Physica B 497 (2016) 59–66

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Physica B
journal homepage: www.elsevier.com/locate/physb

Synthesis and characterizations of NaNbO3 modified BNT–BT–BKT

ceramics for energy storage applications
M. Chandrasekhar, Sonia, P. Kumar n
Department of Physics, National Institute of Technology, Rourkela, Odisha 769008, India

art ic l e i nf o a b s t r a c t

Article history: Lead-free (1
x)[0.884BNT–0.036BT–0.08BKT]–xNaNbO3 samples (with x ¼0, 0.04, 0.08, 0.12 and 0.16)
Received 31 March 2016 were synthesized in single perovskite phase by solid state reaction route. Decrease of grain size with the
Received in revised form increase of NaNbO3/NN content was related to the grain boundary pinning effect. Dielectric study con-
14 June 2016
firmed the relaxor nature of x ¼ 0.08, 0.12 and 0.16 samples. Energy storage density and efficiency were
Accepted 15 June 2016
Available online 16 June 2016
calculated from polarization vs. electric field hysteresis loops. Value of energy storage efficiency in-
creased with the increase of NaNbO3 content. A relatively large energy storage density of  0.721 J/cm3
Keywords: was obtained in the x ¼0.08 samples. Electric field induced polarization and strain loops, respectively
Grain boundary pinning effect suggested the increase of AFE ordering with the increase of NN content.
Energy storage density
& 2016 Elsevier B.V. All rights reserved.
Relaxor
Non-polar phase

1. Introduction where, E is the applied electric field and P is the polarization.

High energy storage density functional materials are used in
compact devices like electrical vehicles, mobile electronics and
different types of pulsed power technologies [1]. Recently,
Bi0.5Na0.5TiO3 (BNT)-based ferroelectric (FE) functional materials
have drawn attention of research community for their promising
use in energy storage applications. In comparison to conventional
dielectrics, antiferroelectric (AFE) materials have small remnant
polarization (Pr) and large charge–discharge speed, and are pre-
ferred in energy storage applications [2,3]. Better energy storage
density and efficiency of BNT system appear near depolarization
temperature (Td) [4]. On the other hand, though FE materials with
square shaped Polarization–Electric field (P–E) hysteresis loops
have high energy storage density than those of the double like P–E
hysteresis loops of the AFE materials, yet they cannot withstand
the large number of charge–discharge cycles [2]. Therefore, double
smaller area P–E hysteresis loops are desirable for achieving large
number of charge–discharge cycles [5,6] in the energy storage
device applications. Energy storage density (W1) of a FE material is
given by the following equation [7]
Pmax
W1 = ∫ EdP…. .
0 (A.1)
n In the present work, dielectric, energy-storage density and ef-
Corresponding author.
E-mail addresses: chanduphy2004@gmail.com (M. Chandrasekhar),
pvn772004@yahoo.co.in (P. Kumar).
According to above equation, materials having large saturated
polarization (Ps), smaller remnant polarization (Pr) and moderate
breakdown field, are suitable for having high energy storage
density. On the other hand, energy storage efficiency (η) of a
functional material is calculated by using the following equation
[7]:
η = W1/(W1 + W2)…. . (A.2)
where, W1 is the stored energy density; W2 is the energy loss
density and calculated by the numerical integration of closed area
of the P–E curves of the hysteresis loops.
Sodium niobate NaNbO3/NN, strontium titanate SrTiO3/ST are
some of the prominent lead-free AFE systems [8]. Chia-Ching Wu
and Cheng-Fu Yang [9] studied the effects of NN modification on
the dielectric properties and relaxor nature of lead-free BNT
ceramics. Wang et al. [10] studied the temperature dependent
electrical properties of BNT–BKT–SrTiO3 piezoceramics. In the lit-
erature, NaNbO3 and BNT–BT–BKT are reported as the promising
lead free AFE and FE systems respectively [11,12]. Para electric
phase transition temperature of NN system lies well below room
temperature (RT). Therefore, modification of effective BNT–BT–BKT
piezoelectric system with NN AFE system will not only lower down
the Td temperature but also increase the energy storage density
and energy storage efficiency.
ficiency properties of NaNbO3 modified BNT–BT–BKT system are
studied and discussed in detail.

http://dx.doi.org/10.1016/j.physb.2016.06.015
0921-4526/& 2016 Elsevier B.V. All rights reserved.
60 M. Chandrasekhar et al. / Physica B 497 (2016) 59–66

Fig. 1. XRD patterns of the samples.

