Materials Today: Proceedings 66 (2022) 3481–3486

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Materials Today: Proceedings

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Study of refractive index and dispersion behaviour of KMnO4 doped

poly-methyl-methacrylate(PMMA)composites
Minal Bafna a,⇑, Neha Sain a, Akanshu Khandelwal a, Farah Deeba b, Ankit Kumar Gupta a
a
Dept. of Physics, Agrawal P.G. College, Jaipur, India
b
SS Jain Subodh PG (Autonomous) College, Jaipur, India

a r t i c l e i n f o a b s t r a c t

Article history: This work presents the analysis of optical characteristics of KMnO4 doped PMMA films synthesized using
Available online 14 July 2022 solution cast technique. The optical absorption spectra of these films in the wavelength range from 300 to
1100 nm were recorded by the help of a UV–VIS spectrophotometer. It has been found that the band gap,
Keywords: effective single oscillator energy (Eo), dispersion energy (Ed), dielectric constant and refractive index for
Polymer Composites zero frequency (eo, go) and dielectric constant and refractive index for very high frequency (e1, g1) opti-
Optical band gap cal mobility (lopt), angular plasma frequency (xP) optical resistivity (qopt) and relaxation time (s) are pre-
Refractive index
dominantly dependent on type of filler and its weight percentage in the polymeric matrix. The structural
Dispersion energy
Oscillator energy
analysis of the prepared sample films has been confirmed by XRD and FTIR analysis.
Optical mobility Ó 2022 Elsevier Ltd. All rights reserved.
Optical resistivity Selection and peer-review under responsibility of the scientific committee of the 3rd International Con-
ference on ‘‘Advancement in Nanoelectronics and Communication Technologies”.

1 Introduction 10,12 ]. Our studies revealed that insertion of metal salts into it
brought in such variations in its physical properties that rendered
Polymeric composite materials are widely used because of their it novel applications. We found that potassium oxide inserted
flexibility, durability and light weight. Polymers are used in auto- PMMA composites exhibited excellent e.m. shielding capabilities
mobile, military, space and many other industries [1,2]. They are [6,9–10], tin chloride doped PMMA composites provided good
increasingly being used in developing passive coatings, electronic transparent flexible conducting films [13–15], carbon-soot doped
devices, electronic and chemical sensors, high performance batter- PMMA composites as good gas sensor devices [16]. In continuation,
ies, data storage and communication [3–5]. Properties of these we then reported FeCl3 doped PMMA composite films to have
composites can be changed according to our needs by the doping excellent electrical and optical properties [17–18]. In all these
of right amount of suitable material. They can be manufactured studies we have also evaluated the physical parameters of interest
at low price with ease and provide high performance and stability. as per theoretical formalism and their variation with frequency or
Polymer nano composites made by organic materials generally wavelength has been investigated which paved our way in devel-
exhibit very high refractive index which makes them a very strong oping a deep understanding of correlation in structure and physical
contender for making LED, electromagnetic shielding, anti refrac- properties of these PMMA metal composites. Literature Survey also
tive coating, show screen, UV screen solar cells and lithography strengthens our understanding of the fact that the optical proper-
[1–12]. ties of PMMA can be further improved by introducing inorganic fil-
PMMA is a polymer with very high transparency, optical clarity, lers like metal, metal oxides, metal chlorides, metal nitrates etc.
dimensional stability, stiffness, heat insulation, recyclable, eco- [19–22]. PMMA has very high transmittance because the electrons
nomical and easy to process and because of its excellent optical are absent from conduction band and all the electrons are strongly
properties PMMA is being widely used in aircraft windows, light bond by covalent bonds to their atoms. Higher transmittance
and durable contact lens, luminous ceilings, LED and lights, dis- causes lower absorbance but if the right amount and type of inor-
plays of electronic devices, solar panels and many more[2–3,6– ganic filler is introduced then its absorbance and transmittance can
be changed in a controlled manner [23–26]. When inorganic filler
⇑ Corresponding author. is introduced inside a polymeric matrix its transmittance decreases
E-mail address: drminalphysics@rediffmail.com (M. Bafna). and its absorbance increases which leads to the increment in

