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IEEE Transactions on Ultrasonics, Ferroelectrics, and Frequency Control , vol. 56, no.

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- mer. The embedded ferroelectric ceramic particles in long
trate (KNO3):poly(vinyl alcohol) (PVA) with different weight chain molecules of the polymers make these films very
percentages of KNO3 have been prepared at 200°C using the
spray-deposition technique. The remanent polarization (Pr)
flexible and viscoelastic, thus increasing the possibility
and peak current density for all composite films was estimated of making large area devices because these films possess
by tracing the polarization-electric field (P-E) hysteresis loop large dielectric relaxation [2]. The proper combination of
and current density-electric field (J-E) loop, respectively, us- the ceramic and polymer with definite weight percent-
ing a modified Sawyer-Tower circuit. Pure KNO3 is known not age ratio allows the fabrication of the new materials with
to exhibit any ferroelectricity under ambient conditions, but
the X-ray diffraction (XRD) studies of PVA:KNO3 composite
desired ferroelectric properties such as low coercive field,
films reveal the presence of a ferroelectric phase III of KNO3 because the presence of the polymer is known to modify
in the composite films at room temperature. The composite the local electric field distribution inside the composite [2].
film containing KNO3:PVA in equal proportions shows maxi- These films also possess good electromechanical proper-
mum Pr and peak intensity ratio of approximately 20.10 μC/ ties, flexibility, and reasonable mechanical strength [1]–[3].
cm2 and 2.67, respectively, at room temperature. The J-E and
capacitance voltage (C-V) characteristics exhibit butterfly fea-
The ferroelectric ceramic-polymer composites have a great
tures that supports the presence of a ferroelectric phase in the potential for applications in the field of microelectronics,
composite films. The field emission scanning electron micros- microelectromechanical systems (MEMS) [7], memory de-
copy (FE-SEM) image of the composite film containing equal vices such as ferroelectric random access memories (Fe-
proportions of KNO3 and PVA shows the homogenous distri- RAMs), nonvolatile random access memories (NVRAMs),
bution of spherical grains of KNO3 of size ~225 nm.
ferroelectric field effect transistors (FeFET), and organic
ferroelectric field effect transistors (OFeFET) [8], [9]. The
remanent polarization and phase stability were found to
I. Introduction
have been improved in ceramic-polymer composite sys-
tems such as sodium nitrite (NaNO2):polyvinyl alcohol
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-
(PVA) [10], KNO3:poly(vinylidene fluoride) (PVDF) [11],
[12], KNO3:polyvinyl fluoride (PVF) [13], triglycine sulfate
(TGS):PVA [14], [15], barium titanate (BiTiO3):PVDF
ducer applications [1]–[3]. Ferroelectric materials possess
[16], and lead zirconate (PZT):polyurethane (PU) [17].
spontaneous polarization even at zero electric field, and
Usually, the ceramic-polymer composites have been
their polarization can be switched under the influence
prepared by the inclusion of polymer matrix in ceramic
of the external electric field [4]. The pure potassium ni-
materials by melt press [2], [11]–[13], sol-gel [2], [18]–[20],
trate (KNO3) crystals exist in phase II with orthorhom-
solvent cast [21], [22], and intercalation techniques [23],
bic (aragonite) crystal structure at room temperature and
[24]. However, under suitable conditions, composite films
atmospheric pressure. It changes to phase I (rhombohe-
obtained from the solvent cast and sol-gel process allows
dral crystal structure) above 130°C. On cooling, phase I
for the better control of the chemical composition of ce-
of KNO3 does not directly revert back to phase II but
ramic and polymer due to proper molecular interactions.
through an intermediate metastable phase III, which is
The composite films obtained by these methods yield ce-
ferroelectric in region ~124 to 110°C. On further cooling,
ramic-polymer with better electroactive and ferroelectric
it changes to phase II [5], [6]. The ferroelectric ceramic-
properties [2]. It has been reported that the preparation
polymer composites have attracted a great deal of atten-
of the composite films of NaNO2, selenide with PVA us-
tion as they combine the ferroelectricity of the ceramic
ing solvent cast technique was helpful in controlling the
material with the good mechanical properties of the poly-
growth of NaNO2, and selenide nanoparticles [10], [22].
Many studies using techniques such as far infrared [25],
Manuscript received November 14, 2008; accepted May 2, 2009. neutron diffraction [26], inelastic neutron scattering [27],
N. Dabra and J. S. Hundal are with the Applied Physics and Materials Raman spectroscopy [28], [29], X-ray [30]–[32], differen-
Science Laboratory, Department of Applied Sciences, Baba Farid College
of Engineering and Technology, Punjab, India (e-mail: navneetdabra@ tial scanning calorimetric [33]–[35], dielectric [36], electri- and cal and thermal conductivity [36], [37], and ferroelectric
K. C. Sekhar, A. Nautiyal, and R. Nath are with the Ferroelectric Ma- [38]–[41], have been carried out in the past by various
terials and Devices Research Laboratory, Department of Physics, Indian
Institute of Technology, Roorkee, Uttarakhand, India. researchers to examine the nature of the phase transitions
Digital Object Identifier 10.1109/TUFFC.2009.1227 in KNO3. The technological interest in KNO3 thin films