sintered stages were confirmed by X-ray diffraction (XRD) (Rigaku

Table 1
Ultima IV, Tokyo, Japan) technique. Micrographs of the sintered
Phase fractions and lattice parameters of the (1
x)[BNT–BT–BKT]
xNN samples.
pellets were taken using Field emission scanning electron micro-
Sample x¼0 x¼ 0.04 x¼ 0.08 x¼ 0.12 x ¼0.16 scope (FESEM NOVA nano SEM). Silver paste was applied on the
polished surfaces of the sintered pellets and then fired at 400 °C for
R.P phase 31 33.4 30.7 31.2 34.2
30 min for good adhesion. Dielectric constant (εr) and dielectric
fraction
Lattice para- (3.8925 Å, (3.8926 Å, (3.8908 Å, (3.8917 Å, (3.8875 Å,
loss (tan) were measured as a function of temperature using a
meters 89.910°) 89.860°) 89.870°) 89.860°) 89.740°) computer interfaced HIOKI 3532-50 LCR-HITESTER. RT Polariza-
(aR, α) tions vs. electric field (P–E) hysteresis loops were measured using
T.P phase 69 66.6 69.3 68.8 65.8 Radiant precision premier II unit (P-HVI210k, Radiant Technologies
fraction
INC. U.S.A). RT bipolar strain vs. electric field (S–E) hysteresis loops
Lattice para- (5.7063, (5.7032, (5.6992, (5.7024, (5.7004,
meters 13.4893) Å 13.4820) Å 13.5033) Å 13.4974) Å 13.5016) Å were measured using Radiant precision premier II attached with
(aT, cT) MTI-2100 Fotonic sensor (MTI Instruments INC, U.S.A).

3. Results and discussion

2. Material and methods
Solid-state reaction route was used to synthesize the selected
materials. Firstly, the 0.884Bi0.5Na0.5TiO3–0.036BaTiO3–
0.08BiKTiO3/BNT–BT–BKT (abbreviated as x¼ 0) ceramics were
prepared by taking stoichiometric weights of Bi2O3, Na2CO3, TiO2,
BaCO3 and K2CO3 (all are 99.9% purity) as the starting precursors.
The mixture of these starting precursors was ball milled for 20 h
(h) by using zirconia balls and acetone as the grinding media. The
dried ball milled powder was calcined at 900 °C and sintered at
1050 °C for 4 h. NN was synthesized by taking stoichiometric
weights of Na2CO3 and Nb2O5 precursors, ball milled under the
same conditions mentioned above and calcined at 800 °C for 4 h.
Finally, the (1
x)[BNT–BT–BKT]–xNN ceramics with x¼0.04, 0.08,
0.12 and 0.16 were synthesized by taking stoichiometric weights of
the calcined BNT–BT–BKT and NN powders. 3 wt% polyvinyl alcohol
binder solution was added to the calcined powders. Green pellets
of  10 mm in diameter and  1.5 mm in thickness were com-
pacted using a uniaxial hydraulic press with 10 MPa pressure.
Optimized sintering temperature for x¼0 i.e BNT–BT–BKT samples
was 1050 °C/4 h and for NN modified BNT–BT–BKT samples it was
1100 °C/4 h. Perovskite phase formation during calcination and
3.1. XRD and microstructure study
Fig. 1(a) shows the XRD patterns of samples, which confirmed
the retention of single perovskite phase [13,14] nature except
x¼ 0.04 samples. Secondary phase in x ¼0.04 sample is caused by
reaction between sodium, titanium and oxygen ions (JCPDS no:
31-1329, 80-1282). In the x ¼0 i.e BNT–BT–BKT samples, sintered
at 1100 °C, there develops secondary phase. The content of sec-
ondary phase of x ¼0.04 samples is less than that of x ¼0 samples,
sintered at 1100 °C. It is further observed that XRD peak intensities
of secondary phase diminish for x 40.04 samples. Therefore, NN
addition enhances the sintering temperature and inhibits the
secondary phase formation in the NN modified BNT–BT–BKT
samples, sintered at 1100 °C. Deconvolution of XRD peak at
2θ  46° of the all (1
x)[BNT–BT–BKT]–xNN samples, shown in
Fig. 1(b), consists of two tetragonal, (200) and (002), and one
rhombohedral (200) peak. Based on integral intensities (I), tetra-
gonal phase (T.P) and rhombohedral phase (R.P) fractions are
calculated using the following relations [15]:
{
T.P.= I( 200) + I( 002)
T T
} / { I( 200)
T
+ I( 002) + I( 200)
T
}…. .
R (A.3)
 M. Chandrasekhar et al. / Physica B 497 (2016) 59–66 61

Fig. 2. FESEM micrographs of the samples.

