Device level optimization of poly(vinylidene fluoride-trifluoroethylene)–zinc oxide

polymer nanocomposite thin films for ferroelectric applications

,
Subash C K , Uvais Valiyaneerilakkal, Kulwant Singh, and Soney Varghese

Citation: J. Appl. Phys. 118, 204102 (2015); doi: 10.1063/1.4936203

View online: http://dx.doi.org/10.1063/1.4936203
View Table of Contents: http://aip.scitation.org/toc/jap/118/20
Published by the American Institute of Physics
 JOURNAL OF APPLIED PHYSICS 118, 204102 (2015)

Device level optimization of poly(vinylidene fluoride-trifluoroethylene)–zinc

oxide polymer nanocomposite thin films for ferroelectric applications
Subash C K,1,a) Uvais Valiyaneerilakkal,1 Kulwant Singh,1,2 and Soney Varghese1
1
Nanomaterials and Device Research Laboratory, School of Nano Science and Technology,
National Institute of Technology Calicut, Calicut, Kerala 673601, India
2
Department of ECE, B.K. Birla Institute of Engineering and Technology, Pilani, Rajasthan 333031, India
(Received 5 June 2015; accepted 5 November 2015; published online 24 November 2015)
Polymer nanocomposite was prepared using poly(vinylidene fluoride-trifluoroethylene) and zinc
oxide (ZnO) nanopowder, which are ferroelectric in nature. Nanocomposite was prepared in
various concentrations(0.2, 0.4, 0.8, and 1 wt. %) using probe ultra-sonication, followed by spin
coating and annealing at 120  C for 2 h to improve the formation of b-phase. Metal-ferroelectric-
metal capacitor was fabricated using this optimized thin film as a ferroelectric layer. Device level
optimization was carried out by polarization-electric field (P-E) hysteresis studies of this film,
which shows polarization enhancement of composite. Various characterization techniques like
atomic force microscopy, Fourier transform infra-red spectroscopy (FT-IR), Differential scanning
calorimetry, and X-ray diffraction were used to study the b-phase formation of nancomposite. The
capacitance–voltage (C-V) and current-voltage (I-V) characteristics were studied through varying
frequency and temperature. C-V measurements show an increase of 79% in the capacitance of
polymer nanocomposite, which can be used for the fabrication of ferroelectric devices. V C 2015

AIP Publishing LLC. [http://dx.doi.org/10.1063/1.4936203]

I. INTRODUCTION The material should provide enhanced properties which

Nanoelectronics, the emerging field of nanotechnology,
utilise various advanced materials. Nowadays, polymer
nanocomposite is extensively employed in day-to-day appli-
cations due to flexibility, lightness, and processability of
polymer. High performing polymer nanocomposite can play
an excellent role in nanoelectronics. Ferroelectric, piezoelec-
tric, and pyroelectric properties of materials are widely
employed in electronic devices. Ferroelectric and piezoelec-
tric polymer such as polyvinyledenefluoride (PVDF) has al-
ready attracted scientists in early 1970s. In addition to the
usual polymer properties mentioned above, an excellent fer-
roelectric switching property triggered the industrial impor-
tance of this polymer.1–3 Four different phases of this
material exists, namely, a, b, c, and d with different proper-
ties. b-phase of this material attracted more interest, particu-
larly for ferroelectric properties; this phase of the material
could be obtained by improving crystalline by annealing,
and orientation of dipoles can be increased by poling pro-
cess. Copolymerization of PVDF and trifluoroethylene
(TrFE) will form poly(vinylidene fluoride-trifluoroethylene)
[P(VDF-TrFE)], which is one of the most promising ferro-
electric copolymer of PVDF. The extra fluorine atom enhan-
ces b phase; hence, properties will be more predominant.
This copolymerisation will provide 80% enhancement in
crystallinity; hence, the polarization characteristics of this
material will be high under applied electric field.
Enhancement in ferroelectricity is the result of electronega-
tivity difference between fluorine, carbon, and hydrogen;
thus, polarisation will be very high due to high electronega-
tivity of fluorine.4–6
a)
Electronic mail: cksubash08@gmail.com
will be useful for a wide range of applications. Some ceramic
nanoparticle which is having same property may give a syner-
getic effect to polymer composite. Functional inorganic pow-
ders such as barium titanate and lead zirconium titanate are
also well known for this interesting property.7–10 The main
drawback of ceramic material is its brittleness. This can be
overcome by using polymer materials in polymer based flexi-
ble systems, which would be a great achievement. Thus, it is
expected to get a synergetic effect in properties while making
a composite of a ferroelectric polymer and nanoparticles.
Properties of composite depend mainly on the method of prep-
aration and dispersion of nanoparticle in polymer matrix.11–14
If it is possible to get an enhancement in beta phase of mate-
rial, then properties will be highly useful for various device
level applications. The optimization of material concentration
will play an important role here, so it is essential to study the
relation between increment in properties and quantity of addi-
tion of inorganic nanoparticle. Device level optimization stud-
ies will give more impact to this material.
Zinc oxide is one of the important inorganic ceramic
materials showing a wide range of properties. The ferroelec-
tric and piezoelectric behaviour of zinc oxide can play an im-
portant role in sensor and energy harvesting applications.15–17
Pure P(VDF-TrFE) polymer polarization switching behaviour
was previously reported by Mao et al.18 by fabricating MFM
capacitors. Enhancement in remnant polarization and piezo-
electric activity by adding higher amount of zinc oxide in
P(VDF-TrFE) was reported by Dodds et al.19 Nguyen et al.
studied the influence of size and surface functionality of zinc
oxide nanoparticle on piezoelectric properties of P(VDF-
TrFE) nanocomposite.20 Cardoso et al. reported electroactive
response of spin coated P(VDF-TrFE) thin films for sensors.21
Here, in this work, property enhancement of the polymer by