0885–3010/$25.00 © 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 1629

Fig. 3. Variation of (a) peak intensity ratio and (b) average grain size
Fig. 2. X-ray scan of (a) pure poly(vinyl alcohol) and composite films with wt.% of KNO3 in composite films.
containing (b) 20, (c) 40, (d) 50, (e) 70  wt.% of KNO3, and (f) pure
KNO3 powder.

show the uniform distribution of KNO3 in PVA matrix

and grain size of ~225  nm. Earlier studies using atomic
XRD pattern for pure KNO3 and were found to be 6.552, force microscopy (AFM) technique also revealed grain size
5.472, and 9.028 Å, respectively. These values are in good of similar order in these films having this composition [52].
agreement with the values previously reported in the lit- However, the clustering of the KNO3 particles has been
erature [51]. PVA film has amorphous nature and exhibits observed in the composite films above 50 wt.% composi-
a broader diffraction peak around 2θ~20.0° corresponding tion of KNO3. The clustering creates porosity that might
to (101) [24], whereas the brass (substrate) peaks occurred be responsible for the decrease of Pr above the 50 wt.%
at 2θ = 31.44 o and 36.41°. composition [10].
The composite films exhibit the ferroelectric phase III
peak at 2θ = 29.71° corresponding to (003) reflection and B. Electrical Properties
another peak at 2θ  =  29.52° for (012) reflection for the
phase II in addition to the peak around 2θ = 19.6° that 1) Hysteresis Loop and Current Density-Electric Field
corresponds to PVA. However, the XRD pattern of the (J-E) Characteristics: The ferroelectric hysteresis loops
pure KNO3 powder exhibits a phase II peak at 2θ = 29.4° (P-E) of the composite films with varying compositions
and no peak corresponding to the phase III. The earlier of KNO3:PVA were recorded at room temperature using
X-ray studies by other workers also suggest the existence a 50 Hz sine wave signal. Fig. 5 shows the P-E loops ob-
of ferroelectric peak around 2θ = 29.8° in addition to peak served for the 20, 40, 50, and 70  wt.% of KNO3 com-
corresponding to phase II around 2θ  =  29.5° in mixed posite films, respectively, prepared at optimized tempera-
KNO3 systems. The composites films of the KNO3:PVDF ture. The value of Pr increases up to 50  wt.% of KNO3
were also known to exhibit enhanced phase III peak at in the composite films and beyond this, the Pr shows a
2θ = 29.8° [12]. Therefore, the present X-ray studies sug- decreasing trend. The value of Pr was estimated in each
gest that ferroelectric phase III has developed in the composite film and the optimum value was found to be
KNO3:PVA composite films. ~20.10 μC/cm2 for the composite film with equal propor-
The variation of the ratio of peak intensity of the phase tions of KNO3 and PVA as shown in Fig. 5(a). A similar
III to peak intensity of the phase II as a function of vary- pattern in the variation of Pr has been reported in the
ing wt.% of KNO3 in the composite films is depicted in KNO3:PVDF and NaNO2:PVA composite films [10], [12].
Fig. 3(a). The relative intensity of phase III to phase II It was found that the Pr remains independent of the elec-
was estimated and found to be a maximum of 2.67 for the trode area. The coercive field (Ec) decreases with increase
composite films with 50 wt.% of KNO3. of the KNO3 content in the composite films. Fig. 5(a)
Field emission scanning electron microscopy (FE-SEM) shows dependence of Ec on the wt.% of KNO3 in the com-
has been employed to obtain the grain size and distri- posite films. The composite films with more than 50 wt.%
bution of KNO3 in the PVA matrix. Fig. 4 shows the KNO3 content were found to be more brittle. In view of
FE-SEM images of the composite films of varying wt.% this observation, the composite films with 50:50 wt.% of
of KNO3. The images of the composites exhibit spherical KNO3 and PVA were chosen for further ferroelectric stud-
grains of KNO3 with an average size in the range of 195 ies. The value of the Pr ~20.10 μC/cm2 in these spray-de-
to 310 nm with increasing composition; see Fig. 3(b). The posited films is more than 4 times as reported in the poled
image of the composite film containing 50 wt.% of KNO3 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

