CuO) nanoparticles

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Synthesis, characterization and electrical insulation of polyester plasma sprayed by (CaO3Si/CuO) nanoparticles Dina M. Hamoda a, Sayed H. Kenawy b,⇑, Gehan T. El-Bassyouni b, Usama M. Rashed c, Gamal M. Turky d a

Textile Research Division National Research Centre, 33 El-Bohouth St, Dokki, Giza 12622, Egypt Refractories, Ceramics and Building Materials Department, National Research Centre, 33 El-Bohouth St, Dokki, Giza 12622, Egypt c Physics Department, Faculty of Sciences, Al-Azhar University, Cairo, Egypt d Department of Microwave Physics &Dielectrics, National Research Centre, 33 El-Bohouth St., Dokki, Giza 12622, Egypt b

a r t i c l e

i n f o

Article history: Received 15 November 2019 Accepted 3 December 2019 Available online xxxx Keywords: Plasma coating Polyester textile Dielectric barrier discharge Electrical insulation Ceramics

a b s t r a c t Textile fabrics possess multitude applications and a wide variety of highly technical uses. Microfiber is one of the most popular synthetic fibers. Its popularity is a result of special properties such as good resiliency, heat resistance, light weight, water proof and durability. In the present work, two woven fabrics were synthesized from polyester microfiber and then coated by calcium silicate/copper oxidenanoparticles, (CaO3Si/CuO)-NPs, using low temperature plasma (dielectric barrier discharge) technique. The coated textiles were investigated by Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray (EDX). A broadband dielectric spectroscopy (BDS) was employed to study the treatment conditions on the electrical and dielectric properties over a wide range of frequencies. The results showed that, the resistivity of the textile samples was remarkably enhanced upon coating with the (CaO3Si/CuO)-NPs) accompanied by a reduction of the static charges accumulated on the surface. These results made the plasma sprayed coated textiles promising for electrical applications like cables isolation as well as packing and packaging. Ó 2019 Elsevier Ltd. All rights reserved. Selection and peer-review under responsibility of the scientific committee of the International Conference on Nanoelectronics, Nanophotonics, Nanomaterials, Nanobioscience & Nanotechnology.

1. Introduction Electrical barrier of ceramic coating was designed to provide a high-quality, long-lasting impact for parts requiring electrical insulation. Electrical barrier is a durable, corrosion-resistant, dielectric spray on dielectric coating that provides unparalleled levels of adhesion and resistance to solvents and chemicals [1]. Textile coatings are a unique technology that imparts both flexibility and excellent wear resistance to the final coating. Nanotechnology for modern textile materials was used in several technical applications. One of the perspective areas was the dielectric applications, in which the new hybrid material will be more resistant to the electrical current flow or to operate as a part of an electric capacitor. Saad, et al., reported the amendment of the electrical properties of the nonwoven polyester fabrics prepared with and without the addition of activated carbons [2]. They displayed enhancement of the conductivity and the buildup of a ⇑ Corresponding author. E-mail address: [email protected] (S.H. Kenawy).

layer at the sample/electrode interface (usually called electrode polarization). Consequently, such action makes the nonwoven polyester a promising material for electrical energy storage technology in addition to the synthetic metals textiles usual applications [3]. There are different methods for textile coatings. One of the well-known methods was to functionalize the textile surfaces from basic textile finishing, dyeing/printing methods to laminate the nonwoven bonding techniques. In this case, textile surfaces were referred to any material intended for the textile usage, of both organic and inorganic origin. Textile coatings are used to add or alter the functionality of the textiles [4]. Functionality is the property of a substance that does not form covalent bonds or adhere to the fabric on its own. It is worthwhile to mention that, the decline of electrical conductivity of the textile to be more insulators has many fields of applications such as; electrical cables isolation, packing and packaging. The electrical resistivity of the textile can be enhanced by the addition of non-conductive coatings. A great development occurred since the production of synthetic fiber industry, was the production of very fine fibers like

https://doi.org/10.1016/j.matpr.2019.12.014 2214-7853/Ó 2019 Elsevier Ltd. All rights reserved. Selection and peer-review under responsibility of the scientific committee of the International Conference on Nanoelectronics, Nanophotonics, Nanomaterials, Nanobioscience & Nanotechnology.

