IEEE Transactions on Ultrasonics, Ferroelectrics, and Frequency Control ,
8, August 2009 1627
Preparation and Characterization of the
Ferroelectric Potassium Nitrate:
Poly(vinyl alcohol) Composite Films
Navneet Dabra, Jasbir S. Hundal, Koppole Chandra Sekhar, Arvind Nautiyal, and Rabinder Nath
Abstract—The composite films of ferroelectric potassium ni-
trate (KNO3):poly(vinyl alcohol) (PVA) with different weight
percentages of KNO3 have been prepared at 200°C using the
spray-deposition technique. The remanent polarization (Pr)
and peak current density for all composite films was estimated
by tracing the polarization-electric field (P-E) hysteresis loop
and current density-electric field (J-E) loop, respectively, us-
ing a modified Sawyer-Tower circuit. Pure KNO3 is known not
to exhibit any ferroelectricity under ambient conditions, but
the X-ray diffraction (XRD) studies of PVA:KNO3 composite
films reveal the presence of a ferroelectric phase III of KNO3
in the composite films at room temperature. The composite
film containing KNO3:PVA in equal proportions shows maxi-
mum Pr and peak intensity ratio of approximately 20.10 μC/
cm2 and 2.67, respectively, at room temperature. The J-E and
capacitance voltage (C-V) characteristics exhibit butterfly fea-
tures that supports the presence of a ferroelectric phase in the
composite films. The field emission scanning electron micros-
copy (FE-SEM) image of the composite film containing equal
proportions of KNO3 and PVA shows the homogenous distri-
bution of spherical grains of KNO3 of size ~225 nm.
I. Introduction
T he composite materials with ferro-, pyro-, and piezo-
electric properties have been the focus of continuous
interest, because these can be tailored to sensor and trans-
ducer applications [1]–[3]. Ferroelectric materials possess
spontaneous polarization even at zero electric field, and
their polarization can be switched under the influence
of the external electric field [4]. The pure potassium ni-
trate (KNO3) crystals exist in phase II with orthorhom-
bic (aragonite) crystal structure at room temperature and
atmospheric pressure. It changes to phase I (rhombohe-
dral crystal structure) above 130°C. On cooling, phase I
of KNO3 does not directly revert back to phase II but
through an intermediate metastable phase III, which is
ferroelectric in region ~124 to 110°C. On further cooling,
it changes to phase II [5], [6]. The ferroelectric ceramic-
polymer composites have attracted a great deal of atten-
tion as they combine the ferroelectricity of the ceramic
material with the good mechanical properties of the poly-
Manuscript received November 14, 2008; accepted May 2, 2009.
N. Dabra and J. S. Hundal are with the Applied Physics and Materials
Science Laboratory, Department of Applied Sciences, Baba Farid College
of Engineering and Technology, Punjab, India (e-mail: navneetdabra@
gmail.com and jshundal@yahoo.com).
K. C. Sekhar, A. Nautiyal, and R. Nath are with the Ferroelectric Ma-
terials and Devices Research Laboratory, Department of Physics, Indian
Institute of Technology, Roorkee, Uttarakhand, India.
Digital Object Identifier 10.1109/TUFFC.2009.1227
0885–3010/$25.00
vol. 56, no.
mer. The embedded ferroelectric ceramic particles in long
chain molecules of the polymers make these films very
flexible and viscoelastic, thus increasing the possibility
of making large area devices because these films possess
large dielectric relaxation [2]. The proper combination of
the ceramic and polymer with definite weight percent-
age ratio allows the fabrication of the new materials with
desired ferroelectric properties such as low coercive field,
because the presence of the polymer is known to modify
the local electric field distribution inside the composite [2].
These films also possess good electromechanical proper-
ties, flexibility, and reasonable mechanical strength [1]–[3].