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V
204102-2 K et al.
FIG. 1. Schematic of the fabricated device structures with bottom and top aluminium metallization.
the addition of zinc oxide was studied. The major beta phase
enhancement of composite material by the addition of various
concentration of ceramic nanomaterial was characterized by
atomic force microscopy (AFM), Fourier transform infra-red
spectroscopy, X-ray diffraction (XRD), and device level opti-
mization of various concentration was carried out by
polarization-electric field (P-E) hysteresis analysis of fabri-
cated MFM capacitors. By utilizing optimized concentration,
Metal–Ferroelectric–Insulator–Semiconductor (MFIS) devices
are fabricated and C-V and I-V analysis was carried out.
II. MATERIAL AND METHODS
P(VDF-TrFE) copolymer powder having 70 mol. %
(VDF) and 30 mol. % (TrFE) was purchased from Solvay
Solaxis, Italy, and was directly used. ZnO nanopowder hav-
ing size of 40–100 nm was purchased from Alfa Aesar.
Initially, different concentrations of ZnO nanoparticle (0.2,
0.4, 0.8, and 1 wt. % with respect to polymer) were well dis-
persed in methyl ethyl ketone (MEK) by sonication for 5 h,
and then, a known quantity of P(VDF-TrFE) powder was
dissolved in each concentration by magnetic stirring for 2 h.
This dissolved nanocomposite solution was coated on well
cleaned glass substrate using spin coating unit (SPS 150) at
an rpm of 1500 for 45 s. The coated film was dried and kept
at 120  C for 2 h in oven and allowed for slow cooling, to
enhance the formation of b phase in material.18
The morphology of ZnO and polymer nanocomposite was
investigated using field emission scanning electron microscope
(FESEM, Hitachi SU6600) at 20 kV accelerating voltage, and
secondary electron images were captured. The elemental map-
ping was carried out using energy dispersive spectrometer
(Horiba, Japan) attached with FESEM. The crystallinity of the
composite thin films was studied by using XRD technique
(Rigaku Miniflex 600 with CuKa radiation (k ¼ 0.15406 nm))
and Fourier transform infrared spectrometer (FT-IR) (Jasco
FTIR 4100). Differential scanning calorimetry (DSC) analysis
was performed using TA instruments Q20-DSC machine at a
heating/cooling rate of 10  C/min in N2 atmosphere. The ther-
mal history of polymer nanocomposite was removed by a heat-
ing and cooling cycle, and enthalpy of fusion was measured in
the third heating cycle. The heat of fusion was directly
obtained from the TA instruments software (TA Universal
analysis). The surface topography was measured using a Park
XE-100 AFM in non-contact mode using silicon nitride canti-
levers with a scanning speed of 1 Hz at a scan size of 20 lm2.
A thin film of nanocomposite was sandwiched between the
J. Appl. Phys. 118, 204102 (2015)
two metal electrodes as a metal-ferroelectric-metal (MFM) ca-
pacitor, different compositions are spin coated over copper
substrate by using spin coater (film thickness of 1 lm), and al-
uminium top electrode was deposited using a hard mask
(500 lm radius) by thermal evaporator. Polarization-voltage
(P-V) study was carried out using a ferroelectric tester
(Precision Premier II, Radiant Technology, Inc.).
Different MFIS devices were fabricated by following the
process flow, and 2 in. p type silicon wafer (1–5 X cm) was
used as a substrate. Oxidation process was carried out using
the dry thermal oxidation method at 1100  C in batch fabrica-
tion of five wafers. The oxide thickness measured on a single
wafer at different surfaces was in the range of 9–10 nm. The
polymer nanocomposite was spin coated on the top of Si/SiO2
stack by using optimized recipe for a thickness of 300 nm.
The top aluminium metal electrode was coated by thermal
evaporation by using a hard mask. Back metallization was
also carried out by using thermal evaporator after successful
back etching of oxide layer. The fabricated MFIS devices
structures are shown in Figure 1, and the thicknesses of differ-
ent layers are confirmed by using Ellipsometer and
Profilometer. Device level characterizations were carried out
using Keithley Model 4200-SCS probe station.
III. RESULTS AND DISCUSSION
Figure 2 shows the FESEM images of nano-ZnO pow-
der, which was used for the preparation of polymer nano-
composite. The particle size was found to be in the range of
40–100 nm with rod shape morphology.
FIG. 2. Scanning electron microscopic image of ZnO nanopowder showing
size in the range of 40–100 nm.
204102-3 K et al. J. Appl. Phys. 118, 204102 (2015)