https://doi.org/10.1016/j.matpr.2022.06.370
2214-7853/Ó 2022 Elsevier Ltd. All rights reserved.
Selection and peer-review under responsibility of the scientific committee of the 3rd International Conference on ‘‘Advancement in Nanoelectronics and Communication
Technologies.
M. Bafna, N. Sain, A. Khandelwal et al. Materials Today: Proceedings 66 (2022) 3481–3486

refractive index [27–28]. Therefore these materials have high Fourier transform infrared (FTIR) spectra of our prepared pure
potential in the field of optoelectronic devices. [6,10,19–29]. and KMnO4 doped PMMA polymer films have been achieved using
In the present work, we have evaluated localized charge density a Perkin Elmer FTIR spectrometer (Frontier spectrometer) in the
value (N/m*), high frequency dielectric constant (e/), relaxation wavelength range of 4000–400 cm1. The XRD patterns of the pre-
time (s), plasma frequency (x), electrical resistivity (q), optical pared films were obtained using X’PERT-PRO X-ray diffractometer
mobility (l), oscillator strength (s0) oscillator energy (E0) and dis- with CuKa radiation source in the 2h range (10°–70°). The absor-
persion energy(Ed) for KMnO4 doped PMMA composites. These bance and transmittance spectra of our prepared sample films
composites have been synthesized by doping 2% and 5% KMnO4 were measured with the help of the EI 2357 UV – VIS double beam
in PMMA solution and casting them into films. The optical charac- spectrophotometer in the wavelength range (300 nm – 1100 nm)
terization done using EL 2375 UV–Vis-NIR double beam spec- at room temperature. This data and the variation of optical prop-
trophotometer provided the transmittance and reflectance data erties viz absorption coefficient (a), extinction coefficient (k),
of these composite films in the wavelength range 400–800 nm. finesse coefficient (F), refractive index (g), real and imaginary
From the transmittance data, the absorption edges provided the parts of dielectric constant (er and ei) and optical conductivity
measure of band gap energy and the variation of refractive indices; (r) has been reported earlier [6]. Based on this earlier study we
extinction coefficient, dielectric constant and optical conductivity have evaluated and analyzed the following optical parameters
which have been reported in our earlier work. Refer reference localized charge density value (N/m*), high frequency dielectric
[9]. This data has been further used to evaluate and analyze the constant (e/), relaxation time (s), plasma frequency (x), electrical
above mentioned characteristic optical parameters reported in resistivity (q), optical mobility (l), oscillator energy (E0) and dis-
the present work. To verify the structural changes that occur on persion energy (Ed) using the theoretical formalism discussed
doping the host polymer with KMnO4; we have done the FTIR below.
and XRD analysis of our prepared samples.
2.3 Theoretical considerations for evaluation of optical parameters

