clay
0.003 0.003
PP+10%wt clay
Tan Delta
Tan Delta
0.002 0.002
PP+0%wt Fumed Silica
0.001 0.001 PP+1%wt Fumed Silica
PP+5%wt Fumed Silica
1E-17 1E-17
PP+10%wt Fumed Silica
1 10 100 1000 10000 100000 1 10 100 1000 10000 100000
-0.001 -0.001
Frequency (Hz) Frequency (Hz)
(a)Clay/PPnanocomposites (b)Fumed Silica/PPnanocomposites
Fig. 2 Measured loss tangent of Polypropylene nanocompositesat room temperature (25oC)
1.2E-09
6E-09
PP+0%wt Fumed Silica
1E-09 PP+0%wt clay 5E-09 PP+1%wt Fumed Silica
PP+5%wt Fumed Silica
8E-10 PP+1%wt clay PP+10%wt Fumed Silica
Capacitance (F)
4E-09
Capacitance (F)
6E-10 3E-09
4E-10 2E-09
2E-10 1E-09
0 0
1 10 100 1000 10000 100000 1 10 100 1000 10000 100000
Frequency (Hz) Frequency (Hz)
(a)Clay/PPnanocomposites (b)Fumed Silica/PPnanocomposites
Fig. 3Measured capacitance of Polypropylene nanocompositesat room temperature (25oC)
Figure 3.a shows capacitance as a function of frequency for Clay/Polypropylene nanocomposites at
room temperature (25oC). The capacitance of Clay/Polypropylene nanocomposite increases with
increasing clay percentage nanofillers up to 1%wt but it falls down with increasing nanofiller
percentage up to 10%wt. Figure 3.b contrasts on capacitance of fumed silica/Polypropylene
nanocomposites at room temperature (25oC). The measured capacitance of Fumed
silica/Polypropylene increases with increasing fumed silica percentage nanofillers up to 10%wt.
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3.2 Effect of Cost-Fewer Nanoparticles on Nanocomposite Polypropylene
Characterization at Temperature (40oc)
Figure 4.a shows loss tangent as a function of frequency for Clay/Polypropylene
nanocomposites at temperature (40oC). The loss tangent of Clay/Polypropylene increases
with increasing clay nanoparticles percentage up to 1%wt, specially, at low
frequenciesthen, the loss tangent decreases with increasing clay nanoparticles percentage
up to 10%wt, specially, at high frequencies. Figure 4.b shows loss tangent as a function of
frequency for Fumed silica/Polypropylene nanocomposites at temperature (40oC). The
loss tangent of Fumed silica/Polypropylene nanocomposite decreases with increasing
Fumed silica nanofillerspercentage up to 1%wt, specially, at low frequencies but, it
increases with increasing Fumed silica nanofillers percentage (1%wt -10%wt).
0.005 0.005
PP+0%wt clay PP+0%wt Fumed Silica
0.0045
PP+1%wt clay 0.004 PP+1%wt Fumed Silica
0.004
PP+5%wt Fumed Silica
PP+5%wt clay
0.0035 PP+10%wt Fumed Silica
0.003
PP+10%wt clay
0.003
Tan Delta
Tan Delta
0.0025 0.002
0.002
0.001
0.0015
0.001
1E-17
0.0005 1 10 100 1000 10000 100000
0 -0.001
1 10 100 1000 10000 100000 Frequency (Hz)
Frequency (Hz)
(a)Clay/PPnanocomposites (b)Fumed Silica/PPnanocomposites
Fig. 4 Measured loss tangent of Polypropylene nanocompositesat a certain temperature
(T=40oC)
Figure 5.a shows capacitance as a function of frequency for Clay/Polypropylene
nanocomposites at temperature (40oC). The measuredcapacitance of
Clay/Polypropylenenanocomposites increases with increasing clay nanofillerspercentage
up to 1wt%, then, it decreases with increasing clay nanoparticles percentage up to 10%wt.
Figure 5.b shows capacitance as a function of frequency for Fumed silica/Polypropylene
nanocomposites at temperature (40oC). The measured capacitance of Fumed silica
/Polypropylene nanocompositesincreases with increasing Fumed silica
nanofillerspercentage up to 10%wt.