The ferroelectric ceramic-polymer composites have a great
potential for applications in the field of microelectronics,
microelectromechanical systems (MEMS) [7], memory de-
vices such as ferroelectric random access memories (Fe-
RAMs), nonvolatile random access memories (NVRAMs),
ferroelectric field effect transistors (FeFET), and organic
ferroelectric field effect transistors (OFeFET) [8], [9]. The
remanent polarization and phase stability were found to
have been improved in ceramic-polymer composite sys-
tems such as sodium nitrite (NaNO2):polyvinyl alcohol
(PVA) [10], KNO3:poly(vinylidene fluoride) (PVDF) [11],
[12], KNO3:polyvinyl fluoride (PVF) [13], triglycine sulfate
(TGS):PVA [14], [15], barium titanate (BiTiO3):PVDF
[16], and lead zirconate (PZT):polyurethane (PU) [17].
Usually, the ceramic-polymer composites have been
prepared by the inclusion of polymer matrix in ceramic
materials by melt press [2], [11]–[13], sol-gel [2], [18]–[20],
solvent cast [21], [22], and intercalation techniques [23],
[24]. However, under suitable conditions, composite films
obtained from the solvent cast and sol-gel process allows
for the better control of the chemical composition of ce-
ramic and polymer due to proper molecular interactions.
The composite films obtained by these methods yield ce-
ramic-polymer with better electroactive and ferroelectric
properties [2]. It has been reported that the preparation
of the composite films of NaNO2, selenide with PVA us-
ing solvent cast technique was helpful in controlling the
growth of NaNO2, and selenide nanoparticles [10], [22].
Many studies using techniques such as far infrared [25],
neutron diffraction [26], inelastic neutron scattering [27],
Raman spectroscopy [28], [29], X-ray [30]–[32], differen-
tial scanning calorimetric [33]–[35], dielectric [36], electri-
cal and thermal conductivity [36], [37], and ferroelectric
[38]–[41], have been carried out in the past by various
researchers to examine the nature of the phase transitions
in KNO3. The technological interest in KNO3 thin films
© 2009 IEEE
1628 IEEE Transactions on Ultrasonics, Ferroelectrics, and Frequency Control , vol. 56, no. 8, August 2009

originates due to the reason that these films have low op-
erating voltage and fast switching response. These are be-
ing employed as ferroelectric capacitors, memory element,
nonvolatile memory devices (NV-RAMs), and dynamic
random access memories (DRAMS) [42], [43]. Recently,
the spray-pyrolysis [44]–[47] and ultrasonic nebulizer tech-
niques [48] have also been employed to prepare the thin
films of various pure ceramics.
In the present article, the composite films of potassium
nitrate KNO3 and PVA with different weight percentages
have been prepared using a spray-deposition technique
[47] with the aim of stabilizing ferroelectric phase III of
KNO3 at room temperature in the new environment. The
KNO3 is known to exhibit ferroelectric properties in phase
III [38]–[40], and PVA has high viscosity, common aque-
ous solubility as KNO3. The composite films so prepared
have better mechanical strength [10] in comparison to
brittle pure KNO3 films. The remanent polarization of
the ferroelectric KNO3:PVA composite films have been
studied by hysteresis loop (P-E). The capacitance-voltage
(C-V) and current density-electric field (J-E) characteris-
tics have been studied to characterize the ferroelectricity
in the composite films. The correlation between electrical
Fig. 1. Flowchart for the preparation of the composite films of KNO3:PVA
and structural properties and the studies on stability of using spray-deposited technique.