2 Experimental details
Optical constants are the parameters which control the optical
behavior of the material and hence the study of their manipulation
2.1 Materials and fabrication of KMnO4 doped PMMA composites
occurred due to addition of filler is significant in controlling the
behaviour of the material which further improves the utility of
To synthesis the pure and KMnO4doped polymeric films of
these materials. The Kramer’s- Kronig relation expresses refractive
PMMA, solution cast technique was used. The detailed method is
index g of a material as a function of reflectance R and extinction
as explained in our earlier work in reference [6,9]. PMMA granules
coefficient k as shown in equation (1).
of average molecular weight (Mw) of 100.12 g/mole per repeat unit sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
and density 1.18gm/cm3 from M/s Gadra Chemicals, Bharuch is 1þR 4R
ultrasonically dispersed in dichloromethane of 99.8% purity, pro- g ¼ þ k
2
ð1Þ
1R ð1  RÞ2
cured from Merck India Pvt ltd, for 2 h to obtain a stable suspen-
sion. To this prepared solution, taken in five different beakers, The dispersion property of a thin film and its refractive index
varying concentration of KMnO4 (0, 2 and 5% by weight) were can be very useful to design very effective optical devices. The
mixed and made to disperse on a magnetic stirrer for 6 h at effective single oscillator energy (Eo) which is proportional to the
70 °C. Thin polymer films were cast from these solutions by pour- oscillator energy and dispersion energy (Ed) which is a parameter
ing them into petri dish of diameter 76 mm kept floated over mer- depending upon charge allocation of each unit cell and coordina-
cury in dust free environment. These were then allowed to dry tion number and related to chemical bonding [4,30], can be calcu-
initially by evaporation and later in an oven for the solvent to com- lated by the help of the single oscillator model proposed by
pletely evaporate. The resulting films were of uniform thickness of Wemple and DiDomenico [30–32].
around 100 lm and had slight yellow tinge of colour depicted in
Ed Eo
Fig. 1. g2  1 ¼
Eo 2  E2
or
2.2 Structural and optical characterization
 1 Eo E2
The understand the possible interactions among the inserted g2  1 ¼  ð2Þ
Ed Ed Eo
filler material with the functional groups of host polymer, the

Fig. 1. Prepared sample films: Pristine PMMA, 2% and 5% by weight KMnO4 doped PMMA films.

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M. Bafna, N. Sain, A. Khandelwal et al. Materials Today: Proceedings 66 (2022) 3481–3486

Considering equation (2) to represent a straight line, for the Where s represents relaxation time and J current density is
curve plotted between (g2 – 1)-1 and E2; the y intercept of the expressed as.
curve will provide the value of Ed/Eo and the slope denotes the
e2 N
value of the (EdEo)-1. Solving the slope and intercept equations, val- J ¼ ð6Þ
ues of the effective single oscillator energy (Eo) and dispersion 8p3 c3 eo m
energy (Ed) can be determined. Using the values of the effective It is explicit that the slope of the curve plotted between єi and k3
single oscillator energy (Eo) and dispersion energy (Ed) in the fol- provides the value of N/m*; the values of which are further used to
lowing relation. estimate the optical mobility (lopt), angular plasma frequency (xP)
Ed and the optical resistivity (qopt) using relations (7–9). [21–25].
eo ¼ g2o ¼ 1 þ ð3Þ
Eo es
lopt ¼ ð7Þ
the static dielectric constant eo or dielectric constant at zero fre-
m
quency or zero photon energy is obtained. Here go is analogous to
e2 N
eo and is referred as static refractive index or refractive index at xP ¼ ð8Þ
zero frequency / zero photon energy.
eo m
Basic optical transition in PMMA polymer composites is mainly
1
idiosyncrasy to the variation of optical dielectric constant, which qopt ¼ ð9Þ
explains the possibility of losing energy by an electron as it travel elopt N
through the surface of composite film. It express in real and imag-
inary dielectric constant. The dielectric constant for a diamagnetic
3 Results and discussions
substance is expressed as the square of the refractive index and is a
complex quantity.
  Here we report the outcome obtained on analyzing the data
2 ¼ g2 ¼ ðg þ ikÞ ¼ g2  k þ 2ik
2 2 obtained from structural and optical characterization.