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3E-09 3E-08
PP+0%wt
clay PP+0%wt Fumed Silica
2.5E-09 PP+1%wt 2.5E-08
clay PP+1%wt Fumed Silica
PP+5%wt
2E-09 clay 2E-08 PP+5%wt Fumed Silica
Capacitance (F)
Capacitance (F)
PP+10%wt Fumed Silica
1.5E-09 1.5E-08
1E-09 1E-08
5E-10 5E-09
0 0
1 10 100 1000 10000 100000 1 10 100 1000 10000 100000
Frequency (Hz) Frequency (Hz)
(a)Clay/PPnanocomposites (b)Fumed Silica/PPnanocomposites
Fig. 5 Measured capacitance of Polypropylene nanocompositesat a certain temperature
(T=40oC)
3.3 Effect of Cost-fewer Nanoparticles on Nanocomposite Polypropylene
Characterization at Temperature (60oC)
Figure 6.a shows loss tangent as a function of frequency for Clay/Polypropylene
nanocomposites at temperature (60oC).The loss tangent of Caly/Polypropylene
nanocomposites decreases with increasing clay nanoparticles percentages up to 10%wt,
specially, at low frequencies. Figure 6.b shows loss tangent as a function of frequency for
fumed silica/Polypropylene nanocomposites at temperature (60oC). The loss tangent of
Fumed silica/Polypropylene nanocomposite decreases with increasing fumed silica
percentage nanofillers up to 10%wt, specially, at low frequencies.However, Figure 7.a shows
capacitance as a function of frequency for Clay/Polypropylene nanocomposites at
temperature (60oC). The capacitance of Clay/Polypropylene decreases with increasing clay
nanofillers percentage up to 10%wt. Figure 7.b shows capacitance as a function of frequency
for fumed silica/Polypropylene nanocomposites at temperature (60oC). The capacitance of
Fumed silica/Polypropylene decreases with increasing fumed silica percentage nanofillers up
to 10%wt.
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0.005 0.005
PP+0%wt Fumed
PP+0wt% clay Silica
PP+1wt% clay 0.004 PP+1%wt Fumed
0.004
Silica
PP+5wt% clay PP+5%wt Fumed
PP+10wt% clay 0.003 Silica
0.003
Tan Delta
Tan Delta
0.002
0.002
0.001
0.001
1E-17
1E-17
1 10 100 1000 10000 100000
1 10 100 1000 10000 100000
-0.001
-0.001 Frequency (Hz)
Frequency (Hz)
(a)Clay/PPnanocomposites (b)Fumed Silica/PPnanocomposites
Fig. 6 Measured loss tangent of Polypropylene nanocompositesat a certain
temperature (T=60oC)
3.5E-09 3.5E-09
PP+0wt% clay PP+0%wt Fumed Silica
3E-09 3E-09
PP+1wt% clay PP+1%wt Fumed Silica
2.5E-09 PP+5wt% clay 2.5E-09
PP+5%wt Fumed Silica
Capacitance (F)
PP+10wt% clay
Capacitance (F)
2E-09 2E-09
1.5E-09 1.5E-09
1E-09 1E-09
5E-10 5E-10
0 0
1 10 100 1000 10000 100000 1 10 100 1000 10000 100000
Frequency (Hz)
Frequency (Hz)
(a)Clay/PPnanocomposites (b)Fumed Silica/PPnanocomposites
Fig. 7 Measured capacitance of Polypropylene nanocompositesat a certain temperature
(T=60oC)
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4. COMPARISON BETWEEN PURE AND NANOCOMPOSITE
POLYPROPYLENE CHARACTERIZATIONS
With respect to all results for depicting the effect of types of nanofillers, whatever,
adding fumed silica hasincreased permittivity of the new nanocomposite materials
whatever, adding clay has decreased permittivity of the new nanocomposite materials as
depicted in table (1).
Thus, comparing with all results for depicting the effect of raising concentration of
nanofillersat room temperature as shown in Figures (2,3), It can be shown that the loss
tangent of polypropylene decreases with increasing clay nanoparticles percentage up to
1%wt, specially, at low frequencies but, it increases with increasing clay nanoparticles
percentage up to 10%wt, specially, at high frequencies. Also, the loss tangent of Fumed
silica/Polypropylene nanocomposite increases with increasing fumed silica percentage
nanofillers up to 10%wt, specially, at high frequencies. Whatever, the capacitance of
Clay/Polypropylene nanocomposite increases with increasing clay percentage nanofillers
up to 1%wt but it falls down with increasing nanofiller percentage up to 10%wt. And so,
the measured capacitance of Fumed silica/Polypropylene increases with increasing fumed
silica percentage nanofillers up to 10%wt.Also, all results for depicting the effect of
raising concentration of nanofillers at 40oC is pointed out in Figures (4,5) and cleared that
the loss tangent of Clay/Polypropylene increases with increasing clay nanoparticles
percentage up to 1%wt, specially, at low frequencies then, the loss tangent decreases with
increasing clay nanoparticles percentage up to 10%wt, specially, at high frequencies.
