Vol.:(0123456789)1 3Journal of Inorganic and Organometallic Polymers and Materials [602794]

Vol.:(0123456789)1 3Journal of Inorganic and Organometallic Polymers and Materials
https://doi.org/10.1007/s10904-018-0916-6
Improving the Optical, Mechanical and Dielectric Properties of PMMA:
Mg1−xCuxO Based Polymer Nanocomposites
H. Abomostafa1 · S. A. Gad2 · A. I. Khalaf3
Received: 12 June 2018 / Accepted: 9 July 2018
© Springer Science+Business Media, LLC, part of Springer Nature 2018
Abstract
The aim of the presented work is to study the optical, mechanical and dielectric properties of Poly methyl methacrylate (PMMA) filled with Mg
1−xCuxO, 0.05 ≤ x ≤ 0.2 synthesized in the form of casted films. Structures of the prepared powder and
films were examined by X-ray diffraction (XRD), where the recorded pattern reveals the existence of cubic phase structure for Mg
1−xCuxO powder and films. Fourier transform infrared (FTIR) spectra confirmed that Mg0.9Cu0.1O nanoparticles were
successfully incorporated into the PMMA. The morphology of the nanocomposite films was studied using field emission scanning electron microscopy (FESEM). Well dispersion of Mg
1−xCuxO nanoparticles in the PMMA matrix and formation
of some cluster were observed. The optical properties of the prepared nanocomposite films were performed by means of UV–Vis technique. The absorption coefficient, optical energy band gap, extinction coefficient and the refractive index of the casted films were calculated. The results showed a decrease in optical energy band gap, and an increase of absorption coefficient, extinction coefficient and refractive index with increasing the percentage ratio of Cu in PMMA matrix. There is an enhancement in mechanical properties. The microhardness increases as the Cu content increases up to x = 0.15 wt% after
that it decreases. The tensile strength was measured and raised from 23.87 to 43.30 MPa with increasing the Cu content up to x = 0.10 after that it decreases. Finally, the permittivity (ε′ ) and dielectric loss (ε″ ) were decreased as the frequency increased
but (ε′) became nearly constant at higher frequency range. Moreover, ε′ and tan δ increased as the Cu content increases. Also
the AC conductivity was measured to study the conduction mechanism in the presented nanocomposite films. The calculated dc conductivity was increased as the Cu content in PMMA matrix increased.
Keywords Polycrystalline Mg
1−xCuxO · Poly methyl methacrylate (PMMA) · Optical properties · Mechanical Properties ·
Dielectric properties
1 Introduction
Nanocomposite materials play an important role in creating
extensive usages in many areas [ 1–5]. In Last years, syn –
thesis of polymer nanocomposites attracted great attention in various high technology aspects, for example, sensors, catalysis, super capacitors, rechargeable batteries, and anti-static textiles [6 –9]. Poly (methyl methacrylate) (PMMA)
is an imperative thermoplastic material, of excellent opti –
cal properties, some great mechanical properties, thermal stability, electrical properties, and easy shaping [10– 13].