FIG. 3. (a) Fourier transform infra-red spectrum, (b) X-ray diffraction pattern of P(VDF-TrFE)/ZnO nanocomposites, and (c) X-ray diffraction pattern of ZnO
nanopowder.

P(VDF-TrFE) while annealing crystallises in ferroelec-

tric b-phase, and the addition of nanoparticles can further
increase the formation of b-phase. This enhancement in crys-
tallinity was studied using FTIR spectrometer and XRD
techniques. Figure 3(a) shows FTIR spectrum of the polymer
nanocomposite with different concentrations of ZnO.
Characteristic vibration bands of P(VDF-TrFE) and its nano-
composites were analysed within the frequency range of
400–4000 cm1. Peaks observed at 1288 cm1, 850 cm1,
and 1400 cm1 are associated with b-phase of the mate-
rial.22–24 The peaks at 1288 cm1 and 850 cm1 belongs to -
CF2 symmetric stretching, and 1400 cm1 band is assigned
to the -CH2 wagging vibration. Vibrations associated with
symmetric CF2 stretching at 1288 cm1 are important char-
acteristics of b-phase peak, which lead to the polarization
and are also visible in the spectrum.25–30 The all bonds above
are highly sensitive to dipole orientation towards the applied
electric field. There are other frequencies associated with the FIG. 4. Differential scanning calorimetric thermogram of P(VDF-TrFE)/
–C-F and C-C bonds on which the applied electric field ZnO polymer nanocomposite.
204102-4 K et al.
influences are insensitive.2 Intensity variation in I-R peaks
shows the enhancement in b-phase of nanocomposite.
Quantitative identification of b-phase was done by calculat-
ing absolute area under the characteristic b-phase peak at
850 cm1. 235% increment in area was observed for 1%
ZnO added composite sample while comparing with pure
sample. Addition of nano-ZnO acts as a seeding nucleus in the
formation of electroactive b-phase. Martins et al. explain the
formation of b-phase by the addition of nanofillers. During sol-
vent casting or spin coating process, the nanofillers will be
encapsulated by the polymer film, and during the drying pro-
cess, the nucleation of the polymer occurs on the surface of the
negatively charged ZnO. The positive side of the PVDF-TrFE
chain interact with this negative charge on the surface of ZnO
and align in the extended trans trans trans (all trans) conforma-
tion, leading to the ferroelectric b-phase.31,32
X-ray diffraction analysis was also carried out for identi-
fying b-phase enhancement by the addition of piezoelectric
nanomaterial. Figure 3(b) shows XRD results obtained for
polymer nanocomposite with different ZnO loading. The
increase in intensity of the peak at 20 corresponds to the
b-phase of the polymer. The diffraction peak at 2h value
nearly at 20 corresponds to (110) and (200) orientation
planes of the polar b-phase. The gradual increase in the in-
tensity of peak was a clear indication of increase in crystal-
line b-phase content of polymer nanocomposite. XRD
analysis was carried out to find quantitative increase in the
b-phase content. The area under the characteristic peak was
calculated22 for each concentration. The intensity of the
characteristic peak was gradually increased, as shown in
Figure 3(b). For 1% ZnO polymer nanocomposite, there is a
210% increase in area with respect to the pure polymer.
These results support the enhancement of the b-phase con-
tent in the polymer by the addition of ZnO nanopowder.
J. Appl. Phys. 118, 204102 (2015)
FIG. 5. AFM topography of pure
P(VDF-TrFE) and optimized 1%P
(VDF-TrFE)/ZnO nanocomposite.
Figure 3(c) shows XRD pattern of ZnO nanopowder, and
characteristic planes of the ZnO are present in the data.
The change in crystallinity of nanocomposite was also
investigated using DSC measurements. Figure 4 shows DSC
thermogram of pure and polymer nanocomposite sample.
The percentage crystallinity of pure and nanocomposite was
