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Applied Physics A (2018) 124:713
https://doi.org/10.1007/s00339-018-2126-z
A comparative study of dielectric and ferroelectric properties
of sol–gel-derived ­BaTiO3 bulk ceramics with fine and coarse grains
Gasidit Panomsuwan1
· Hathaikarn Manuspiya2
Received: 17 June 2018 / Accepted: 19 September 2018 / Published online: 24 September 2018
© Springer-Verlag GmbH Germany, part of Springer Nature 2018
Abstract
Fine and coarse-grained B
­ aTiO3 (BTO) ceramics were prepared by conventional sintering of sol–gel-derived BTO nanopowders at 1150 and 1350 °C, respectively. Based on characterization results, fine and coarse-grained BTO ceramics had
an average grain size of about 1 and 12 µm, respectively. They exhibited a tetragonal structure with tetragonality (c/a ratio)
of 1.0105. The dielectric properties of fine and coarse-grained BTO ceramics were measured in the frequency range of
100 Hz–10 MHz and temperature range of −45–180 °C. A dominant dielectric relaxation was observed at high frequency
above 1 MHz for both BTO ceramics. Room-temperature dielectric constant of fine-grained BTO (1502) was greater than
that of coarse-grained BTO (1082) at 1 kHz due to the grain size effect. For temperature dependence measurement, dielectric
constant of fine-grained BTO was less sensitive with changing temperature at phase transition than coarse-grained BTO.
Polarization–electric field (P–E) loop of coarse-grained BTO at room temperature revealed a well-defined hysteresis loop,
confirming its ferroelectric switching behavior. In contrast, a lossy hysteresis loop was found for fine-grained BTO owing to
its high leakage current. Our results in this work provide a useful information and progress in the dielectric and ferroelectric
properties of sol–gel-derived BTO bulk ceramics.
1 Introduction
Barium titanate ­(BaTiO3, BTO) ceramic, a well-known perovskite oxide material, has long been considered as one of
the most promising ferroelectric materials for several decades since the first discovery in 1941 [1, 2]. Currently, they
are practically embedded in a broad range of miniature and
integrated electronic devices, such as actuators [3], sensors
[4], micro-electromechanical systems (MEMS) [5], and nonvolatile memories [6]. To date, a significant progress has
Electronic supplementary material The online version of this
article (https​://doi.org/10.1007/s0033​9-018-2126-z) contains
supplementary material, which is available to authorized users.
* Gasidit Panomsuwan
gasidit.p@ku.ac.th
* Hathaikarn Manuspiya
hathaikarn.m@chula.ac.th
1
Department of Materials Engineering, Faculty
of Engineering, Kasetsart University, Bangkok 10900,
Thailand
2
The Petroleum and Petrochemical College, Center
of Excellence on Petrochemical and Materials Technology,
Chulalongkorn University, Bangkok 10330, Thailand
been made in optimizing and controlling dielectric and ferroelectric properties of BTO ceramics to realize the fabrication of advanced electronic devices with high performance
and reliability. In BTO ceramics, grain size plays a significant role in determining their dielectric and ferroelectric
properties [7, 8]. The dielectric constant of the BTO ceramics could reach the maximum value at grain sizes range of
0.8–1.3 µm [8–14]. A larger or smaller grain size than such
a critical range results in the reduction of dielectric constant.
The maximum dielectric constant of the BTO ceramics at an
intermediate grain size can be attributable to several factors
based on the effects of internal residual stress in each individual grain [9], 90° ferroelectric domain [11], and domain
size [12].
Despite numerous efforts toward this direction, a deeper
and wider understanding of the grain-size effects on the
dielectric and ferroelectric properties of the BTO ceramics
is now still considered to be a major research topic from both
the scientific and technological viewpoints. More importantly, the grain size in the BTO ceramics is strongly associated with several experimental factors involving the preparation of raw BTO powders and ceramics (e.g., synthesis route,
starting precursors, calcination and sintering temperatures)
13
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713 Page 2 of 8
G. Panomsuwan, H. Manuspiya
[8, 15–18]. Therefore, there are plenty of rooms remaining
for further investigation and development of BTO ceramics.