ferroelectric phase III in the composite films have been
investigated using the X-ray diffractions (XRD) of the
composite films. The hysteresis loop (P-E) and current density-electric
field (J-E) characteristics of the composite films have been
studied using modified Sawyer-Tower circuit [11] connect-
II. Experiment ed with a storage oscilloscope and computer. The X’Pert-
Pro X-ray diffractometer (PANalytical B.V., Almelo, The
Potassium nitrate powder supplied by E. Merck (In- Netherlands) with Ni-filtered Cu Kα radiation of wave-
dia) Limited (Mumbai, India) was dissolved in double- length 0.154 nm was used for X-ray diffraction studies of
distilled water until saturation. The solution was kept for the composite films. The field emission scanning electron
few days in a closed environment. The KNO3 crystals that microscopy (FE-SEM) was used to study the distribu-
developed in the solution were taken out, dried in vacuum tion and grain size of KNO3 in PVA matrix. The capaci-
oven at 130°C, and then powdered. The composite films tance-voltage (C-V) characteristics were recorded at room
of powdered KNO3 and PVA were prepared with varying temperature using a Keithley C-V analyzer (590 model,
compositions ranging from 20 to 90% by weight of KNO3. Keithley Instruments, Inc., Cleveland, OH).
For a particular composition, the powders of KNO3 and
PVA weighing a total of 200 mg were dissolved in 50 mL
of double-distilled water at 40°C while stirring [10], [49]. III. Results and Discussion
The deposition of the composite films of KNO3:PVA with
different wt.% of KNO3 was done using the spray-deposi- A. Structural Properties
tion procedure. The details of spray-deposition setup, flow
rate, and carrier gas pressure have been communicated XRD and Field Emission Scanning Electron Micros-
elsewhere [47]. The flowchart for the preparation of com- copy: The XRD measurements were performed to obtain
posite films is shown in Fig. 1. The smooth well-polished the information about the existence of the ferroelectric
circular brass discs of diameter 1 cm and thickness 2 mm phase III in the composite films deposited at optimized
were used as substrates for the deposition of the com- temperature. Fig. 2 shows the X-ray scans of pure PVA,
posite films of varying compositions. The composite films pure KNO3 powder, and composite films of varying wt.%
approximately 14 µm thick with varying composition of KNO3. The most common diffraction peaks of phase
were prepared at optimized substrate temperature, i.e., II at 2θ = 23.57°, 23.83°, 29.40°, 32.33°, and 32.82° were
200°C. Each film was then annealed at 200°C for 50 h and observed in the KNO3 powder for the planes of (h k l)
then slowly cooled down to room temperature. Indium values (111), (021), (012), (102), and (112), respectively.
electrodes [50] of cross-sectional area ~1.867 × 10−2 cm2 These peaks have also been seen in the XRD patterns of
were deposited by thermal evaporation under the vacuum KNO3 taken by Schaffer and Mikkola [41]. The lattice pa-
~2.0 × 10−5 mbar onto the respective composite films. rameters a, b, and c for KNO3 have been calculated from
dabra et al.: preparation and characterization of KNO3:PVA composite films
Fig. 2. X-ray scan of (a) pure poly(vinyl alcohol) and composite films
containing (b) 20, (c) 40, (d) 50, (e) 70  wt.% of KNO3, and (f) pure
KNO3 powder.
XRD pattern for pure KNO3 and were found to be 6.552,
5.472, and 9.028 Å, respectively. These values are in good
agreement with the values previously reported in the lit-
erature [51]. PVA film has amorphous nature and exhibits
a broader diffraction peak around 2θ~20.0° corresponding
to (101) [24], whereas the brass (substrate) peaks occurred
at 2θ = 31.44 o and 36.41°.
The composite films exhibit the ferroelectric phase III
peak at 2θ = 29.71° corresponding to (003) reflection and
another peak at 2θ  =  29.52° for (012) reflection for the
phase II in addition to the peak around 2θ = 19.6° that
corresponds to PVA. However, the XRD pattern of the
pure KNO3 powder exhibits a phase II peak at 2θ = 29.4°
and no peak corresponding to the phase III. The earlier
X-ray studies by other workers also suggest the existence
of ferroelectric peak around 2θ = 29.8° in addition to peak
corresponding to phase II around 2θ  =  29.5° in mixed
KNO3 systems. The composites films of the KNO3:PVDF
were also known to exhibit enhanced phase III peak at
2θ = 29.8° [12]. Therefore, the present X-ray studies sug-
gest that ferroelectric phase III has developed in the
KNO3:PVA composite films.
