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Vol. 8. Issue 4.
Pages 3596-3602 (July - August 2019)
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Vol. 8. Issue 4.
Pages 3596-3602 (July - August 2019)
Original Article
DOI: 10.1016/j.jmrt.2019.05.022
Open Access
Effect of CuO nanofiller on the spectroscopic properties, dielectric permittivity and dielectric modulus of CMC/PVP nanocomposites
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Naziha Suliman Alghunaim
Department of Physics, Faculty of Science, University of Jeddah, Jeddah, Saudi Arabia
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Abstract

System of nanocomposite films containing carboxymethyl cellulose (CMC) and polyvinyl pyrrolidone (PVP) embedded copper oxide (CuO) nanoparticles were synthesized using the casting method solution and it was described by appropriate techniques. The semicrystalline nature of the structure for the nanocomposites was confirmed by X-ray spectra. The main characteristic bands of IR groups of CMC and PVP were clearly founded in the IR spectra. The intensity of some bands was reduced confirms a well reacts between CuO the main IR groups inside CMC/PVP polymer were occurring. The estimations of M′ were studied according to the conduction phenomenon related to short-range mobility of charge carriers. Minimum values of M″ at lower frequency were attributed to the indication of transport for ions with one relaxation peaks were founded which increase with an increase of CuO attributed to the relaxation process. The presence of a semicircle shape in the relation between M′ and M″ was observed demonstrating the presence of broad relaxation processes. The behaviour of ɛ′ was reduced as an increase of the frequency ascribed to polarization effects and it reaches to constant values at a higher frequency according to the contribution for charge accumulation. The behaviour of Z′ and Z″ was reduced as the increase of frequency as well as CuO. The magnitude of tanδ was also reduced because the hopping of charge carriers does not cause any changes of the applied field.

Keywords:
CMC/PVP nanocomposites
CuO nanoparticles
X-ray
FT-IR
Dielectric permittivity
Dielectric modulus
Full Text
1Introduction

Polymer nanocomposites can be communicated as materials contain modest amounts of nanoparticles fillers are appropriated in polymers homogenously by the various amount [1,2]. As compared with micro composites, the nanocomposites refer to nanometers in size normally under 100nm. Where different with nine orders in their number density while three orders of the amount in length. So, the distance in nanocomposites between neighbouring additives as compared with micro composites is much smaller. Therefore, in nanocomposites, the interaction of fillers with polymers is expected to be much more [3,4].

Nanocomposites are a novel fabrication material refers to a hopeful field in nanoscience. Besides these properties, it demonstrates the amazing advantages of structure, electrical, optical, biocompatibility, and biodegradability in various industrial, medical, drug release packaging, and agricultural applications. Inside polymer blends the filler of nanoparticles interaction between them to form molecular bridges for nanocomposites [5,6]. This is the origin for improved structural, electrical and optical properties of the nanocomposite as identified with customary smaller scale micro composites [7,8].

Carboxymethyl cellulose (CMC) is synthetic from cellulose. It discovers use in numerous industrial parts (for example, paper, pharmaceuticals, food, agriculture, barriers, and so on.) because of its high viscosity. CMC is hygroscopic, and it well soluble in hot or cold water to obtain a viscous solution. The CMC has great compatibility with other water-soluble, glues, softeners, and resin [9,10].

Polyvinyl pyrrolidone (PVP) is a vinyl polymer containing planar and essentially polar side groups in the ring. The PVP has a semicrystalline nature with a high glass transition temperature (Tg) considering the vicinity in pyrrolidone group [11,12].