PMMA has been utilized as a part of skeletal surgery and more recently is utilized as a delivery agent for local high-dose antibiotics to treat soft tissue and osseous infections [14]. It has been amazingly used for antibiotic delivery sys-
tem purposes for the treatment of osteomyelitis [15]. Like-wise, PMMA is a broadly utilized support medium for the implanting of in place, decalcified bone [16]. Its hardness makes it perfect for calcified tissue segmenting and ensu-ing histological examination [17]. The dispersion of met-als nanoparticles in polymer matrix could commonly add unique physical properties to the associated matrixes such as responsiveness to mechanical, etc to produce very useful
* H. Abomostafa
halaabomostafa@yahoo.com
1 Faculty of Science, Physics Department, Menoufia
University, Shebin El Koom, Egypt
2 Solid State Physics Department, Physics Research Division National Research Centre, El-Bohoos str., Dokki, Giza 12622, Egypt
3 Polymers and Pigments Department, National Research Centre (NRC), 33 El Bohouth St. (former El Tahrirst.), Dokki, Giza, Egypt

Journal of Inorganic and Organometallic Polymers and Materials
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nanocomposites [ 18–21]. In the recently years, synthesis
of the nanoparticles of transition conducting metal oxides
(TCMOs) attracted a great attention due to their techno-logical applications [22– 25]. It is used in the fabrication of
microelectronic circuits, sensors, fuel cells and as catalysts [26–28]. The TCMO nanoparticles have superior physical
and chemical properties as a result of their limited sizes and high density of corner or edge surface sites [29]. Recently, the II–VI semiconductor nanocrystals are elaborated as a class of nanomaterials whose unique physico-chemical prop-erties helping to create a new generation of nano-photonics, nano-optoelectronics and nano-electronics [30– 32]. Synthe-
sis and characterization of CuO–MgO nanocrystal was stud-ied by different techniques [33– 35]. The properties of the
synthesized TCMOs could be promising materials for mod-ern materials design. Different methods have been used to synthesize various metal-polymer composites e.g. (i) Direct mixing of nanoparticles in the polymer [36] (ii) Sol–gel methods [37] (iii) in-situ techniques [38] and (iv) deposi-tion method [39]. The previous work did not investigate the optical, mechanical and dielectric properties of Mg
1−xCuxO/
PMMA nanocomposite films. In this work, Nanocompos-ites films of Mg
1−xCuxO nanoparticles dispersed in PMMA
matrix with 0.05 ≤ x ≤ 0.2 were synthesized by solution cast-
ing method.
The structure, optical, mechanical and dielectric proper –
ties were also investigated. Also, we expected new cross properties to appear in their physical properties of the nan-composites films.
2 Experimental
Polycrystalline Mg1−xCuxO (where x = 0.05, 0.1, 0.15 and
0.2) samples were prepared using solid state reaction tech-nique, using high purity (99.999%) MgO and CuO obtained from Sigma-Aldrich. The appropriate weight (4 gm) of PMMA was dissolved in 100 ml of chloroform. The mixture was magnetically stirred continuously at room temperature for 2 h, until the mixture solution has a homogenous viscous appearance. Mix 2 wt. % of prepared powder Mg
1−xCuxO
with the PMMA solution and stirred for 1 h. The final prod –
uct of the composite Mg1−xCux O/PMMA was casted in
glass Petri dishes and left 1 day for drying. The structure of casted films were characterized by XRD using analyti-cal Xʼ Pert PRO MRD diffract meter system having CuKα
(λ = 1.540598 Å) with 2θ = 5°–100°. In order to examine
the presence of Mg
1−xCuxO in the PMMA matrix, FTIR
(Vertex 70) spectroscopic study was carried out in the fre-quency range (3500–500) cm
−1. Field emissions scanning
electron microscope (FESEM) Quanta FEG 250 was used to analyze the films topography. The optical measurements of the prepared films were investigated using UV–Vis spectrophotometer type JASCO 570. The micro hardness (Hv) was measured from the residual impression of Vick –
ers square-based diamond indenter after an indentation time of 30 s. Loads of 2.942 N was used to derive a load-independent value of Hv . Five indentations were made at
different points and the H-values were determined within an error of ± 3%. Microhardness is measured according to SHI-
MADZU. Tensile properties of the vulcanizates were evalu-ated using an Instron Universal Test Machine Model 1425, according to ASTM D412. The dielectric and conductivity measurements were carried out by means of high-resolution broadband impedance analyzer (Schlumberger Solartron 1260). The frequency range of the applied ac electric field was between 0.1 Hz and 1 M Hz. The measurements were automated by interfacing the impedance analyzer with a personal computer through a GPIB cable IEE488. A com-mercial interfacing and automation software Lab view was used for acquisition of data. The error in ε′ and ε″ amounts
to 1 and 3%, respectively.