Also, the loss tangent of Fumed silica/Polypropylene nanocomposite decreases with
increasing Fumed silica nanofillers percentage up to 1wt%, specially, at low frequencies
but, it increases with increasing Fumed silica nanofillers percentage (1%wt-10%wt).
Whatever, the measure capacitance of Clay/Polypropylene nanocomposites increases with
increasing clay nanofillers percentage up to 1%wt, then, it decreases with increasing clay
nanoparticles percentage up to 10%wt. And so, the measured capacitance of Fumed silica
/Polypropylene nanocomposites increases with increasing Fumed silica nanofillers
percentage up to 10%wt.
Finally, with respect to all results for depicting the effect of raising concentration of
nanofillers at 60oC is pointed out in Figures (6,7) wherever,the loss tangent of
Caly/Polypropylene nanocomposites decreases with increasing clay nanoparticles
percentage up to 10%wt, specially, at low frequencies. And so, the loss tangent of Fumed
silica/Polypropylene nanocomposite decreases with increasing fumed silica percentage
nanofillers up to 10%wt, specially, at low frequencies. Whatever, the capacitance of
Clay/Polypropylene decreases with increasing clay nanofillers percentage up to 10%wt.
And so, the capacitance of Fumed silica/Polypropylene decreases with increasing fumed
silica percentage nanofillers up to 10%wt.
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5. CONCLUSIONS
Modified polypropylene applications by nanotechnology composites depend on types,
concentration of nanoparticles and surrounded temperatures., Whatever, adding
fumed silica increases permittivity of the new Polypropylene nanocomposite materials
but, adding clay decreases permittivity of the new Polypropylene nanocomposite
materials.
Adding Clay nanoparticles, at room temperature (25oC), the loss tangent of
polypropylene decreases with increasing clay nanoparticles percentage up to 1%wt,
specially, at low frequencies but, it increases with increasing clay nanoparticles
percentage up to 10%wt, specially, at high frequencies. Whatever, the capacitance of
Clay/Polypropylene nanocomposite increases with increasing clay percentage
nanofillers up to 1%wt but it falls down with increasing nanofiller percentage up to
10% wt. But, at moderate and high temperatures (40oC:60oC), the loss tangent and
capacitance of Clay/Polypropylene decreases with increasing clay nanoparticles
percentage up to 10%wt, specially, at high frequencies.
Adding Fumed silica nanoparticles, At room and moderate temperatures (25oC:40oC),
the loss tangent and capacitance of Fumed silica/Polypropylene nanocomposite
increase with increasing fumed silica percentage nanofillers up to 10%wt, specially, at
high frequencies. But, at high temperatures (60oC), the loss tangent and capacitance of
Fumed silica/Polypropylene nanocomposite decrease with increasing fumed silica
percentage nanofillers up to 10%wt, specially, at low frequencies.
ACKNOWLEDGEMENTS
The present work was supported by the Science and Technology Development Fund
(STDF), Egypt, Grant No: Project ID 505.
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AUTHORS’ INFORMATION
Ahmed Thabet was born in Aswan, Egypt in 1974. He received the BSc
(FEE) Electrical Engineering degree in 1997 and MSc (FEE) Electrical
Engineering degree in 2002 both from Faculty of Energy Engineering,
Aswan, Egypt. PhD degree had been received in Electrical Engineering in
2006 from El-Minia University, Minia, Egypt. He joined with Electrical
Power Engineering Group of Faculty of Energy Engineering in Aswan
University as a Demonstrator at July 1999, until; he held Associate
Professor Position at October 2011 up to date. His research interests lie in the areas of
analysis and developing electrical engineering models and applications, investigating novel
nano-technology materials via addition nano-scale particles and additives for usage in
industrial branch, electromagnetic materials, electroluminescence and the relationship with
electrical and thermal ageing of industrial polymers. Many of mobility’s have investigated for
supporting his research experience in UK, Finland, Italy, and USA …etc. On 2009, he had
been a Principle Investigator of a funded project from Science and Technology development
Fund “STDF” for developing industrial materials of ac and dc applications by nano-
technology techniques. He has been established first Nano-Technology Research Centre in
the Upper Egypt (http://www.aswan.svu.edu.eg/nano/index.htm). He has many of
publications which have been published and under published in national, international
journals and conferences and held in Nano-Technology Research Centre website.
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