Copper oxide (CuO) has been concentrated as a p-type semiconductor material with limited band hole due to the regular wealth of its beginning material, minimal effort creation preparing, nontoxic nature, and its sensibly great electrical and optical properties [13–15]. CuO nanoparticles are of extraordinary enthusiasm because of its potential applications in a wide assortment of zones including electronic and optoelectronic gadgets, for example, microelectromechanical frameworks, field impact transistors, electrochemical cells, gas sensors, attractive capacity media, sun powered cells, field producers, and nanodevices for catalysis. It has likewise been as of late underscored that separated from the size, the state of the nanostructure is similarly imperative for controlling distinctive properties, for example, optical ingestion in CuO nanostructures and the synergist exercises. CuO nanoparticles are doped in the different polymer or polymer mix and their belongings are being examined broadly for some, functional applications like a proficient reactant operator, gas detecting material, solar cells, the optical switch and attractive stockpiling media, and so on [16,17].

The CMC/PVP blend is used as basic material to prepare different nanocomposites by adding CuO to improve the properties over the blend [18–20]. Then, the aim of this article is to prepare and study the spectroscopic properties, dielectric permittivity and dielectric modulus of the CMC/PVP polymer blend filled with different concentrations (0.0, 0.1, 0.2, 0.4 and 0.6wt.%) of CuO nanoparticles.

2Experimental work2.1Materials and preparation

The polymers employed in the present study are carboxymethyl cellulose polyvinyl pyrrolidone (PVP) were purchased from Sigma-Aldrich. The CMC/PVP films were prepared using casting techniques like the following: The CMC solution was added to that of PVP drop by drop with constant stirring. The mixture solution of the blend was stirred about 60min at 25°C. The copper oxide (CuO) nanoparticle has a size less than 100nm was used as a nanofiller. Double deionized water is used as a solvent during the preparation. The amounts (0.1, 0.2, 0.4 and 0.6wt.%) of CuO nanoparticles solution were added to the CMC/PVP solution with stirring. The nanocomposites (CMC/PVP–CuO) solution was cast in a Petri dishes and kept drying at 35°C around 2 days to obtain the nanocomposite films. The thickness of the samples is 20μm for FT-IR and UV–visible measurements and about 120–150μm for the other measurements.

2.2Used techniques

The X-ray spectra were recorded using a PANalytical X’Pert PROXRD analyzer with Cu Kα radiation and wavelength λ=0.154056nm at 25kV. The FT-IR spectra were obtained by Nicolet iS10, USA spectrometer in the wavenumber from 4000 to 400cm−1. The AC measurements were carried out by LCR (Hioki 3531Z Hitester) at the frequency (f) in the range 100–5MHz and temperature range 25–125°C. The AC conductivity (σ) was estimated from the relation:

where d (cm), R and A are thickness, resistance and cross-section area of the sample respectively. The σAC is the AC electrical conductivity, ω is the angular frequency (ω=2πf) and σDC is the DC conductivity. The dielectric constant ε′ was as [12]:
where C is the capacitance, ε0=8.85×10−12 F m−1 and ε″ is the dielectric loss. The reaction mechanism for CMC/PVP/CuO samples is shown in Scheme 1.

Scheme 1.

The reaction mechanism for CMC/PVP/CuO composites.

(0.08MB).
3Results and discussion3.1The X-ray study

Generally, the X-ray diffraction is used to investigate the degree of amorphosity of polymer, and high conductivity is obtained in amorphous regions inside the polymers.

To study the effect of CuO content onto the semicrystalline nature of CMC/PVP polymeric chains, the X-ray spectra of pure CuO nanoparticles, CMC/PVP blend, and CMC/PVP–CuO nanocomposites are recorded as shown in Fig. 1. The X-ray spectra show one broad peak cantered at Bragg angle of 2θ=20.01°. In the pure CMC/PVP blend, there is no significant peak except for two small peaks at 2θ=18.18° and 20.25° that related to the crystalline cellulosic structure [21].

Fig. 1.

The X-ray diffraction of pure CuO nanoparticles, pure carboxymethyl cellulose/poly vinyl pyrrolidone (CMC/PVP) and CMC/PVP filled with 0.1, 02, 0.4 and 0.6wt.% of CuO.

(0.26MB).