where its real part er = g2 – k2 governed by the refractive index 3.1 FTIR analysis
of the material, exhibits quantitatively the ability of material to
slow down the speed of the EM wave and imaginary part ei = 2ik FTIR have been performed to confirm the presence of KMnO4 in
dominated by extinction coefficient, provides a measure of the PMMA polymer. Fig. 2 represents the FTIR spectra of pure and
capacity of absorbing energy due to polarization. Using the stan- doped PMMA films where the characteristics peaks represent the
dard values for charge of electron e as 1.602  1019 C, velocity various vibrational modes of the PMMA molecule.
of light c = 2.99  108 m/s, mass of electron me = 9.1  10-31kg, The main bands of pure PMMA sample were observed at
dielectric constant for free space e0 = 8.85*1012f in the well 2951 cm1, 1725 cm1, 1435 cm1, 1384 cm1, 1236 cm1,
known Spitzer-Fan relation [18,25]. 1192 cm1,1141 cm1, 984 cm1, 845 cm1,748 cm1 and
  1
485 cm .These peaks correspond to the C-H stretching of methyl
e2 N
er ¼ g2  k2 ¼ e1    k2 ð4Þ group, C = O stretching mode CH3 asymmetric stretching, CH3 sym-
4pc2 eo m
metric stretching, torsion of methylene (CH2) group, CH2 wagging
the values for high frequency dielectric response e1 and charge mode, C-O (ester group) symmetric stretching in C-O-C linkage
carrier concentration N can be measured. If we plot a curve (bending mode), CH2 rocking mode, C– C stretching bands respec-
between er and k2 then the value of the y intercept of the curve will tively.[14,15,19–25].
show the value of dielectric constant for high frequency e1 and The strong characteristic peak at 3300–3500 cm1 has become
slope of the curve will tell the value of the ratio of the charge car- broader for the doped samples, indicating the interaction of KMnO4
rier density N and effective mass m*. Here the square of e1 helps with PMMA matrix. The slight shift and change in intensity of the
evaluation of long wavelength refractive index g1. peaks are clear indications of formation of charge transfer complex
The complex dielectric function is also significant in providing between KMnO4 salt and the PMMA molecules; effects similar to
the density of localized electronic states within the forbidden gap those reported in literature[19–25].
of the composites made. The imaginary part of the optical dielectric
constant is also related to wavelength k as shown in equation (5). 3.2 XRD analysis:
3
Jk
ei ¼ ð5Þ The X-ray diffraction pattern of pure and KMnO4 doped PMMA
s are presented in Fig. 3. The X-ray pattern of pure PMMA shows a

Fig. 2. Vibration modes of pure PMMA (blue) and PMMA doped with KMnO4 with 2% (red curve) and 5% (black curve).
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M. Bafna, N. Sain, A. Khandelwal et al. Materials Today: Proceedings 66 (2022) 3481–3486

Table 1
Optical parameters obtained for Pure and doped PMMA with KMnO4 for 0.5 and 5%.

