experimental investigation on thermal electric and dielectric characterization for polypropylene

International Journal of Electrical Engineering and Technology (IJEET), ISSN 0976 –

6545(Print), ISSN 0976 – 6553(Online) Volume 4, Issue 2, March – April (2013), © IAEME

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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

[email protected]

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

INTERNATIONAL JOURNAL OF ELECTRICAL ENGINEERING

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ISSN 0976 – 6545(Print) ISSN 0976 – 6553(Online) Volume 4, Issue 2, March – April (2013), pp. 01-12

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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

Constantat

1kHz

Resistivity

(Ω.m)

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.

Fig. 2 Measured loss tangent of Polypropylene nanocompositesat room temperature (25oC)

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.

-0.001

1E-17

0.001

0.002

0.003

0.004

0.005

1 10 100 1000 10000 100000

Tan

Del

ta

Frequency (Hz)

PP+0%wt clay

PP+1%wt clay

PP+5%wt clay

PP+10%wt clay

(a)Clay/PPnanocomposites

(b)Fumed Silica/PPnanocomposites

-0.001

1E-17

0.001

0.002

0.003

0.004

0.005

1 10 100 1000 10000 100000

Tan

Del

ta

Frequency (Hz)

PP+0%wt Fumed Silica






0

2E-10

4E-10

6E-10

8E-10

1E-09

1.2E-09

1 10 100 1000 10000 100000

Cap

acit

ance

(F

)

Frequency (Hz)

PP+0%wt clay

PP+1%wt clay

0

1E-09

2E-09

3E-09

4E-09

5E-09

6E-09

1 10 100 1000 10000 100000

Cap

acit

ance

(F

)

Frequency (Hz)







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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).

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.



0

0.0005

0.001

0.0015

0.002

0.0025

0.003

0.0035

0.004

0.0045

0.005

1 10 100 1000 10000 100000

Tan

Del

ta

Frequency (Hz)

PP+0%wt clay

PP+1%wt clay

PP+5%wt clay

PP+10%wt clay

-0.001

1E-17

0.001

0.002

0.003

0.004

0.005

1 10 100 1000 10000 100000

Tan

Del

ta

Frequency (Hz)







7

Fig. 5 Measured capacitance of Polypropylene nanocompositesat a certain temperature (T=40

oC)

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 (60

oC). 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.

0

5E-10

1E-09

1.5E-09

2E-09

2.5E-09

3E-09

1 10 100 1000 10000 100000

Cap

acit

ance

(F

)

Frequency (Hz)

PP+0%wt clay

PP+1%wt clay

PP+5%wt clay



0

5E-09

1E-08

1.5E-08

2E-08

2.5E-08

3E-08

1 10 100 1000 10000 100000

Cap

acit

ance

(F

)

Frequency (Hz)







8

Fig. 6 Measured loss tangent of Polypropylene nanocompositesat a certain temperature (T=60oC)

Fig. 7 Measured capacitance of Polypropylene nanocompositesat a certain temperature (T=60oC)



-0.001

1E-17

0.001

0.002

0.003

0.004

0.005

1 10 100 1000 10000 100000

Tan

Del

ta

Frequency (Hz)

PP+0wt% clay

PP+1wt% clay

PP+5wt% clay

PP+10wt% clay

-0.001

1E-17

0.001

0.002

0.003

0.004

0.005

1 10 100 1000 10000 100000

Tan

Del

ta

Frequency (Hz)

PP+0%wt Fumed SilicaPP+1%wt Fumed SilicaPP+5%wt Fumed Silica



0

5E-10

1E-09

1.5E-09

2E-09

2.5E-09

3E-09

3.5E-09

1 10 100 1000 10000 100000

Cap

acit

ance

(F

)

Frequency (Hz)

PP+0wt% clay

PP+1wt% clay

PP+5wt% clay

PP+10wt% clay

0

5E-10

1E-09

1.5E-09

2E-09

2.5E-09

3E-09

3.5E-09

1 10 100 1000 10000 100000

Cap

acit

ance

(F

)

Frequency (Hz)






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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 (25

oC:40

oC),

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.

experimental investigation on thermal electric and dielectric characterization for polypropylene

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