After the addition of CuO to the polymer blend, it again showed that it causes a decrease of the main broad peak which means that the increase in the amorphous nature for CMC/PVP blend. This is revealed to the amorphous behaviour of the CMC/PVP blend. The X-ray spectra CMC/PVP–CuO display the semicrystalline behaviour with the main characteristic peaks for all component in the nanocomposites. This confirms the reaction between CMC/PVP blend and CuO nanoparticles tack places. The increase of CuO into the CuO/PVP causes the changes in the intensity and broadness of the unique peak. The increase in the intensity with the reduction of the reveal to a reduction of the degree of crystallinity in CMC/PVP polymeric chains. The degree of the crystallinity the nanocomposite samples surmises the efficient arrangement of polymeric chains or by the development of single or various helices due to the long-range order of polymeric chain possesses the degree of crystallinity. New peaks are observed at 2θ=32.25° and 35.81° attributed to CuO nanoparticles indicating a hexagonal structure of CuO [22,23].

3.2FT-IR analysis

The FT-IR spectra of pure CMC/PVP and the CMC/PVP incorporated by different contents of CuO nanofiller in the wavelength range of 400–4000cm−1 are shown in Fig. 2.

Fig. 2.

The FT-IR absorbance spectra of pure CuO nanoparticles, pure carboxymethyl cellulose/poly vinyl pyrrolidone (CMC/PVP) and CMC/PVP filled with 0.1, 02, 0.4 and 0.6wt.% of CuO.

(0.15MB).

The IR spectrum of CMC/PVP exhibits the principle bands and the function groups related to CMC and PVP polymers. The assignment of both CMC and PVP is discussed as: the FT-IR spectrum of CMC contains a hydroxyl group (OH stretching) at 3400cm−1, a hydrocarbon group (CH stretching of the CH2 groups) at 2881cm−1, a carbonyl group (CO stretching) at 1593cm−1, a CH2 scissoring around 1412cm−1 and ether groups (O stretching) at 1026cm−1[24]. And the principle bands for PVP is assigned as: two bands are observed at 1454cm−1 and 1288cm−1 due to CH2 wagging and asymmetric twisting modes. Two bands are observed at 1087cm−1 and 834cm−1 attributed to CO and CC stretching modes [25,26]. The small band is clearly observed at 1494cm−1 attributed to the CN (pyridine ring) inside PVP structure.

The absorption band around 623cm−1, may be assigned to Cu (I)–O mode [27]. For doped samples (CMC/PVP–CuO), the intensity of the IR-band at 2881cm−1, assigned to CH stretching hydrocarbon group has significantly increased confirms that the CuO reacts by these functional groups with the CMC/PVP blend. However, the absorption broad band appeared at about 609cm−1 is reflected in the presence of Cu(I)–O vibrational group confirm the presence of any other cupric oxide impurity [28].

3.3Electrical modulus behaviour

The complex permittivity (ε*) related to the electrical modulus (M′ and M″) is given as [28–30]:

The variation of the real part of the electrical modulus (M′) with Log (f) of this system is shown in Fig. 3. As we see from the figure, the values of (M′) can be divided into three regions: The first region at low frequency, the values of (M′) is very low (≈zero) confirming that the polarization of the electrode to M′ make a negligible contribution to the nanocomposite materials where the polarization of the electrode occurs at the interface of the blend matrices and CuO. The second region at intermediate frequencies, there is an exponential increase of (M′) is clear but at higher frequencies, the behaviour of (M′) tend to nearly straight of constant. These data can be discussed according to the conduction phenomenon related to the short-range mobility of charge carriers (especially ions).

Fig. 3.

The M′ depends on Log (ω) of pure CuO nanoparticles, pure carboxymethyl cellulose/poly vinyl pyrrolidone (CMC/PVP) and CMC/PVP filled with 0.1, 02, 0.4 and 0.6wt.% of CuO.

(0.13MB).