The variation of the ratio of peak intensity of the phase
III to peak intensity of the phase II as a function of vary-
ing wt.% of KNO3 in the composite films is depicted in
Fig. 3(a). The relative intensity of phase III to phase II
was estimated and found to be a maximum of 2.67 for the
composite films with 50 wt.% of KNO3.
Field emission scanning electron microscopy (FE-SEM)
has been employed to obtain the grain size and distri-
bution of KNO3 in the PVA matrix. Fig. 4 shows the
FE-SEM images of the composite films of varying wt.%
of KNO3. The images of the composites exhibit spherical
grains of KNO3 with an average size in the range of 195
to 310 nm with increasing composition; see Fig. 3(b). The
image of the composite film containing 50 wt.% of KNO3
1629
Fig. 3. Variation of (a) peak intensity ratio and (b) average grain size
with wt.% of KNO3 in composite films.
show the uniform distribution of KNO3 in PVA matrix
and grain size of ~225  nm. Earlier studies using atomic
force microscopy (AFM) technique also revealed grain size
of similar order in these films having this composition [52].
However, the clustering of the KNO3 particles has been
observed in the composite films above 50 wt.% composi-
tion of KNO3. The clustering creates porosity that might
be responsible for the decrease of Pr above the 50 wt.%
composition [10].
B. Electrical Properties
1) Hysteresis Loop and Current Density-Electric Field
(J-E) Characteristics: The ferroelectric hysteresis loops
(P-E) of the composite films with varying compositions
of KNO3:PVA were recorded at room temperature using
a 50 Hz sine wave signal. Fig. 5 shows the P-E loops ob-
served for the 20, 40, 50, and 70  wt.% of KNO3 com-
posite films, respectively, prepared at optimized tempera-
ture. The value of Pr increases up to 50  wt.% of KNO3
in the composite films and beyond this, the Pr shows a
decreasing trend. The value of Pr was estimated in each
composite film and the optimum value was found to be
~20.10 μC/cm2 for the composite film with equal propor-
tions of KNO3 and PVA as shown in Fig. 5(a). A similar
pattern in the variation of Pr has been reported in the
KNO3:PVDF and NaNO2:PVA composite films [10], [12].
It was found that the Pr remains independent of the elec-
trode area. The coercive field (Ec) decreases with increase
of the KNO3 content in the composite films. Fig. 5(a)
shows dependence of Ec on the wt.% of KNO3 in the com-
posite films. The composite films with more than 50 wt.%
KNO3 content were found to be more brittle. In view of
this observation, the composite films with 50:50 wt.% of
KNO3 and PVA were chosen for further ferroelectric stud-
ies. The value of the Pr ~20.10 μC/cm2 in these spray-de-
posited films is more than 4 times as reported in the poled
KNO3:PVA films prepared by solvent cast technique [53]
1630 IEEE Transactions on Ultrasonics, Ferroelectrics, and Frequency Control , vol. 56, no. 8, August 2009

Fig. 4. The field emission scanning electron microscopy images of the composite films containing (a) 20, (b) 50, (c) 70, and (d) 90 wt.% of KNO3.

TABLE I. Composition Dependence of Various Parameters in Ferroelectric KNO3:PVA Composite

Films.
Pr Ec J Intensity ratio = Peak IIII / Grain size Cmax
Wt. % of KNO3 (μC/cm2) (kV/cm) (mA/cm2) Peak III (nm) (nf)
20 3.95 4.25 6.43 0.995 195 0.06
30 7.02 4.02 12.02 1.23 200 0.10
40 12.06 3.60 20.99 1.96 217 0.15
50 20.10 3.42 37.04 2.67 225 0.21
60 15.4 3.33 25.42 2.02 241 0.18
70 8.76 3.29 13.42 1.30 264 0.14
80 4.25 3.25 7.07 0.79 296 0.09

and about more than twice that observed in pure fused
KNO3 films [40]. This value of Pr is slightly greater than
that reported for KNO3:PVDF composite films prepared
by hot press method [12] and approximately half that of
the fused KNO3:PVDF [11].