According to several earlier reports, nanocrystalline
BTO powders with narrow size distribution are greatly
required in a subsequent sintering process to obtain uniform grain size without abnormal grain growth in BTO
ceramics. Among a number of synthesis routes, the sol–gel
method has been recognized as a promising and efficient
route to prepare nanocrystalline BTO powders with narrow size distribution. It also offers several potential advantages over conventional solid-state reaction, such as higher
purity, better chemical homogeneity, ease of processing,
and controllable particle size [18, 19]. Until now, there are
a huge number of published works made by researchers to
synthesize BTO nanopowders by sol–gel method. However, the preparation and investigation on sol–gel-derived
BTO bulk ceramics have been rarely reported in literature.
A large majority of publications have only been focused
on how to control size and crystal structure of BTO nanopowders without further investigation of sintered-bulk
BTO ceramics [19–23]. Moreover, considerable attention
has also been directed toward the preparation of sol–gelderived BTO films on various kinds of substrates rather
than bulk form [24–27]. It is known that the distinct forms
of BTO (i.e., film and bulk) exhibit difference in dielectric
and ferroelectric properties. Therefore, dual measurements
of dielectric and ferroelectric properties of sol–gel-derived
BTO bulk ceramics with different grain sizes are highly
needed to promote the progress in this field.
In this work, we aim to study the dielectric and ferroelectric properties of fine and coarse-grained BTO ceramics. The BTO nanopowders were firstly synthesized by a
sol–gel method using a calcination temperature of 800 °C.
The sol–gel-derived BTO powders were subsequently sintered at 1150 and 1350 °C to produce fine and coarsegrained BTO ceramics, respectively. The morphological
and structural properties of BTO ceramics were investigated by scanning electron microscopy (SEM) and X-ray
diffraction (XRD), respectively. Moreover, comprehensive
measurements on dielectric and ferroelectric properties
of the BTO ceramics were carried out and compared with
other published works.
2 Experimental details
purity ≥ 99.9%) were purchased from RCI LabScan. All
of the chemicals were analytical grade and used without
further purification.
2.2 Synthesis of BTO nanopowders by sol–gel
method
Barium acetate was firstly dissolved in warm acetic acid
under vigorous stirring. Methanol was then added into a
clear solution with the acetic acid-to-methanol ratio of
1:2. Subsequently, an equimolar amount of titanium (IV)
butoxide was added slowly into the mixture. The solution
was kept vigorous stirring at room temperature until it
became a transparent gel. The gel was dried in a vacuum
oven at 100 °C for 12 h to obtain a dried gel. The dried
BTO gel was then calcined at 800 °C for 80 min in an
electrical furnace under air atmosphere. The calcination at
800 °C is at least temperature to obtain single-phase BTO
powders without impurity and intermediate phases (Fig.
S1). The sol–gel-derived BTO powders calcined at 800 °C
is hereafter denoted as BTO-800.
2.3 Preparation of fine and coarse‑grained BTO
ceramics
The calcined BTO powders with a binder were pressed
vertically into a pellet shape (10 mm diameter) using a
force of 10 tons for 10 min. The sintering process was
performed by placing the BTO pellets in an electrical furnace. The temperature increased from room temperature to
300 °C with a heating rate of 2 °C/min and soaked for 2 h.
Then, the temperature increased to 550 °C with a heating
rate of 2 °C/min and soaked for 5 h to completely remove
the binder. After that, the BTO pellets were sintered at
1150 and 1350 °C for 2 h with a heating rate of 4.5 °C/min
from 550 °C. After sintering, the specimens were naturally
cooled to room temperature. The sintered BTO ceramics
were then polished on sand papers (400, 800 and 1200
grit) to obtain a flat and parallel surface, followed by ultrasonically cleaning in acetone and ethanol, respectively.
The final thickness of BTO ceramics was about 1 mm. The
BTO ceramics sintered at 1150 and 1350 °C are hereafter
denoted as BTO-1150 (fine grains) and BTO-1350 (coarse
grains), respectively.