Lattice parameters along with phase fractions of rhombohedral

Table 2
Dielectric and ferroelectric properties of the samples.
and tetragonal structures are listed in the (Table 1). Both the
phases exist in all the samples, which confirm the morphotrophic
Sample Grain εr (RT) εm at Td (°C) Tc (°C) Ec Pr Ps (μC/ phase boundary (MPB) nature of these samples.
size at 1 kHz at at (kV/ (μC/ cm2)
Fig. 2 shows the microstructure of the (1
x)[BNT–BT–BKT]

(μm) 1 kHz 1 kHz 1 kHz cm) cm2)
xNN samples. Average grain size, calculated using linear intercept
x¼0 1.4 1375 3360 70 299 22 22 36.8 method, is given in (Table 2). It is observed that with the mod-
x ¼ 0.04 0.47 1529 3220 112 306 11.6 7 30.69 ification of NN phase, grain size of (1
x)[BNT–BT–BKT]
xNN
x ¼ 0.08 0.70 1583 3488 110 260 8.1 4.1 30.66
x ¼ 0.12 0.69 1618 3050 107 255 7.8 3.5 25.80 samples decreases, which may be attributed to the pinning effect
x ¼ 0.16 0.71 1445 2799 106 245 7.3 2.9 22.78 of defect dipoles. Sung et al. [16,17] reported that in oxide per-
ovskites, sintered at high temperatures, defect dipoles, denoted
below, are generated
R.P=1−T.P = { I( ) } / { I(
200
R
200)
T T R
}
+ I( 002) + I( 200) …. ..
(A.4) ′ − VO•• − VNa
VNa ′ …. (A.5)
62 M. Chandrasekhar et al. / Physica B 497 (2016) 59–66
Fig. 3. Temperature dependence of dielectric constant and loss of the samples.
Where, VNa ′ is sodium-ion and VO•• is oxygen-ion vacancies (Kro-
ger–Vink notation). Generation of defect dipoles in these samples
can cause grain boundary pinning effect, which can account the
development of smaller grains [16,17]. In x ¼0.04 samples, grain
size decreases drastically, which may attributed to combined
effect of presence of secondary phase and the grain boundary
pinning effect. Higher average grain size, which is almost con-
stant, is observed in x ¼0.08, 0.12 and 0.16 samples compared to
x ¼0.04 samples. In x 4 0.04 samples, due to the absence of sec-
ondary phase, the grain size is higher than the x ¼ 0.04 samples.
Generally, in Na based perovskite oxides, liquid phase sintering is
prominent, which favors grain growth [18]. Therefore, increased
grain size of x ¼0.08, 0.12 and 0.16 samples, compared to x ¼ 0.04
samples, can be the effect of liquid phase sintering in these
samples.
3.2. Dielectric study
Fig. 3 shows the temperature (T) dependence of εr and tan δ ,
measured at different frequencies of the samples. Decrease of εr
with the increase of frequency can be related with the decrease of
net polarization [19]. Whereas, increase of εr with the increase of
temperature can be related with the increase of dipole orientation.
Value of εr increases up to a particular temperature called max-
imum dielectric constant temperature (Tm), and beyond it de-
creases with the further increase of temperature. Dielectric spectra
show two anomalies; one near Td and other near Tm [20]. In
x¼ 0.08, 0.12 and 0.16 samples, diffused phase transition and shift
of Tm to higher temperature side with the increase of frequency is
observed, which confirms the relaxor nature of these samples.
Relaxor behavior in complex perovskite FE materials is accounted
in terms of generation of cation-ordered clusters [21]. Therefore,
relaxor nature of x¼ 0.08, 0.12 and 0.16 samples suggests the onset
of generation of cation-ordered clusters in xZ0.08 samples. Value
of tan δ at different frequencies of all the NN modified samples is
nearly constant up to Td. At a particular frequency, tanδ is constant
up to Td. Occurrence of tanδ peaks at higher temperatures suggests
the presence of oxygen vacancies in the samples [22,23]. The tan δ
(at low frequency) at high temperatures drastically increases for
x¼ 0.12 samples, which may be attributed to increase of electrical
conductivity due to the increase of space charge effect [24]. The
 M. Chandrasekhar et al. / Physica B 497 (2016) 59–66 63

Fig. 4. ln (1/εr
1/εm) vs. ln (T
Tm) plots of the samples.