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microfibers and nanofibers. Polyester fibers is one of the most popular synthetic fibers [5], its popularity was a result of special properties as good resiliency, heat resistance and chemical inertness. The fabrics produced from microfiber (whose width <1 detex) was characterized by its light weight, resisting wrinkling, durability, retain shape, waterproofness, resist pilling, luxurious drape body and breathability [6]. Dielectric and electrical properties of the investigated samples is the main topic of this study. The immense frequency range characterizes the broadband of dielectric spectroscopy (BDS), and makes it much more useful than other eminent spectroscopic techniques. The dielectric spectrum basically originates from different dynamic processes at the sub-molecular and molecular scales [7]. So, BDS was the foremost tool to study and gain information about different dynamic relaxation processes; mechanisms of charge carrier’s transportations, accumulation at the interfaces causing the interfacial polarizations [8]. The translational motion of the charge carriers reflected the conductivity contribution in the dielectric spectrum. It is redundant to say that the dielectric relaxation spectroscopy was just the response of the sample if an external electric field was applied [9]. In the present study, the electrical and dielectric parameters at a broad range of frequencies were interpreted. This is usually a superposition of different relaxation dynamic processes at molecular and sub-molecular scales due to the fluctuation of polar molecules and/or terminal or functional groups. In addition, there was a reflection of the charge carriers’ transportation causing conductivity or accumulated at the interphases in the composite materials or at the electrodes causing the electrode polarization. In textile industry, the plasma treatment technology was considered to be environmentally and economically talented. Furthermore, plasma treatments propose the option to obtain typical textile finishes deprived of changing the key textile properties. The efficiency of plasma treatment depends on: the nature of the textile and the treatment functioning conditions [10]. Plasmas can be categorized into cold and hot plasma liable on the temperature of the plasma zone. For the surface modification of textile materials, only low-temperature plasmas (LTPs) are proper [11]. Low temperature plasma can be generated in low pressure or in atmospheric pressure. Recently, efforts were directed to the development of non-thermal plasma reactors working at atmospheric pressure. One promising technology for producing atmospheric plasmas is based on the use of dielectric barrier discharge (DBD). It is a non-thermal discharge under atmospheric pressure which generates low-temperature plasma in the air, without the restriction of vacuum conditions. DBD refers to a kind of gas discharge in which plasma is separated from one or two electrodes by a dielectric barrier. It consists of a large number of microdischarges of short duration (in nanoseconds), which are randomly distributed in the gas gap. DBDs have high number of industrial applications because they operate at atmospheric pressure and does not require expensive high power supplies [12,13]. In addition, DBD in air is commonly used to treat polymer and textile surfaces to improve the wettability, printability and adhesion [14]. The chemical effect of plasma treatment consists of reactions between the plasma species and textile surface can form different polar groups, such as, –OH, C–O, C–OH, C@O etc. Such polar groups increase the surface energy and enhance the material wetting properties [15]. The main objective of the present work is to prepare polyester coated by (ceramic/CuO)-NPs using dielectric barrier discharge plasma (DBD) treatment of the textile materials. The effect of treatment conditions on the electrical and dielectric properties of the prepared samples using a wide range of frequencies was investigated using the broadband dielectric spectroscopy (BDS).

2. Material & methods 2.1. Fabric specification - Materials Selection: Two different microfiber polyester types (A & B) were used. - Design of Fabrics: Woven fabrics of weave type plain 1/1 & Warp yarn count: 70/1 denier were used. The conditions of the A & B fabrics were presented in the following Table 1. The Polyester textile samples were woven on a SULZER Projectile weaving, model machine, model TW-11with the following specifications: - Loom speed: 250 (ppm) – Max reed width: 160 (cm) – No. of harness frames; 6-Fabric structure: plain 1/1-Filling yarn counts: 150/1, 70/1-No of ends/cm: 36-No of ends/inch: 91No of picks/cm: 24, 30 picks cm with warp yarn count 70/1 denier. - Fabric Cover Factor (K): Cover factor (K) is a number that designates the degree to which the area of a fabric is covered by one set of threads. It also means the distance covered by the threads warps or wefts-in fabric [16] and is calculated as follows:

S K¼p N

ð1Þ

where, S is the threads per inch and N is the count. Cover factors of the fabrics are calculated for warp and weft, so pair of values can be quoted in descriptions of fabrics [Ahmed et al., 2018]. The chief value of cover factors comes from their continued use to establish familiarity. The fraction of the area covered by both sets of threads is given by the following equation:

K ¼ K1 þ K2 

K1K2 28

ð2Þ

where, K 1 = warp cover factor, K 2 = weft cover factor [17]. 2.2. Preparation and characterization of CaO3Si/CuO nanoparticles The calcium silicate doped with 10 M% CuO was prepared using pure limestone (calcium carbonate, CaCO3), silica gel (SiO2) and copper (II) carbonate (CuCO3), via the wet precipitation route. This method was considered as ingenious and financial method for the development of nanoparticles [18,19]. Homogenous gel formed after drying at 100 °C was fired at 550 °C for 2 h, then milled into fine powder using ball mill. The physicochemical characterization of the sample was undertaken by XRD (Bruker, D8 Advanced Cu target, Germany). Measurement was conducted over a diffraction angle at 2h range of 4–65°. The crystalline phases were recognized using the powder diffraction files. Pattern was drawn using the ORIGIN 8.0 software. Material was also examined via scanning electron microscopy SEM/supplemented with EDX (model Quanta 250, Holland). 2.3. Techniques Polyester textile were treated by Dielectric Barrier Discharge (DBD) plasma reactor. The schematic diagram of DBD reactor is shown in Fig. 1. It consists of two parallel plate electrodes. The upper electrode is an aluminum sheet of dimensions 25  25 cm2 pasted on a dielectric glass plate of thickness 1.5 mm and the lower electrode is a stainless-steel plate of the same dimensions. The gap distance between the two plates is 2 mm. Plasma discharges were

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D.M. Hamoda et al. / Materials Today: Proceedings xxx (xxxx) xxx Table 1 The characteristic features of the used Polyester Textile. Fabric ID

Weft Count

No of Filament

Denier per filament

Cover factor

Fabric Setting

Weight gm./m2

Warp Tensile strength (N)

Weft Tensile strength (N)

A B

1 50/1 70/1

144 144

1.04 0.4

18.5 14.9

36  30 36  24

82 84

44.7 42.6

17.2 23.2

* Denier: Is the weight in grams of 9000 Meters of a fiber, filament or yarn [Brody, H., Synthetic fiber materials, Longman Group UK, LIMITED, 1994].

Fig. 1. Schematic diagram of DBD cell used for polyester textile coating.

generated by a 25 kV/30 mA, AC power supply of frequency 50 Hz, connected to the upper electrode, while the lower electrode is connected to earth through a resistor R of 100 X or a capacitor C of 3.35 lf. The voltage across discharge electrodes was measured using a resistive potential divider (1:1000) connected in parallel with the discharge electrodes. The discharge current was estimated by measuring the voltage drop across the resistor R through a digital storage two channel oscilloscope (GWinsTEX GDs-1072-u, 70 MHZ). The dissipated power during the discharge has been estimated using a capacitor to calculate the charge flow through the reactor. Two samples of dimension 3  3 cm2 were cut from the two different microfiber polyester types (A & B) and about 0.5 g of the nanoparticles were sieved to cover the surface of the sample, then hand pressed to ensure homogeneously on the textile surfaces. Textiles covered with nanoparticles were placed in the gap between the two electrodes and DBD system was operated at air atmospheric pressure. For a period of 15 min, the plasma discharge power of 10.15 W was applied. The A & B textiles after being plasma sprayed were nominated as C & D respectively. Coated samples were investigated by Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray (EDX) (model Quanta 250, Holland). 2.4. Dielectric characterization The electrical conductivity and dielectric properties were performed in a parallel plate geometry using a broadband dielectric spectroscopy (BDS) via a high resolution Alpha analyzer with an active sample head (Novocontrol GmbH). All measurements were

carried out at ambient room temperature and frequency range of 0.1 Hz-20 MHz. Samples were sandwiched between two gold-plated brass electrodes of 20 mm diameter. The complex permittivity, e ð¼ e0  ie00 Þ was measured over the considered frequency range, where, e0 is the real part and e00 is the imaginary part. The equivalent complex conductivity r*(= r0 + r00 ) was deduced to study the different aspects of the underlying mechanisms of charge transport and molecular dynamics. The real part of conductivity characterized by a plateau yields the dc-conductivity ðrdc Þ at the lower frequencies and follows the universal power law on the higher frequencies. The determined rdc was the product of the mobility and the number density of charge carriers participating in the conduction process. This provides a novel possibility to determine the mobility and the active number density of charge carriers from the measured conductivity separately [20,21].