3 Results and Discussion
3.1 XRD and SEM Investigations
The XRD patterns for Mg1−xCuxO powder, 0.05 ≤ x ≤ 0.2
are shown in Fig.  1. It was found that samples with Cu con-
tent up to x = 0.15 show a single phase of MgO rock salt structure type ICDD card no. 98-006-0497, while for x = 0.2 two phases were detected; namely, MgO rock salt structure and Cu
2O cuprite cubic phase card no. 98-017-3982. X-ray
diffraction analysis was investigated for the prepared com-posite films (Mg
1−xCuxO/PMMA) as shown in Fig.  2. The
hump observed at 2θ = 17°–19° is due to the amorphous
nature of PMMA [10]. The most intense peaks found in XRD of the powder appear nearly at the same position in the Mg
1−xCuxO/PMMA diffraction pattern. From XRD pat-
tern, the crystallite size (D) of Mg1−xCuxO nanoparticles
was calculated from the FWHM of the most intense peak corresponding to (200) plane using Scherrer’s formula as listed in Table  1. From the reported data in Table  1, it was
found that, the crystallite size increases with Cu content in Mg
1−xCuxO increases up to x = 0.15, and then deceases at
x = 0.2.
Figure 3 shows FTIR spectra for PMMA, (Mg0.9Cu0.1O)
nanoparticles and (Mg0.9Cu0.1O/PMMA) nanocompos –
ite. Firstly, FTIR spectrum for (Mg0.9Cu0.1O) nanoparti-
cles curve (b), shows the absorption band at 2357 cm−1 is
ascribed to the stretching vibrations of C–O due to adsorp-tion of atmospheric carbon dioxide. Whereas the absorption band at 1533 cm
−1 is attributed to O–H bending [ 34]. Fig –
ure 3 curve (a) shows FTIR spectrum of PMMA. The broad
peak at 2950 cm−1 is due to the presence of C–H stretching

Journal of Inorganic and Organometallic Polymers and Materials
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vibration. A sharp intense peak at 1725 cm−1 appeared due
to the presence of ester carbonyl group stretching vibra-
tion. The peak at 1443 cm−1 assigned to C–H bending
vibration. The broad peak at 1148 cm−1 was attributed to
the C–O (ester bond) stretching vibration. The broad band at 984 and 750 cm
−1 assigned to the C–H bending vibra-
tion, and C–C stretching vibration respectively [18]. On the other hand, the FTIR spectrum of Mg
0.9Cu0.1O/PMMA
nanocomposite was shown in Fig.  3 curve (c). It is observed Fig. 1 X-ray diffraction patterns
of Mg1−xCuxO powder
Fig. 2 X-ray diffraction patterns of Mg1−xCuxO/PMMA nanocompos-
ite films with different Cu content
Table 1 The crystallite size of Mg1−xCuxO/PMMA nanocomposite
films
Composition Crystallite
size (nm)
Mg0.95Cu0.05O/PMMA 25.75
Mg0.9Cu0.1O/PMMA 26.50
Mg0.85Cu0.15O/PMMA 31.49
Mg0.8Cu0.2O/PMMA 14.50
Fig. 3 FTIR spectra for (a) PMMA polymer, (b) Mg0.9Cu0.1O nano-
filler and (c) Mg0.9Cu0.1O/PMMA nanocomposite film

Journal of Inorganic and Organometallic Polymers and Materials
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the same characteristic peaks of PMMA beside the char –
acteristic peaks of Mg0.9Cu0.1O. This study confirmed that
Mg0.9Cu0.1O nanoparticles were successfully incorporated
into the PMMA.
A detailed view to the morphology of the casted films
surface can be obtained by FESEM is indicated in Fig.  4a–e.
The SEM micrographs, reveals that the films with less Cu
content characterized by groups of the finer rounded grains. Also, some of these grains are compacted side by side to be conductive paths in PMMA matrix as observed from Fig.  3a. Increasing Cu content, the coalescence of particle
increased to be elliptical shape and consequently existing more conductive paths. Large network-like conductive paths created in the polymer matrix. The network-like conduct-ing paths can be clearly observed from light lines from the modified SEM photograph with artistic effect as shown from Fig. 4e.
3.2 Optical Properties
The optical properties were investigated by measuring the transmission spectra in the wavelength range 200–1600 nm. Figure  5 shows the transmission decreases as x content of
Mg
1−xCuxO/PMMA increases. On the other hand the pure
Fig. 4 FESEM photographs for different  Mg1−xCuxO/PMMA samples (a) Mg0.95Cu0.05O/PMMA (b) Mg0.9Cu0.1O/PMMA  (c) Mg0.85Cu0.15O/
PMMA (d) Mg0.8Cu0.2O/PMMA (e) SEM photograph with artistic

Journal of Inorganic and Organometallic Polymers and Materials
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Poly methyl methacrylate (PMMA) has high transmittance
due to the formation of layer of covalent bonds formed between polymer chains and Mg
1−xCuxO that decrease the
transmitting of the incident light particularly at the shortest wavelengths. This means that the electrons are emphatically connected to their atoms through covalent bonds and the breaking of electron linkage and moving to the conduction band require photon with high energy [40]. The transmission spectrum of pure PMMA reach to 90% while, Mg
1−xCuxO/
PMMA films show a decreasing in the transmission spec-
trum and the maximum transmission (70%) is clearly seen for x = 0.05 as seen in Fig.  5.