2.1 Materials
2.4 Characterizations
Barium acetate (Ba(CH3COO) 2, purity ≥ 99.999%) and
titanium (IV) butoxide (Ti(O(CH2)3CH3)4, purity ≥ 97.0%)
were purchased from Sigma Aldrich. Gracial acetic acid
­( CH 3COOH, purity ≥ 99.9%) and methanol ­(CH 3OH,
The morphology of sol–gel-derived BTO powders and
sintered BTO ceramics was investigated with a JEOL
JSM-6480LV scanning electron microscope (SEM) at an
acceleration voltage of 15 kV. The XRD patterns were
13
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A comparative study of dielectric and ferroelectric properties of sol–gel-derived B
­ aTiO3…
recorded on a Rigaku Dmax 2002 diffractrometer with
Cu Kα radiation (λ = 0.15406 nm) operated at 40 kV and
30 mA to identify the crystal and phase structure. The density of sol–gel-derived BTO powders was measured using
a Quantachrome Ultrapycnometer 1000 under helium
purge at a pressure of 20 psi.
2.5 Dielectric and ferroelectric measurements
For the preparation of specimens, gold electrodes were
deposited on both-side surfaces of the BTO ceramic pellets
by a direct current (DC) sputtering. The dielectric properties
of the BTO ceramics were measured using a Hewlett–Packard 4194A impedance/gain phase analyzer. The measurements were carried out in the frequency range of 100
Hz–10 MHz and the temperature range of − 45 to 180 °C.
The dielectric constant (εr) was calculated from the measured capacitance using the following equation:
𝜀r =
CA
,
𝜀0 d
(1)
where C is the capacitance (F), ε0 is the dielectric constant
of free space (8.85 × 10−12 F/m), A is the electrode area (­ m2),
and d is the thickness of specimen (m).
The polarization–electric field (P–E) loops of the BTO
ceramics were recorded at room temperature using a Radiant
Technology RT66A standardized ferroelectric measurement
test system with an applied voltage from ± 1000 to ± 4000 V.
3 Results and discussion
3.1 Morphology
The SEM image of sol–gel-derived BTO powders (BTO800) is displayed in Fig. 1a. The BTO-800 revealed aggregates of uniform round-shaped particles with a narrow
Page 3 of 8 713
size distribution. The average particle size of BTO-800
was determined to be 95 ± 15 nm, which is very close to
commercially available BTO nanopowders, < 100 nm
(Sigma Aldrich). For the sintered BTO ceramics, the SEM
images of BTO-1150, and BTO-1350 are illustrated in
Fig. 1b, c, respectively. An obvious increase in grain size
was clearly seen for BTO-1150 and BTO-1350. The average
grain size was estimated to be 1.0 ± 0.3 µm for BTO-1150
and substantially increased to 12.2 ± 4.6 µm for BTO-1350.
This result indicates that grain size of BTO increased with
increasing sintering temperature.
3.2 Crystal structure
To analyze the phase and crystal structure, the XRD patterns of BTO-800, BTO-1150 and BTO-1350 are shown in
Fig. 2a. For BTO-800, a set of detectable diffraction peaks
can be assigned to the BTO phase (JCDPS no. 31-0174)
without other crystalline phases. A splitting phenomenon
of the diffraction peak, especially 002/200 peaks, is typically used as the identification of ferroelectric BTO with
a tetragonal structure [13, 15, 17]. However, a symmetric
single peak without splitting feature was observed for all
diffraction peaks of BTO-800. This result suggests that the
crystal structure in BTO-800 exhibited a cubic structure,
rather than a tetragonal structure. The formation of the cubic
phase is generally found in case of nano-sized BTO particles [28, 29]. Using a helium pycnometer, the density of
BTO-800 was determined to be 5.39 g/cm3, which is about
90% of the bulk density (6.02 g/cm3), indicating the dense
nanoparticular structure.
After sintering, the evident splitting of the 002 diffraction peak into 002 and 200 peaks was clearly visible for
BTO-1150 and BTO1350, as shown in Fig. 2b. The splitting feature was also observed on the 100/001, 101/110,
102/210, 112/211, and 202/220 diffraction peaks, excepting
the 111 diffraction peak (JCDPS no. 05-0626). This result
confirms that the tetragonal structure of the BTO ceramics
Fig. 1 SEM images of a BTO-800, b BTO-1150 and c BTO-1350
13
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713 Page 4 of 8
G. Panomsuwan, H. Manuspiya
Fig. 2 a XRD patterns of BTO800, BTO-1150, and BTO1350. b Enlarged view of XRD
patterns for all samples around
111 and 002/200 diffraction
peaks
was formed well after sintering at high temperature. The
peak intensity ratio (I002/I200) of BTO-1150 and BTO-1350
was nearly close to 1:2, which is in agreement with tetragonal BTO reported in several previous reports [28, 30, 31].