dielectric parameters at 1 kHz frequency of the samples are given
in (Table 2). Temperature zone from Td to Tm gradually decreases
with the increase of NN content, which suggests the increased
antiferroelectric ordering at RT [25,26]. Tm deceases with the in-
crease of NN content, which can be related to the stabilization of
tetragonal phase [27].
Diffuseness of the samples was studied using the modified
Curie–Weiss law, given as:
γ
(1/εr –1/εm)=( T − Tm) /C…. . (A.6)
where, γ and C are constants and value of γ lies between 1 and
2 and gives information about the characteristic of the phase
transition. γ ¼1 for normal ferroelectrics and γ ¼ 2 for ideal relaxor
ferroelectrics [8]. Fig. 4 shows the ln (1/εr
1/εm) vs. ln (T
Tm)
64 M. Chandrasekhar et al. / Physica B 497 (2016) 59–66
Fig. 5. P–E hysteresis loops of the samples.
Fig.6. Variation of Pr and Ps with NN content of the samples.
Fig. 7. Energy storage density and energy storage efficiency of the samples.
plots of the samples. In these plots, slope of linearly fitted curves
give γ factor. γ values are found to be  1.69, 1.79, 1.91, 1.75 and
1.84 for the x ¼0, 0.04, 0.08, 0.12 and 0.16 samples, respectively,
which confirm the diffusive nature of phase transition.
3.3. P–E hysteresis loop and Energy storage study
Fig. 5 shows the P–E hysteresis loops of the samples. P–E hys-
teresis loop study suggest the dominant AFE nature of all the
compositions (except x¼ 0). Coercive field (Ec), Pr and Ps values of
the samples are given in (Table 2). Fig. 6 shows the variation of Pr
and Ps with the variation of NN content. Decrease of Ec and Pr
values with the increase of NN content suggest the decrease of FE
nature of these sample. Appreciable decrement in Pr value is ob-
served for x Z0.08 samples, whereas, very little compositional
influence was observed on Ps value. This indicates that the FE order
is perturbed by NN and the free energy of the ferroelectric phase
appears competitive enough with that of the “non-polar” phase,
which leads to ergodic relaxor state [28]. Therefore, for x¼ 0.08,
0.121 and 0.16 ceramic samples can exhibit relaxor behavior, which
also was confirmed from dielectric study. With the increase of NN
content, Ec value decreases, which further suggest the decrease of
FE ordering and increase of AFE ordering at RT [29].
Fig. 7 shows the stored energy density (W1) and energy storage
efficiency (η%) as a function of NN content in the samples. Due to
decrease of Pr and retention of same Ps, W1 increases up to x ¼0.08
samples. In x 40.08 samples, W1 decreases due to the large de-
crease of Ps than the Pr values. Initially, value of η% increases up to
x¼ 0.08, which can be related to drastic decrease of Pr values.
Beyond x ¼0.08, increment in η% is small, which can be related
with reduction of polar phase (confirmed by P–E hysteresis loop
study) [27]. To the best of our knowledge, the sample with x ¼0.08
shows the maximum energy storage density 0.721 J/cm3, which
is larger than the earlier reported 0.37 J/cm3 at 120 kV/mm of
Ba0.4Sr0.6TiO3 [30],  0.598 J/cm3 at 52 kV/cm of 0.93BNT–
0.06BT3–0.01KNN [20] and 0.4 J/cm3 at 90 kV/mm of BaTiO3–
glass composites [31], and many other lead based systems
[5,32,33]. Therefore, x ¼0.08 samples are suitable for energy sto-
rage applications.
3.4. S–E hysteresis loop study
Fig. 8 shows the RT S–E hysteresis loops of the samples. The
sample x ¼0 shows butterfly shaped S–E loop, which suggests its
piezoelectric nature. Non butterfly shape of S–E loops of all the NN
modified samples suggests their non-piezoelectric nature. This
non-piezoelectric nature in these samples can be associated with
the AFE nature of NN phase [18]. Asymmetry in S–E loops in the
NN modified samples can be attributed to the back switching of
domains during bipolar cycles of the applied external electric field
[34]. Maximum electric field induced strain of  0.63, 0.1, 0.13,
0.07 and 0.08 % were observed in x ¼0, 0.04, 0.08, 0.12 and 0.16
samples, respectively. Drastic decrease of maximum strain% for the
x¼ 0.04 samples can be associated with grain boundary pinning
effect, which reduces the switching and movement of domain
walls [35–37].
4. Conclusions
Except x¼ 0.04 sample, XRD patterns of the samples show the
retention of single perovskite phase nature. Increase of grain
boundary pinning and liquid phase sintering effects were ac-
counted for the variation of grain size with the increase of NN
content of the samples. Dielectric study confirmed the relaxor
behavior of x ¼0.08, 0.12 and 0.16 samples. Highest value of energy
storage density suggested the suitability of x ¼0.08 samples for
energy storage applications. P–E and S–E hysteresis loop study
confirmed the reduction of FE, piezoelectric and increase of AFE
phase nature with the increase of NN content.
 M. Chandrasekhar et al. / Physica B 497 (2016) 59–66
Fig. 8. S–E loops of the samples.
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