The current density-electric field (J-E) studies carried
out on these composite films depict the butterfly behavior
(figure not shown) in each composition with maximum
current density ~37 mAcm−2 for the composite film con-
taining equal proportions of KNO3 and PVA as shown.
Fig. 5(b) shows the variation of current density (J) with
the wt.% of KNO3 in the composite films.
2) Capacitance Voltage (C-V) Characteristics: Fig. 6
depicts the C-V characteristics of the composite films of
varying compositions taken at frequency ~100 KHz. The
applied voltage was varied between from −15 V to +15 V
with step bias of 1 V and vice versa for forward and re-
versed cycles. Two sharp peaks were observed in the C-V
characteristics of all the composite films. The Cmax was
highest in the films containing equal proportions of KNO3
and PVA as shown in Fig. 6 (inset). The orientations of
domains along the field direction are responsible for in-
crease in the capacitance during voltage variation. The
maxima in C-V occur close to Vc for each composition.
dabra et al.: preparation and characterization of KNO3:PVA composite films 1631

Fig. 5. Hysteresis loops (P-E) of the composite films composed of (a) 20, (b) 40, (c) 50, and (d) 70 wt.% of KNO3. (a) Composition dependence of
Pr and Ec in composite films; (b) variation of peak current density with wt.% of KNO3 in composite films.

Fig. 6. Capacitance-voltage characteristics of the composite films of (a) 20, (b) 40, (c) 50, and (d) 70 wt.% of KNO3. (Inset): Variation of normalized
Cmax with composition in composite films.

The maximization of the domain wall motion and forma-
tion of new domain close to Vc could be responsible for
occurrence of peaks in C-V spectra [10], [54]. The nonlin-
ear behavior (butterfly) observed in C-V spectra strongly
indicates the presence of ferroelectricity in the composite
films [10], [12], [13]. The variation of Pr, Ec, J, intensity
ratio, grain size, and Cmax with different weight percent-
ages of KNO3 in the composite films has been indexed in
Table I.
IV. Conclusions
The spray-deposited KNO3:PVA composite films con-
taining equal proportions of KNO3 and PVA show maxi-
1632 IEEE Transactions on Ultrasonics, Ferroelectrics, and Frequency Control ,
mum Pr and current density at room temperature as evi-
dent from P-E studies of the composite films. The XRD
studies on these composite films reveal more intense fer-
roelectric phase III peak relative to phase II peak. The
FE-SEM image of 50  wt.% KNO3:PVA composite film
shows that the KNO3 particles are uniformly dispersed in
the PVA matrix. The occurrence of butterfly features in
J-E and the C-V characteristics confirm the existence of
ferroelectric phase III in KNO3:PVA composite films at
room temperature.
Acknowledgments
The authors acknowledge the chairman of Baba Far-
id College of Engineering and Technology, Bathinda, for
providing the research facilities for this work. The help
and guidance provided by the director of the Sophisti-
cated Analytical Instrumentation Facility (SAIF), Panjab
University, Chandigarh, for extending the facility for the
X-ray scans is also greatly acknowledged.
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Navneet Dabra was born in Gidderbaha (Pun-
jab), India on May 26, 1979. He received his B.Sc.
degree from D.A.V. College, Malout, India, and
M.Sc. degree in applied physics from the Depart-
ment of Physics, Punjabi University, Patiala, In-
dia, in 1998 and 2002, respectively. He has started
his research career in the area of thin-film ferro-
electric polymer composite materials in 2005 and
registered as a Ph.D. student with Punjab Techni-
cal University, Jalandhar, India.