3. Results & discussion 3.1. Characterization of DBD reactor The voltage applied to the electrodes and the discharge current were measured using a resistive potential divider and the resistor R. Fig. 2 shows waveform of the applied voltage and the associated discharge current measured in air plasma at atmospheric pressure. The applied voltages and the discharge currents are phase-shifted by approximately 90°and the voltage followed the current. The reason for these two effects was the capacitive properties of the electrode configurations. The signal of the discharge current has

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15000

0.03

Current Voltage

Air 10000

0.01

5000

0.00

0

V(V)

I (A)

0.02

-0.01

-5000

-0.02

-10000

-0.03 0.00

0.02

-15000 0.04

time (sec) Fig. 2. Waveform of the applied voltage and the associated discharge current measured in air plasma at atmospheric pressure.

also a sinusoidal shape, but in addition several high frequency peaks are superimposed at the maximum amplitude. The high frequency peaks superimposed on the current signal originate from the ignited plasma. The individual peaks are very narrow, which corresponds to a short burning time of the individual filaments in the nanosecond range. This clearly indicated that the discharge regime was filamentary [22]. The filaments are uniformly distributed over the dielectric surface. They cross the discharge gap and spread on the surface of the dielectric barrier, building up surface charges, which produce electric field opposite to that of the applied voltage. After a short time (several ns), the filament activity in that spot was extinguished, followed by filament initiation in another location. The peak of each individual spike was related to the number of instantaneous microfilaments formed at this instant, and hence a high current spike indicates that a high number of micro discharges were simultaneously initiated. A simple method for obtaining the consumed power is using the discharge Lissajous figures, obtained by plotting transported electric charge Q through the discharge as a function of the applied periodical voltage [23,24]. The charge Q is delivered from the voltage drop across a measuring capacitor of 3.35 lF. The average electric energy dissipated in a discharge cycle is simply the area of the characteristic Lissajous figure, which is nearly a parallelogram [25]. Fig. 3 exhibits the Lissajous diagram plotted at applied voltage of 10 KV.

The dissipated power has been calculated by multiplying the area of the parallelogram by the frequency of the used AC power supply (50 HZ) to be 10.15 W. 3.2. Microstructure and energy dispersive X-ray (EDX) The typical morphological structure of the calcium silicate doped with 10% CuO studied by SEM was shown in Fig. 4. Generally, the sample showed an agglomerated interconnected irregular fragments-like shaped powder in the range of 31–40 nano sized particles. Consequently, the formation of nano sized particles was confirmed [26,27]. X-ray diffraction pattern (XRD) of the prepared CaO3Si/CuO)NPs composite, was revealed in Fig. 5. It illustrated the crystallization of quartz (JCPDS card № 82-1574, SiO2), wollastonite (JCPDS card № 76-1846, CaSiO3), Ca-olivine (JCPDS card № 80-942, Ca2SiO4) and tenorite (CuO) (JCPDS card № 01-080-1268). The peaks at 33, 35.4° and 38.7° were related to the tenorite [28–30]. Fig. 6 (C & D) showed a scale of different fine particles growing on the surface and in between the polyester fibers. The fine particles formed pits on the fiber surface. It can be detected that the nanoparticles wrinkled onto the fiber surfaces [31]. Consequently, it could be decided that the nano-particles were entrapped in between the yard structures in a strong condition and infused into the polyester fibers owing to the plasma action. The energy dispersive X-ray (EDX) analysis of the treated fabric was carried out to

Fig. 3. Lissajous diagram measured for Air plasma at atmospheric pressure.

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Fig. 4. SEM of calcium silicate powder doped with 10% CuO.

Fig. 5. XRD of calcium silicate incorporated with 10% CuO.

regulate the surface chemical composition upon coating using the plasma spray technique. The occurrence of Ca, Si, Cu, C & O on the surface of the treated fabrics were confirmed by the EDX analysis. 3.3. Dielectric and electrical investigations The real and imaginary parts of the complex dielectric constant,

e*(=e0 -ie00 ), were represented in Fig. 7 against frequency at room temperature for the four samples under considerations. At higher frequencies, the permittivity displayed stability. There is no remarkable effect neither of the frequency nor of the structure on e0 which has values ranging between 1.5 and 2.0 till about 100 Hz. The permittivity values showed spreading out with further decrease of frequency. This behavior was accompanied by a gradual increase with decreasing frequency. This usually reflected the effect of free charge carriers accumulated at the surface of the textile. Close inspection of the figure, showed the remarkable enhancement of the dielectric properties of the textile as the polyester samples were coated by nano-CS/CuO particles using the plasma technique (C & D) ever since the dielectric loss e00 values decreased. The high frequency displayed a small dynamic peak relaxation originated from the interfacial polarization usually found in most the multicomponent structures [32]. The removal of the static charges from the surface of the fabrics before coating (A & B) was the main feature of the coating by nano-CS/CuO particles