Optical parameter Pure PMMA PMMA/KMnO4 PMMA/

(0.5%) KMnO4 (5%)
Effective single oscillator 3.873 3.25 3.102
energy Eo (eV)
Dispersion energy Ed (eV) 5.164 5.913 6.715
Static dielectric constant 2.33 2.891 3.165
(eo)
Static refractive index 1.527 1.679 1.779
(go)
High frequency dielectric 2.866 3.956 4.719
constant (e1)
High frequency refractive 1.693 1.989 2.172
index (g1)
N/m* (m3) 56
1.16  10 56
4.29  10 5.064  1056
Fig. 3. XRD patterns of pure PMMA (black) and PMMA doped with KMnO4 with 2% Relaxation time s (sec) 1.6848  1012 6.1775  1012 7.3  1012
(blue curve) and 5% (red curve). Plasma frequency xp 1.275  1018 3.799  1018 4.099  1018
Optical resistivity qopt 2.004  106 1.474  107 1.057  107
Optical mobility lopt 0.296 1.086 1.283
strong broad hump characteristic of its amorphous nature at
2h = 10.4⁰ only. A clear shift in the position and intensity of this
hump can be noticed for XRD pattern of KMnO4 doped PMMA. the formation of defects in host polymer on insertion of filler. It
For 2% doping the peak shifts to 2h = 13.5⁰ and for 5% it shifts to is evident from Table 1 that the dispersion energy increases indi-
2h = 14.5⁰ and shows two new peaks around and 27.2⁰ and 29.9⁰ cating the increase in disorder content and irregularities between
in respective curves. The significant increase in the relative inten- HOMO and LUMO in polymers or the increase in amorphous por-
sity of the characteristic peak of PMMA in the doped samples tion. We see that the addition of fillers has introduced several
clearly indicates that the crystalline fraction has increased as a trapped energy states, which reduce the value of optical band
result of KMnO4 addition [19–25 ]. gap energy, similar to the results obtained in our earlier work
too. The more the concentration of filler, more are the energy tails
3.3 Optical characterization leading to decrease of the optical band gap energy. The addition of
KMnO4 filler has actually lead to formation of ionic complexes, dis-
In this work we report the dispersion behaviour of PMMA films order, and imperfections in the structure of the host polymer, lead-
on insertion of KMnO4 filler into it. The absorbance edges have ing to create new localized states of various depths in the
been measured from the absorbance spectra obtained using EI forbidden band gap energy. Further Eo and Eg are related to each
2357 UV–VIS double beam spectrophotometer in the wavelength other and there ratio remains constant. The static dielectric con-
range (300 nm – 1100 nm) at room temperature and reported in stant eo and static refractive index go both also depict an increase
our earlier work in reference [6]. in value on increase in filler concentration. Similarly high fre-
From those estimated values of refractive index g and band gap quency dielectric constant and refractive index (e1, g1) also
energy (E = Eg) in reference [9], we have calculated the effective increases with doping concentration, this effect can be explained
single oscillator energy (Eo) and dispersion energy (Ed) using equa- by the densification of the material [7,30,32] which shows that
tion (2) and have shown in Fig. 4. The value of effective single oscil- using KMnO4 refractive index and dielectric constants of PMMA
lator energy (Eo) decreases with the increase of the doping can be changed according to the doping concentration which can
concentration of KMnO4 because it is related to the energy band further increase the uses of PMMA in the field of optoelectronic
gap (Eg) and doping increases localized states in energy band gap devices.
which further increases low energy transitions, whereas increase The values of e1, and N/m ⁄ have been estimated from intercept
in doping concentration increases the dispersion energy (Ed) which at er axis, and the slope of the linear fitting using equation (4) as
shows the change in the structural order of the material. shown in Fig. 5and values mentioned in Table 1. It is evident that
The dispersion energy is interpreted as width of the tails of values of e1 and N/m ⁄ for our prepared samples increase with
localized states in the forbidden band gap and helps in realizing increasing salt content. This reveals that with increasing concen-

Fig. 4. Variation of (g2-1)-1 with the square of photon energy E2 for composite films of pure PMMA (light blue) and PMMA doped with KMnO4 with 2% (red coloured curve)
and 5% (dark blue colour curve).

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M. Bafna, N. Sain, A. Khandelwal et al. Materials Today: Proceedings 66 (2022) 3481–3486

Fig. 5. Variation of real part of dielectric constant er with square of wavelength k2 for PMMA films pure (light blue) and PMMA doped with KMnO4 with 0.5% (red coloured
curve) and 5% (dark blue colour curve).

Fig. 6. Variation of imaginary part of dielectric constant ei with k3 for pure PMMA films (light blue) and PMMA doped with KMnO4 with 0.5% (red coloured curve) and 5%
(dark blue colour curve).

tration of KMnO4 free ionic carriers increase. Charge career density and FTIR studies strengthen our outcomes.The large absorption
N/m* increases with the doping concentration and due to increase coefficient and the compositional dependence of the optical
in free charge career density, number of charge increases and they parameters make this system suitable for opto-electronic devices
take part in the polarization process and therefore the value of (e1) application.
increases too [3,17,32] and which further increases the value of
relaxation time s and plasma frequency xp calculated using equa- Declaration of Competing Interest
tions (5)–(8) and data from Figs. 5 and 6 [Refer Table 1]. Increase in
relaxation time further increases optical mobility lopt which The authors declare that they have no known competing finan-
directly decreases optical resistivity qopt [refer Table 1]. The reason cial interests or personal relationships that could have appeared
for this change in the values of s, xp, lopt and qopt is given by a to influence the work reported in this paper.
local electric field which is induced inside the composite due to
the inorganic filler’s dipole moment which increases the polariza-
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