Currently, Mr. Dabra is working as lecturer
in physics in the Department of Applied Sciences, Baba Farid College
of Engineering and Technology, Bathinda, Punjab State, India. He has
published 7 scientific papers in various international journals and for
international conferences and written 1 book. His research interest lies
in thin-film ferroelectric composite materials and devices. Presently, he
is engaged to develop the ferroelectric nanocomposites memory devices
and multiferroics/composites for industrial applications.
1633
Jasbir S. Hundal was born in Faridkot, Punjab,
India, on December 12, 1963. He received the
M.Sc. and M. Phil degrees in physics from the
Department of Physics, Guru Nanak Dev Univer-
sity, Amritsar, Punjab, India, in 1984 and 1986,
respectively. While working toward his M.Phil. de-
gree, he carried out research on metallic glasses.
He received his Ph.D. degree for his dissertation
entitled “Study of Piezoelectricity and Stored Po-
larization in Some Corona Charged Cyano Poly-
mers” from the Department of Physics, Indian
Institute of Technology, Roorkee, (formerly University of Roorkee) in
1998. He carried out research work in the Materials Research Institute
on actuators, transducers, and relaxor ferroelectric polymers as a post-
doctoral research scholar at the Pennsylvania State University, Univer-
sity Park, PA, from February 2001 to July 2001. He has about 20 years
of teaching and research experience and taught engineering physics, ma-
terials science and engineering, and an overview of information technol-
ogy materials from 1989 to 2008 at Giani Zail Singh College of Engineer-
ing and Technology, Bathinda, Punjab State, India. He is Founder
Director-Principal, Baba Farid College of Engineering and Technology,
Bathinda. Presently, he is involved in the development of innovative fer-
roelectric nanomaterials and miltiferriocs for device applications. He is
author and co-author of about 20 research papers that have been pub-
lished in various international journals and presented at international
conferences.
K. C. Sekhar was born in Markapur, Andhra
Pradesh, India on June 5, 1980. He received his
M.Sc. degree in physics from Nagarjuna Universi-
ty Campus, Gunter, India, in 2003. He taught
physics at the national degree college in Palvon-
cha, India, from May 2003 to April 2004 and at
A.K.R.G. College, Nallajerla, India, from June
2004 to June 2005. He has been doing his doctoral
research work in the Department of Physics at the
Indian Institute of Technology, Roorkee, India,
since July 2005. His research interests are ferro-
electric composite thin films and multiferroics. He has published 9 papers
on ferroelectric and switching properties of composite films and pre-
sented 11 papers at international and national conferences.
Arvind Nautiyal was born in Tehri Garhwal,
Uttarakhand, India, on April 1, 1983. He received
his M.Sc. degree in physics from Sri Guru Ram
Rai (P.G.) College, Dehradun, Garhwal University
(Srinagar), Uttarakhand, India, in 2004. He has
been doing his doctoral research work in the De-
partment of Physics at the Indian Institute of
Technology, Roorkee, India, since July 2006. His
research interests are ferroelectric-polymer com-
posite thin films and their application in micro-
wave tunable devices.
Rabinder Nath was born in Patiala, Punjab,
India on November 10, 1951. He received the
Ph.D. degree from the Indian Institute of Technol-
ogy, Delhi, India, in 1978. He carried out research
work in the Dept. of Physics at College Militaire
Royal De Saint-Jean Quebec, Canada, on charge
storage and ferroelectric polymers from 1986 to
1989. He is currently professor of physics in the
Department of Physics at the Indian Institute of
Technology Roorkee (formerly University of Roor-
kee). He has developed the Ferroelectric Materials
and Devices Research Laboratory and teaches the courses on nanotech-
nology and nanodevices, solid-state electronic materials. He has worked
since 1978 in the research areas of piezo, pyro, and ferroelectric and
charge storage devices. He is currently involved in the area of ferroelec-
tric memory devices and innovative ferroelectric materials for device
applications. He is author and co-author of about 60 scientific papers
and has guided 6 Ph.D. theses.