In addition, the diffraction peaks of both sintered BTO
ceramics were intense and sharp, indicating their good crystallinity. The crystallite size (D) was determined using the
Scherrer’s equation based on the position (2θ) and full-width
at half maximum (β) of the 111 diffraction peak as follows:
D=
K𝜆
,
𝛽 cos 𝜃
(2)
where λ is the wavelength of X-ray (0.15406 nm) and K is
the Scherrer constant (herein 0.94).
The 111 diffraction peak was chosen for calculating crystallite size owing to its no splitting feature. The calculated
crystallite size of BTO-800, BTO-1150, and BTO-1350 was
27.5, 43.1, and 46.3 nm, respectively. This result indicates
that the crystallite size of BTO became larger after sintering;
however, only a slight change was observed between BTO1150 and BTO-1350. In association with the SEM results,
the average grain sizes of the sintered BTO ceramics were
much larger than their crystallite size calculated from the
Scherrer’s equation. This means that each individual grain
of the sintered BTO ceramics was constituted of several ferroelectric crystalline domains.
Furthermore, in-plane (a) and out-of-plane lattice constants (c) of BTO-800, BTO-1150, and BTO-1350 were
calculated using the Bragg’s law from the 200 and 002
diffraction peaks, respectively. In case of BTO-800, the calculated a and c values were both equal to 0.4010 nm owing
to its inseparable 002 diffraction peak (cubic structure) as
mentioned above. For BTO-1150 and BTO-1350, the c values were larger than a values because of their tetragonal
structure (c > a). Tetragonality (c/a ratio) of the BTO-1150
and BTO-1350 had the almost same value of about 1.0105.
The results of the lattice constant, crystallite size, and tetragonality are summarized in Table 1. Based the SEM and XRD
results, it suggests that although sintering temperature had
a significant influence in substantially increasing grain size,
only a slight change in crystallite size and tetragonality was
observed for BTO-1150 and BTO-1350.
3.3 Dielectric properties
The dielectric properties of BTO-1150 and BTO-1350 in
the frequency range from 100 Hz to 10 MHz at room temperature are shown in Fig. 3a, b, respectively. At a frequency
of 1 kHz, the dielectric constant of BTO-1150 was 1502
with tanδ of 0.016, while the dielectric constant and tanδ
of BTO-1350 were 1082 and 0.021, respectively. A similar
changing trend of dielectric constant and tanδ with varying
frequency was noticed for both BTO ceramics. In the range
of 100 Hz–1 MHz, the dielectric constant decreased slowly,
while tanδ varied slightly. With a further increase of frequency above 1 MHz, an abrupt drop in the dielectric constant and a rapid increase in tanδ were observed. This characteristic behavior is attributed to the orientational dielectric
Table 1 Summary of in-plane lattice constant (a), out-of-plane lattice constant (c), tetragonality (c/a), unit-cell volume (V), crystal structure, and
crystallite sizes (D) of BTO-800, BTO1150, and BTO-1350
Sample
A (nm)
c (nm)
c/a
V ­(nm3)
Crystal structure
D (nm)
BTO-800
BTO-1150
BTO-1350
0.4010
0.3994
0.3995
0.4010
0.4036
0.4037
1.0000
1.0105
1.0105
0.0645
0.0644
0.0644
Cubic
Tetragonal
Tetragonal
27.5
43.1
46.3
13
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A comparative study of dielectric and ferroelectric properties of sol–gel-derived B
­ aTiO3…
Page 5 of 8 713
Fig. 3 Dielectric constant and tanδ in the frequency range from 1 kHz to 10 MHz at room temperature of a BTO-1150 and b BTO-1350
Fig. 4 Dielectric constant of BTO-1150 and BTO-1350 as a function of temperature from − 45 to 180 °C in the frequency range from
100 Hz to 1 MHz
relaxation owing to the domain-wall vibration induced by
external electric field [12].