The absorbance is calculated from the relation between
incident intensity (I) and penetrating light intensity I
0 is
given by eq:
where t is the thicknesses of the film (cm) and α is the
absorption coefficient (cm)−1, where log (I/ I0) represents the
absorbance ( A). The absorbance spectra as function of the
wavelength for Mg1−xCuxO with different concentration of
Cu doped with PMMA is shown in Fig.  6. The absorbance
increases as x content of Mg1−xCuxO/PMMA increases. This
figure shows an increase in the absorption with increasing Cu content due to nanocrystalline [ 41]. Also, the absorption
spectra of polymeric nanocomposites showed no peak was observed in the visible region. This assures that the synthe-sized specimen could be used as UV-shielding block and UV-filters [12].
The absorption coefficient can be calculated by
Beer–Lambert’s law [42] as:(1)
I=I0e−/u1D6FCt
(2) /u1D6FC=2.303 log (A∕t)The relation between the absorption coefficient (α) and
the photon energy was represented in Fig.  7. It is shown
that an increase in the values of the absorption coefficient with the increasing of Cu content at higher energy which indicates the crystalline nature of the samples [43]. The absorption coefficient α (cm)
−1 value is constant and small
at low photon energy which means that the possibility of electron transition is little because the incident photon energy is not sufficient to transfer the electron from the valence band to the conduction band ( hυ < Eg ). While at
high photon energy the absorption coefficient value is big-ger and hence a great possibility for electron transitions.
Fig. 5 Transmittance spectra of Mg1−xCuxO/PMMA nanocomposite
films with different Cu contents
Fig. 6 The absorption spectra of Mg1−xCuxO/PMMA nanocomposite
films with different Cu content
Fig. 7 Absorption coefficient versus photon energy for all investi-
gated samples

Journal of Inorganic and Organometallic Polymers and Materials
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The absorption coefficient helps in finding out the nature
of electron transition, if the values of the absorption coef-ficient are low (α < 10
4) (cm)−1, it is expected that transi-
tion of electron is indirect and the electronic momentum is maintained with the assistance of the phonon [44].The optical energy band gap of the presented films is
related to the absorption coefficient by the following rela-tion [45, 46]:
where E
g, B, and hυ are the optical energy gap, constant,
the incident photon energy, respectively and m is the index (3) /u1D6FC(/u1D710)h/u1D710=B(h/u1D710−Eg)m
Fig. 8 Optical energy band gap of Mg1−xCuxO/PMMA nanocomposite films as a function of photon energy

Journal of Inorganic and Organometallic Polymers and Materials
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which can have different values of 1/2, 3/2, 2, and 3 depend –
ing on the nature of the electronic transition [47]. Fig-
ure 8a–e, represents the relation between (αhυ)1/2 for casting
materials as a function of photon energy. At the intercepts extrapolations of the curve to the values (αhυ)
1/2 = 0, the
indirect allowed gap transition is determined. It is found that, there are two indirect energies gaps. Moreover, these ener –
gies decrease with the increase of x content of Mg
1−xCuxO/
PMMA as shown in Fig.  9. The decrease in both energy
gaps may be due to the formation of the localized states
(additional energy levels) in the PMMA structure [48, 49].
So the transition of the conducting electron was done by two stages that include the transfer of electron from the valence band to the local levels to the conduction band. Also, the energy gaps are decreased because of the filler introduces electronic paths in the PMMA which facilitates the crossing of electron from the valance band to the conduction band [50] as seen by FESEM. The obtained results indicate the
possible application of Mg
1−xCuxO/PMMA nanocomposite
in optical switching devices, in visible region.