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 2) Capacitance Voltage (C-V) Characteristics: Fig. 6
KNO3 films [40]. This value of Pr is slightly greater than depicts the C-V characteristics of the composite films of
that reported for KNO3:PVDF composite films prepared varying compositions taken at frequency ~100 KHz. The
by hot press method [12] and approximately half that of applied voltage was varied between from −15 V to +15 V
the fused KNO3:PVDF [11]. with step bias of 1 V and vice versa for forward and re-
The current density-electric field (J-E) studies carried versed cycles. Two sharp peaks were observed in the C-V
out on these composite films depict the butterfly behavior characteristics of all the composite films. The Cmax was
(figure not shown) in each composition with maximum highest in the films containing equal proportions of KNO3
current density ~37 mAcm−2 for the composite film con- and PVA as shown in Fig. 6 (inset). The orientations of
taining equal proportions of KNO3 and PVA as shown. domains along the field direction are responsible for in-
Fig. 5(b) shows the variation of current density (J) with crease in the capacitance during voltage variation. The
the wt.% of KNO3 in the composite films. 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- ages of KNO3 in the composite films has been indexed in
tion of new domain close to Vc could be responsible for Table I.
occurrence of peaks in C-V spectra [10], [54]. The nonlin-
ear behavior (butterfly) observed in C-V spectra strongly IV. Conclusions
indicates the presence of ferroelectricity in the composite
films [10], [12], [13]. The variation of Pr, Ec, J, intensity The spray-deposited KNO3:PVA composite films con-
ratio, grain size, and Cmax with different weight percent- taining equal proportions of KNO3 and PVA show maxi-
1632 IEEE Transactions on Ultrasonics, Ferroelectrics, and Frequency Control , vol. 56, no. 8, August 2009