Fig. 4 shows the values of the imaginary part (M″) of the electrical modulus various of Log (f). The lower values of the imaginary part (M″) at the lower frequency are the indication of transport of the ions. Well resolved one relaxation peaks are founded for these curves attributed to the imperfections within the crystalline phase. It is seen that, the peak intensity of M″ is increasing as an increase of CuO attributed to that CuO contributes to the relaxation process. The presence of one peak in M″ confirms that nanocomposite films are ionic conductors. The shift of the peaks towards the lower frequency as the increase in CuO is observed. The broad shape of the peak confirms the spread of relaxation and hence a non-Debye type of relaxation is founded.

Fig. 4.

The M″ depends on Log (ω) of pure CuO nanoparticles, pure carboxymethyl cellulose/poly vinyl pyrrolidone (CMC/PVP) and CMC/PVP filled with 0.1, 02, 0.4 and 0.6wt.% of CuO.

(0.14MB).

The relation between the real part (M′) and the imaginary part (M″) for the samples is shown in Fig. 5. The curves display the formation of semicircle shape conforming the presence of broad relaxation processes. The presence of one semicircle is the significance of single relaxation inside the obtained samples and the littles of radius semicircle are related to the highest capacitance in the CMC/PVP–CuO nanocomposites.

Fig. 5.

The complex variation plots (M′ and M″) of pure CuO nanoparticles, pure carboxymethyl cellulose/poly vinyl pyrrolidone (CMC/PVP) and CMC/PVP filled with 0.1, 02, 0.4 and 0.6wt.% of CuO.

(0.13MB).
3.4The dielectric properties

The complex permittivity (ε*) related to free dipole oscillating can be studied according to Debye relation as ε*=ε′−iε″[31].

Fig. 6 shows the plot between the dielectric constant (real part ɛ′) and Log (f) of CMC/PVP blend and the blend doped with 0.1, 0.2, 0.4 and 0.6wt.% of CuO nanoparticles over the frequency range from 100 to 106Hz. The real part ɛ′ is a measure of the electrical energy storing ability from an external electric field is the sample where ɛ′ is a function of capacitance as: ε′=C(d/(ε0A)), where C is the equivalent capacitor, A is the area of the electrode, t is the thickness of the sample and ɛ0 is the permittivity of space. It is also observed that in the lower frequency range, dielectric constant showed non-Debye behaviour, i.e., these decrease with the increase in frequency.

Fig. 6.

The dielectric constant (ε′) depends on Log (ω) of pure CuO nanoparticles, pure carboxymethyl cellulose/poly vinyl pyrrolidone (CMC/PVP) and CMC/PVP filled with 0.1, 02, 0.4 and 0.6wt.% of CuO.

(0.09MB).

The plot ε′ is systematically decreases with the increase of the frequency ascribed to polarization effects and it reaches to constant values at a higher frequency due to the contribution of charge accumulation at the prepared films.

Fig. 7 shows the relation between the imaginary part (ɛ”) and the frequency of the prepared samples. The behaviour of ɛ” is also systematically reduced as the increase of frequency due to the polarization which created with ionic exchange of some ions by locally displacing in the direction of the applied field due to the space charges cannot support and comply with the outside field which causes a decrease in the polarization. For CMC/PVP–CuO samples, as an increase of the frequency, the dipole will no longer to rotate and the oscillation being the lag those of the applied field.

Fig. 7.

The dielectric loss (ε″) depends on Log (ω) of pure CuO nanoparticles, pure carboxymethyl cellulose/poly vinyl pyrrolidone (CMC/PVP) and CMC/PVP filled with 0.1, 02, 0.4 and 0.6wt.% of CuO.

(0.1MB).
3.5Impedance analysis

The complex impedance (Z*) as a function of the impedance modulus (Z′ and Z″) is given as [32]:

where Z′ is the real part and Z″ is the imaginary part of the impedance modulus.