using plasma technique. The reduction of the dielectric loss in the inset Fig. 7a is a promising action in the shielding applications [33]. On the other hand, the frequency dependence of the conductivity (Fig. 7b) exhibited a reduction of conductivity of the samples by about one and two orders of magnitude. Such outcome reflected once again the improvement of the electrical insulation features after coating with the CaO3Si/CuO nano-particles. The resistivity of the investigated samples at low frequency point of 0.1 Hz that usually related to the dc-conductivity was represented in Fig. 8. The figure shows that the resistivity of sample A has lower value of resistivity than sample B. Temporarily, sample C revealed the highest resistivity value reflecting the much more homogenous distribution of the sub-micro-particles which became more efficient in comparison with sample D. The improvement of the dielectric and electrical insulation was clearer in sample A after being coated with CaO3Si/CuO-NPs, sample C, than that in case of sample B. This confirmed the less distribution of the submicron particles around the fibers in sample D which was found by the EDX characterization shown previously. The electric modulus which is the reciprocal permittivity (M* = 1/e*) was useful in the electrical characterization [34]. The 00

00

electrical loss modulus spectrum M00 (m) (M ¼ e0 2eþe}2 ) revealed sim-

ilar peaked behavior as the dielectric loss e00 (m). It could be analyzed in an analogous way. The analysis of the electric modulus peak made it possible to determine the hopping time of the charge

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A

C

B

D

Fig. 6. SEM of polyester fabrics (A, B) & SEM, EDX of the polyester coated by (CaO3Si /CuO)-NPs) particles using the plasma spray technique (C, D).

carriers. This provides time scale of transportation inversely related to the electric conductivity [35,36]. Fig. 9 illustrated graphically the determined imaginary part of electric modulus as a function of frequency. The steady increase in the dielectric loss at lower frequencies shown in the inset of Fig. 7a caused by ionic conduction was con-

verted to specific conduction peak. This peak showed shift towards lower frequencies for the coated samples i.e. the so-called conductivity hopping time, characterized by the frequency of the maximum peak position, became longer and the conductivity dynamic was slowed down. This outcome confirmed, once again, the effect of coating by the nano-ceramic/CuO particles on the enhancement

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D.M. Hamoda et al. / Materials Today: Proceedings xxx (xxxx) xxx

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Fig. 7. a The permittivity, e0 and dielectric loss, e00 as a function of frequency (as inset) b the conductivity (r0 ) as a function of frequency.

14

0.1 Hz

log ( [ .cm])

12 10 8 6 4 2 0

A

B

C

D

Fig. 8. The determined resistivity of the four fabrics at spot point frequency 0.1 Hz.

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Modulus''

0.1

0.01

0.001 -1 10

101

103

105

107

Freq. [Hz] Fig. 9. The electric modulus loss vs. frequency of the 4 fabrics.

of the insulation behavior of the two polyester textile samples. It is also noticed that this action in case of sample A to be C with more homogeneous distribution of nano-ceramic/CuO is more reliable than in case of B to be D. The shoulder shown at higher frequencies is due to the interfacial polarization. This is due to the accumulation of charge carriers at interfaces between different species in multicomponent materials. 4. Conclusion Woven fabrics made from polyester micro fiber when coated by (CaO3Si/CuO)-NPs) using low temperature plasma technique became more insulator and they have numerous fields of applications such as: electrical cables isolation, packing and packaging. Fabric (A) which has the higher cover factor has the ability of more (CaO3Si/CuO)-NPs) coating particles and showed more insulation feature than that of fabric (B) of lower cover factor. So, it is found that the improvement of the electrical insulation was clearer in sample A when coated with (CaO3Si/CuO)-NPs) particles than that in case of sample B. This confirmed the less distribution of the submicron particles around the fibers in sample B which was found because of its low covering factor. Author contributions The authors are shared equally in this work. Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper. References [1] R. Ghasemi, H. Vakilifard, Plasma-sprayed nanostructured YSZ thermal barrier coatings: Thermal insulation capability and adhesion strength, Ceram. Int. 43 (2017) 8556–8563. [2] M.A. Saad, M.F. Nasr, H.A. Yassen, G.M. Turky, Electrical and dielectric properties of stitched non-woven engineered fabrics containing activated carbon fiber, Egypt. J. Chem. 61 (3) (2018) 559–568. [3] C. Mostert, B. Ostrander, S. Bringezu, T.M. Kneiske, Comparing electrical energy storage technologies regarding their material and carbon footprint, Energies 11 (3386) (2018) 2–25.

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Please cite this article as: D. M. Hamoda, S. H. Kenawy, G. T. El-Bassyouni et al., Synthesis, characterization and electrical insulation of polyester plasma sprayed by (CaO3Si/CuO) nanoparticles, Materials Today: Proceedings, https://doi.org/10.1016/j.matpr.2019.12.014