mum Pr and current density at room temperature as evi- [15] S. A. Khairy and S. S. Ibrahim, “Comments on the temperature-
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[42] J. F. Scott, Ferroelectric Memories. Berlin: Springer-Verlag, 2000. respectively. While working toward his M.Phil. de-
[43] A. K. Kulkari, G. A. Roher, L. D. Mcmillian, and S. E. Adams, gree, he carried out research on metallic glasses.
“Dependence of the electrical properties of KNO3 memory devices He received his Ph.D. degree for his dissertation
on fabrication and processing parameters,” J. Vac. Sci. Technol. A, entitled “Study of Piezoelectricity and Stored Po-
vol. 7, no. 3, pp. 1461–1466, 1988. larization in Some Corona Charged Cyano Poly-
[44] A. M. E. Raj, L. C. Nehru, M. Jayachandran, and C. Sanjeeviraja, mers” from the Department of Physics, Indian
“Spray pyrolysis deposition and characterization of highly (100) ori- Institute of Technology, Roorkee, (formerly University of Roorkee) in
ented magnesium oxide thin films,” Cryst. Res. Technol., vol. 42, no. 1998. He carried out research work in the Materials Research Institute
9, pp. 867–875, 2007. on actuators, transducers, and relaxor ferroelectric polymers as a post-
[45] P. Pushparajah, A. Kariem Arof, and S. Radhakrishna, “Physical doctoral research scholar at the Pennsylvania State University, Univer-
properties of spray pyrolysed pure and doped ZnO thin films,” J. sity Park, PA, from February 2001 to July 2001. He has about 20 years
Phys. D Appl. Phys., vol. 27, pp. 1518–1521, 1994. of teaching and research experience and taught engineering physics, ma-
[46] P. Murugave, R. Sharma, A. R. Raju, and C. N. R. Rao, “A study terials science and engineering, and an overview of information technol-
of ferroelectric thin films deposited on a LaNiO3 barrier electrode ogy materials from 1989 to 2008 at Giani Zail Singh College of Engineer-
by nebulized spray pyrolysis,” J. Phys. D Appl. Phys., vol. 33, pp. ing and Technology, Bathinda, Punjab State, India. He is Founder
906–911, 2000. Director-Principal, Baba Farid College of Engineering and Technology,
[47] K.C. Sekhar and A. Nautiyal, andR. Nath, “Structural and fer- Bathinda. Presently, he is involved in the development of innovative fer-
roelectric properties of spray deposited sodium nitrite: Poly(vinyl roelectric nanomaterials and miltiferriocs for device applications. He is
alcohol) composite films,” J. Appl. Phys., vol. 105, art. no. 024109, author and co-author of about 20 research papers that have been pub-
2009. lished in various international journals and presented at international
[48] Y. Ye, Y. Jiang, T. Wang, Z. Wu, and H. Zeng, “Ferroelectric poly- conferences.
meric PVDF films prepared ultrasonic atomization method,” J.
Mater. Sci. Mater. Electron., vol. 17, pp. 631–635, 2006.
[49] F. M. Herman, Encyclopedia of Polymer Science and Technology, 3rd K. C. Sekhar was born in Markapur, Andhra
ed. New York: Wiley, 2003, vol. 8, p. 401. Pradesh, India on June 5, 1980. He received his
[50] D. B. Fraser and J. R. Maldonado, “Improved aging and switching M.Sc. degree in physics from Nagarjuna Universi-
of lead zironate-lead titanate ceramics with indium electrodes,” J. ty Campus, Gunter, India, in 2003. He taught
Appl. Phys., vol. 41, pp. 2172–2176, 1970. physics at the national degree college in Palvon-
[51] International Center for Diffraction Data, JCPDS files, no. 74–2055, cha, India, from May 2003 to April 2004 and at
1998. A.K.R.G. College, Nallajerla, India, from June
[52] N. Dabra,, J. S. Hundal, K. C. Sekhar, A. Nautiyal, and R. Nath, 2004 to June 2005. He has been doing his doctoral
“Ferroelectric phase stability studies in spray deposited KNO3:PVA research work in the Department of Physics at the
composite films,” J. Am. Ceram. Soc., vol. 92, pp. 834–838, 2009. Indian Institute of Technology, Roorkee, India,
[53] N. Kumar and R. Nath, “Ferroelectric properties of polyvinyl since July 2005. His research interests are ferro-
alcohol:potassium nitrate composite films,” Ferroelectrics, vol. 329, electric composite thin films and multiferroics. He has published 9 papers
pp. 85–89, 2005. on ferroelectric and switching properties of composite films and pre-
[54] G. A. C. M. Spierings, M. J. E. Ulenaers, G. L. M. Kampschoer, sented 11 papers at international and national conferences.
H. A. M. Van Hal, and P. K. Larson, “Preparation and ferroelec-
tric properties of PbZr0.53Ti0.47O3 thin films by spin coating and
metalorganic decomposition,” J. Appl. Phys., vol. 70, pp. 2290–2298,
1991. 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
Navneet Dabra was born in Gidderbaha (Pun- research interests are ferroelectric-polymer com-
jab), India on May 26, 1979. He received his B.Sc. posite thin films and their application in micro-
degree from D.A.V. College, Malout, India, and wave tunable devices.
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 Rabinder Nath was born in Patiala, Punjab,
his research career in the area of thin-film ferro- India on November 10, 1951. He received the
electric polymer composite materials in 2005 and Ph.D. degree from the Indian Institute of Technol-
registered as a Ph.D. student with Punjab Techni- ogy, Delhi, India, in 1978. He carried out research
cal University, Jalandhar, India. work in the Dept. of Physics at College Militaire
Currently, Mr. Dabra is working as lecturer Royal De Saint-Jean Quebec, Canada, on charge
in physics in the Department of Applied Sciences, Baba Farid College storage and ferroelectric polymers from 1986 to
of Engineering and Technology, Bathinda, Punjab State, India. He has 1989. He is currently professor of physics in the
published 7 scientific papers in various international journals and for Department of Physics at the Indian Institute of
international conferences and written 1 book. His research interest lies Technology Roorkee (formerly University of Roor-
in thin-film ferroelectric composite materials and devices. Presently, he kee). He has developed the Ferroelectric Materials
is engaged to develop the ferroelectric nanocomposites memory devices and Devices Research Laboratory and teaches the courses on nanotech-
and multiferroics/composites for industrial applications. 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.