The plot between Z′ and Log (f) is observed in Fig. 8. The behaviour of Z′ and Z″ is dramatically reduced as an increase of the frequency as well as CuO contents. This is the trend of the most polymeric materials. Also, the values of Z′ is reduced as an increase of CuO content in the low frequency ranges and thereafter founded to merge in the high frequency values attributed to the release of space charge polarization as a rise in frequencies. The space charge polarization occurs maximum at a higher frequency for higher concentration attributed to the reduction in barrier characterization of the materials which responsible for the enhancement of the electrical conductivity of these samples. The complex impedance is high at low frequency attributed to the space charge polarization.

Fig. 8.

The Z′ depends on Log (ω) of pure CuO nanoparticles, pure carboxymethyl cellulose/poly vinyl pyrrolidone (CMC/PVP) and CMC/PVP filled with 0.1, 02, 0.4 and 0.6wt.% of CuO.

(0.11MB).

Fig. 9 displays the relation between Z″ depends on Logf (usually called a loss spectrum) of the nanocomposites. The values of Z″ are reduced as an increase of frequency and increase of CuO content. New peaks in this plot confirm the existence of the relaxation process. With increase of CuO contents, the values of Z″ is reduced with the low shift of the peaks towards the higher frequency. Then, all spectra merge in high-frequency region.

Fig. 9.

The Z″ depends on Log (ω) of pure CuO nanoparticles, pure carboxymethyl cellulose/poly vinyl pyrrolidone (CMC/PVP) and CMC/PVP filled with 0.1, 02, 0.4 and 0.6wt.% of CuO.

(0.1MB).

Fig. 10 shows the relation between tanδ and Logf. The calculated magnitude in the loss tangent tan(δ) is estimated from the dielectric permittivity equation as [33]:

Fig. 10.

The tangent loss (tan δ) depends on Log (ω) of pure CuO nanoparticles, pure carboxymethyl cellulose/poly vinyl pyrrolidone (CMC/PVP) and CMC/PVP filled with 0.1, 02, 0.4 and 0.6wt.% of CuO.

(0.12MB).

From the figure, it is found that the magnitude of tanδ is reduced as an increase of the frequency attributed to the hopping frequency of charge carriers do not follow any changes of the applied field. The increase of tanδ values as an increase of CuO concentration is expected because of the increase of the conductivity in these films due to addition of CuO.

4Conclusion

A system of CMC/PVP–CuO nanocomposite films was synthesized by the casting solution techniques. The nanocomposite samples were investigated using X-ray diffraction and FT-IR spectroscopy. The electrical conductivity was studied using dielectric permittivity and impedance modulus. The X-ray spectra of CMC/PVP–CuO display a unique characteristic of the samples implying co-existence in mixed crystalline and semicrystalline nature. The intensity of the IR-band at 2881cm−1 is reduced which confirms that the CuO interacts with this functional group. However, the absorption broad-band appeared at about 609cm−1 was attributed to the presence of Cu(I)–O group confirm the presence in any other cupric oxide impurity. The behaviour of the real part (M′) was divided into three regions due to the conduction phenomenon related to the short-range mobility of charge carriers (ions). The lower values of the imaginary part (M″) at the lower frequency are the indication of transport of the ions. Well resolved one relaxation peaks are founded for these curves attributed to the imperfections within the crystalline phase. The broadening of the peak indicates the spread of relaxation and hence a non-Debye type of relaxation in the materials is observed. The plot between real part (M′) and imaginary part (M″) displays the formation of semicircle arc indicating the presence of broad relaxation processes. The behaviour of both ε′ and ɛ” was systematically reduced with an increase of the frequency ascribed to polarization effects and it reaches to constant values at a higher frequency due to the contribution of charge accumulation. The increase of tanδ values as an increase of CuO concentration is expected because the increase of the conductivity in these films due to the addition of CuO.

Conflicts of interest

The authors declare no conflicts of interest..

.

[29].

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