The relationship between the extinction coefficient (K)
and the wavelength is shown in Fig.  10. It is noted that K
increases as the Cu content increases due to higher absorp-tion coefficient. The extinction coefficient values (≈ 10
−4)
show that the samples still transparent [51]. The variation in the value of extinction coefficient is important in the application of optical devices [52].
Figure  11 shows the relation between the refractive
indices and the wavelength in the range 350–800 nm. It is indicated that the refractive indices increase with the increasing of x content of Mg
1−xCuxO/PMMA this may
be attributed to the increasing the packing density of
the investigated films. Moreover, the refractive index of the composite samples is tunable upon the addition of Mg
1−xCuxO powder concentration. Finally, it is found
that the small value of the refractive indices obtained in this work reveals that PMMA based polymer composites are very suitable as low-index claddings for wave guide applications [53]. The optical properties in this work con-firm that the refractive index and energy gap are strongly correlated.
3.3 Mechanical properties
Figure  12 shows the micro hardness as a function of Cu
content. The micro hardness increases as the x content
Fig. 9 The calculated energy gap of the nanocomposite films with
different Cu content
Fig. 10 The relation between the extinction coefficient and wave-
length for the prepared nanocomposite films
Fig. 11 The refractive index vs. wavelength for the prepared nano-
composite films with different Cu content

Journal of Inorganic and Organometallic Polymers and Materials
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of Mg1−xCuxO/PMMA increases until x = 0.15 and then
decreases. The enhancement in the value of micro hardness
may be due to adsorbed Cu nanocomposites among PMMA chains and act as a restriction sites for the movement of poly –
mer chains [54]. The micro hardness decreases after x = 0.15
may be due to the formation of coalescence behavior in the Cu nanocomposites as a weakening point.
The stress–strain behavior of PMMA was affected by
incorporation of Cu doped MgO and its concentration as shown in Fig.  13. The tensile properties, such as ten-
sile strength and elongation at break for pure PMMA and Mg
1−xCuxO doped with PMMA have been determined and the results are collected in Table  2. The value of tensile
strength was raised from 23.87 to 43.30 MPa with increas-ing the Cu content up to x = 0.1 and then it decreases with
increasing concentration of Cu. The enhancement in the ten-sile strength may be owing to the formation of high surface area of the filer so that it interacts with PMMA matrix and reduces the chain mobility [10]. The decrement in tensile strength can be referred to the filler–filler interactions which result in Mg
1−xCuxO agglomeration in the nanocomposites
as discussed by (FESEM). Filler coalescence was consid-ered as a weakening point that leads to the broken of the nanocomposite samples so easily when the stress was trans-ferred onto it, thus the tensile strength would decrease once the Mg
1−xCuxO concentrations increase. On the other hand,
incorporation Mg1−xCuxO with different concentration of
Cu leads to increase in the elongation at break compared to unfilled PMMA.
3.4 Dielectric Properties
The permittivity ε′ and dielectric loss ε″ as a function of both
frequency and Cu content were illustrated in Fig.  14a–d.
Firstly, ε′ and ε″ decrease with increasing frequency but ε′
till reaching a nearly constant value at higher frequencies as shown in Fig.  14a, c. It is known that the permittivity aris-
ing due to electronic, ionic, and dipole orientation contribu-tions to the polarizability. As the frequency of the applied field increased, both of the permittivity and dielectric loss decreased. The reason for this decreasing may be due that the dipoles are in arrears of the alternating field direction [55–57]. In this case, the polarization cannot reach the satu-
ration point and the permittivity decreases. Therefore, polar –
ization decreases which exhibits reduction in the values of ε ′
and ε″ with increase in frequency [58]. At higher frequency
the permittivity ε′ and dielectric loss ε″ tend to be constant
because the dipoles have no time to start the turn rapidly so that their oscillations begin to lag behind those of the applied field. Secondly, the variation of ε′ and tan δ with Cu content
in Mg
1−xCuxO in the polymer matrix (PMMA) was studied
and shown in Fig.  14b, d. This figure shows an increase in
ε′ and tan δ by increasing the Cu content in PMMA matrix.