extracted from the heating curve by using change in enthalpy
value 104.7 J/g for the melting enthalpy of 100% crystalline
PVDF. The pure polymer shows a heat of fusion of 31.64 J/g
and 29% crystallinity, but by the addition of 1% ZnO, the
heat of fusion increased to 34.77 J/g and the crystalline phase
becomes 33%. The results show enhancement in crystallinity
by the addition of nano-ZnO into the polymer matrix.
The topography of polymer nanocomposite was studied
using AFM technique in the non-contact mode. Figure 5
shows the AFM images of pure P(VDF-TrFE) and polymer
nanocomposite with 1% ZnO concentration. Nest like struc-
ture was observed for the pure polymer, which is a typical
b-phase character. In the case of polymer nanocomposite, a
completely different morphology was observed. During the
formation of polymer nanocomposite solution, the nanofiller
will be covered by the polymer chains, and after spin coat-
ing, the films show core–shell morphology. Figure 6 shows
the FESEM images of the pure polymer and the polymer
nanocomposite. The nest like morphology was also visible in
this micrograph of the pure polymer. The distribution of the
nano-ZnO in the polymer matrix was studied using energy
dispersive spectroscopic (EDS) mapping technique. Figure 7
shows EDS elemental mapping of the polymer nanocompo-
site sample. It was observed that there is a uniform disper-
sion and distribution of nanoparticles in the polymer matrix.
The polarisation–electric field (P-E) analysis was carried
out in a metal-ferroelectric-metal (MFM) capacitor. P-E hys-
teresis loops for different composition of ZnO in P(VDF-
FIG. 6. FESEM images of pure
P(VDF-TrFE) (left), P(VDF-TrFE)/
ZnO(right) nanocomposite with 1%
ZnO concentration.
204102-5 K et al.
TrFE) with a film thickness of 1 lm at a frequency of 100 Hz
are shown in Figure 8. Remnant polarisation, coercive volt-
age, and saturation polarisation values of composite were
improved by the addition of nanoparticle. The results show
improved polarization capability of polymer nanocomposite.
Remnant polarization (Pr) of the composite was
increasing gradually by the addition of nanoparticle, and
the hysteresis loop becomes more and more open in the
polarization direction. Quantitatively, the Pr value of the
pure polymer in this MFM device was 3.43 lC/cm2, and Pr
was increased to 4.67 lC/cm2 for 1% ZnO added composi-
tion. This is corresponding to 37% increase in polarization.
The coercive voltage of the composite was decreased to
61 V from 64 V, and the capacitance of MFM with polymer
nanocomposite was improved to 3.36 nF from 2.33 nF.
FIG. 8. Polarisation (P) vs applied voltage/thickness (V/t) hysteresis loop
measured at a frequency of 100 Hz for different concentrations of ZnO in P
(VDF-TrFE).
J. Appl. Phys. 118, 204102 (2015)
FIG. 7. Energy dispersive spectros-
copy elemental mapping of P(VDF-
TrFE)/ZnO nanocomposite with 1%
ZnO content.
These results can be attributed to the increased formation of
b-phase in the composite by the addition of nano-ZnO and
its synergistic effect.
The device level optimization of thin film was carried
out by fabricating different device structures. The thickness
of polymer thin film was kept constant for uniformity and
comparison. Different devices like MFS1 (Al/P (VDF-
TrFE)/Si), MFS2 (Al/P(VDF-TrFE) þ ZnO/Si), MIS3(Al/
SiO2/Si), MFIS4 (Al/P(VDF-TrFE)/SiO2/Si), and MFIS5
(Al/P(VDF-TrFE) þ ZnO/SiO2/Si) were fabricated, and the
breakdown voltage was analysed, which is shown in Figure
9. The results shows devices MFS1 and MFS2, which were
deprived of SiO2 failed at lower voltage, i.e., less than 7 V.
In the case of other devices, MIS3, MFIS4, and MFIS5 are
having 10 nm SiO2 layer. Among these, MIS3 was taken as a
reference without any ferroelectric polymer film, and the
breakdown voltage was found to be 9 V. The devices with
FIG. 9. A comparative study of breakdown voltage of different devices.
204102-6 K et al.
300 nm polymer film and 10 nm SiO2, MFIS4, and MFIS5
show a breakdown voltage of 23 and 24 V, respectively. The
devices without oxide layer (MFS1 and MFS2) were not
withstanding in higher voltage. So, to demonstrate the effi-
ciency of optimized material in device applications, higher
voltage withstanding devices with small oxide layer (MFIS4
and MFIS5) was further characterized.
Capacitance–Voltage/thickness (C-(V/t) responses of dif-
ferent devices are recorded. Figure 10(a) shows the C-V/t
response of MIS structure with 10 nm SiO2, and there is no
hysteresis loop in the output as expected since there is no fer-
roelectric polymer in the device. Figures 10(b)–10(d) shows
very strong hysteresis due to the polarization of the material.
The hysteresis behaviour was visible in the graph, and the
polarization efficiency was clear from the capacitance value.
In the case of the pure polymer (Figure 10(b)), the capacitance
drastically changed with an increment in frequency in contrast
to the nanocomposite polymer (Figure 10(c)). The maximum
values of capacitance were 5.2  109 F at 0.015 V/t for
MFIS5 (Nanocomposite) and 2.9  109 F for MFIS4 (pure
polymer) at a frequency 10 kHz. The influence of frequency
on C-V curves for nanocomposite devices is negligible
(MFIS5). Therefore, it has the potential application at high
FIG. 10. Capacitance–Voltage/thickness (C-(V/t)) recordings of different device: (a) Al/SiO2/Si device (MIS3); (b) Al/SiO2/P(VDF-TrFE)/Si device (MFIS4);
and (c) Al/SiO2/P(VDF-TrFE) þ ZnO/Si device(MFIS5). (d) Comparative plot of Al/SiO2/P(VDF-TrFE)/Si device(MFIS4) and Al/SiO2/P(VDF-TrFE) þ ZnO/
Si device(MFIS5) at 10 kHz.
J. Appl. Phys. 118, 204102 (2015)
frequency with stable performance. Figure 10(d) shows the
comparative C-V/t behaviours (MFIS4 and MFIS5), and the
results pave the way for realization of the cost effective ZnO
nanocomposite based FETs for memory application at higher
frequency.
Temperature dependent C-V/t performance was investi-
gated. In device point of view, temperature dependent stud-
ies are also important. The temperature was varied from 25
to 80  C. Figure 11(a) shows the C-V/t graph of the pure
polymer MFIS4 device. The polarization and capacitance are
changing with temperature. The increase in capacitance was
due to higher polarization in the presence of higher tempera-
ture. Figure 11(b) shows the C-V recordings of the polymer
nanocomposite MFIS5 device acquiring almost similar high
accumulation capacitance at different temperatures. So, it is
observed that the device with polymer nanocomposite shows
a better stability at different temperatures. The device level
optimization of this material shows higher and stable polar-
ization at different temperatures. The C-V characteristic at
different temperatures shows the existence of hysteresis
loop, which indicates the acceptance of the material at a
higher temperature. The studies were carried out below the
Curie temperature of P(VDF-TrFE), which is 80  C. From
204102-7 K et al. J. Appl. Phys. 118, 204102 (2015)

FIG. 11. Temperature dependent Capacitance–Voltage/thickness (C-V/t) recordings of MFIS device: (a) Al/SiO2/P(VDF-TrFE)/Si device(MFIS4) and (b) Al/
SiO2/P(VDF-TrFE) þ ZnO/Si device(MFIS5).

initial material study onwards, the polymer nanocomposite ACKNOWLEDGMENTS

material shows enhanced polarization behaviour when com-
The authors would like to acknowledge the entire staff of
pared with the pure polymer, and similar results are obtained
CEN, IITB, and SNST, NIT Calicut. Device fabrication and
in device level optimizations.
characterization was carried out at IITBNF, IITB under INUP,
which is sponsored by DeitY, MCIT, Government of India.
IV. CONCLUSION
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