This increase in both ε′ and tan δ is attributed to charge
Fig. 12 The relation between microhardness and Cu content for the
prepared nanocomposite films
Fig. 13 The stress–strain curve with different Cu content for
Mg1−xCuxO/PMMA nanocomposite filmsTable 2 Tensile strength and elongation at break values
Composition Tensile strength (MPa) Elongation
at break (%)
PMMA 23.87 ± 0.004 6 ± 0.3
Mg0.95Cu0.05O/PMMA 37.74 ± 0.007 15 ± 0.3
Mg0.9Cu0.1O/PMMA 43.30 ± 0.001 7 ± 0.3
Mg0.85Cu0.15O/PMMA 35.88 ± 0.002 14.±0.3
Mg0.8Cu0.2O/PMMA 26.46 ± 0.003 18 ± 0.3

Journal of Inorganic and Organometallic Polymers and Materials
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carriers (Cu2+ ions doped in MgO lattice) and introduces
more space charge into the polymer matrix especially in the
interfacial region. Figure  15 a shows the relation between ac
electrical conductivity and the frequency. It was seen that the electrical conductivity σ
ac increases as the frequency
increases in accordance to universal power law Aωs [59, 60]
where A is constant independent on temperature and the factor s is the frequency exponent. It was calculated from the slope of the logarithmic plot between σ and the angular frequency where 0 < s < 1. Stand on the attained results; s is
slightly decreasing by increasing x content of Mg
1−xCuxO/
PMMA, its values were listed in Table  3. Figure  15a shows
the higher increase of the ac conductivity as x content of Mg1−xCuxO/PMMA increases due to increase of the free
charges (growth of conducting phase) which makes them more frequency independent. The dc conductivity (σ
dc)
results from extrapolating the curves in Fig.  15a toward low
frequency. Figure  15b shows the relation between σdc and the
x content in Mg1−xCuxO/PMMA. It seems that, σdc increases
as the x content of Mg1−xCuxO/PMMA increases. Its values
increased from 1.17 × 10−12 to 6.5 × 10−10 (S m−1) as Cu
increased from 0 to 0.15 wt%. As the Cu increases up to
0.2 wt%, the percolation takes place and the conductivity increases to 4.91 × 10
− 9 (S m−1). The increment in σdc may
be due to (growth of conducting phase) and the formation of the pathway of the conductive filler as seen by FESEM
Fig. 14 The frequency dependence of permittivity ε′ and dielectric loss ε″ for Mg1−xCuxO/PMMA nanocomposite films with different Cu con-
tent

Journal of Inorganic and Organometallic Polymers and Materials
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[61] and also may be due to the formation of Cu2O second
phase as seen from X- ray.
4 Conclusion
Polymeric films based on PMMA filled Mg1−xCuxO,
0.05 ≤ x ≤ 0.2 by casting methods. The interaction between
inorganic nano fillers Mg1−xCuxO, 0.05 ≤ x ≤ 0.2 and poly –
mer matrix (PMMA) was confirmed using FTIR and XRD
studies. Well dispersion of Mg1−xCuxO nanoparticles in
the PMMA matrix and formation of cluster investigated by FMSEM. The optical properties of prepared composite material were performed by means of UV–Vis technique. The results showed a decrease in optical band gap, and an increase of absorption coefficient, extinction coefficient and refractive index with increasing the percentage ratio of Cu (Mg
1−xCuxO) in PMMA matrix. There is an enhancement
in mechanical properties. The microhardness increases as the Cu content increases up to x = 0.15 wt% after that
it decreases. The tensile strength was measured and raised from 23.87 to 43.30 MPa with increasing the Cu content up to x = 0.1 and then it decreases. The permittivity (ε′ ) and
dielectric loss (ε ″) decreased as the frequency increased but
(ε′) became constant at higher frequency range while they
increased as the Cu content increases. Also, the AC con-ductivity was measured to study the conduction mechanism in the presented nanocomposite films. The calculated dc conductivity increased as the Cu content in PMMA matrix increased. Finally, we can conclude that PMMA enhanced in optical, mechanical and dielectric properties by the addition of Mg
1−xCuxO. The nanocomposite material will be suitable
as low- index claddings for wave guide applications, UV-shielding block, UV-filters, and optical switching devices in visible region. Also, it will be suitable for calcifying tissue segmenting and ensuing histological examination.References
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