More detailed information on dielectric properties of
the BTO ceramics with fine and coarse grains was further
drawn by analyzing the temperature-dependent dielectric
constant during cooling, as shown in Fig. 4. There were
two peaks in each dielectric constant curve within the
measured temperature range from − 45 to 180 °C, corresponding to the tetragonal-to-cubic (T–C) phase transition
and the orthorhombic-to-tetragonal (O–T) phase transition
of the BTO. It was noticed that the dielectric constant of
BTO-1150 and BTO-1350 reached the maximum values
of 2500 and 8730, respectively (1 kHz), at the T–C phase
transition or Curie temperature (TC = 125 °C). With a further decrease in temperature, a smaller and broader peak
corresponding to the O–T transition appeared at 0 °C for
BTO-1350, while a shift toward higher temperature was
found for BTO-1150. From temperature-dependent dielectric constant, it was evident that the dielectric peaks at
both phase transitions of BTO-1150 became more diffused
and broader than those of BTO-1350. The diffused feature
at phase transition of BTO-1150 can be explained by distribution of distributed TC as a result of inhomogeneity due
to the different types of defects and various local densities existing in BTO-1150. In addition, another important
aspect is that dielectric constant of BTO-1150 was greater
than that of BTO-1350 at temperature below TC. Such a
dielectric behavior is almost similar to the results reported
by Arlt et al. [11] and Lee et al. [32]. Higher dielectric
constant of BTO-1150 arises from its higher internal stress
in an individual fine grain as compared to BTO-1350. Our
result is in agreement with those obtained by other works
(Table 2) that the dielectric constants at room temperature
were in the range of about 700–1500 for a broad grain
size between 0.8 and 40 μm [33–41]. It can conclude that
although sol–gel-derived BTO ceramics have different
grain sizes, a difference in precursors and preparation conditions do not affect significantly to their dielectric properties at room temperature. The additional chemicals may be
needed in the sol–gel synthesis for further enhancement of
dielectric constant. For example, Cui’s group employed the
various kinds of organic acids as surfactants (i.e., decanoic
acid, decanedioic acid, cetylic acid, and stearic acid) in the
sol–gel synthesis of BTO powders [40, 41]. They found
that the dielectric constant at room temperature enhanced
up to 2000–4000 depending on type of organic acids since
the relative density of the ceramic was quite close to theoretical density. In contrast, unlike at room temperature, the
dielectric constant at TC of BTO ceramics varied broadly
from 2500 to 9000, which strongly depended on grain
size (see Table 2). Therefore, the diffused behavior at the
T–C phase transition of sol–gel-derived BTO ceramics can
be manipulated by adjusting grain size. Moreover, there
13
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Ba(CH3COO)2/TTIP
Ba(CH3COO)2/TTIP
Ba(CH3COO)2/TTIP
BaCO3/TBOT
Ba(CH3COO)2/TTIP
Ba(NO3)2 ·8H2O/Ti/H2O2
Ba(CH3COO)2/TTIP
Ba(CH3COO)2/TBOT
Ba(CH3COO)2/TBOT
Ba(CH3COO)2/TBOT
Sharma et al. [33]
Sharma et al. [34]
Lobo et al. [35]
Deshpande et al. [36]
Li et al. [37]
Devi et al. [38]
Mahmood et al. [39]
Yu et al. [40]
Cui et al. [41]
This work
800 °C/1.3 h
900 °C/2 h
900 °C
850 °C/4 h
900 °C/2 h
750 °C/2 h
700 °C/1 h
500 °C/6 h
750 °C/6 h
700 °C/2 h
Calcination
condition
1350 °C/2 h
1250 °C/2 h
1300 °C/2 h
1300 °C/2 h
1350 °C/2 h
1280 °C/4 h
1200 °C/2 h
1300 °C/2 h
1400 °C/2 h
1250–1350 °C/4 h
1300 °C/6 h
1250 °C/2 h
Sintering condition
TTIP titanium (IV) tetraisopropoxide ­(C12H28O4Ti), TBOT titanium (IV) butoxide ­(C16H36O4Ti)
Precursor
References
–
–
0.8
5–15
0.8
20
40
–
18
0.5
2.0
0.7
1.5
2.0
45
1.0
12.2
Grain size
(μm)
700
1170
–
1280
1082
1040
1021
1452
800
2169
3270
3120
3392
3278
4569
1502
1082
εr at 25 °C
Table 2 Precursors, calcination and sintering conditions of sol–gel-derived BTO bulk ceramics and their dielectric properties
–
0.011
–
0.016
0.028
0.021
0.024
0.043
–
0.030
0.018
0.029
0.032
0.033
0.027
0.016
0.021
tanδ at 25 °C
2500
4370
6200
7200
1642
6170
5190
4092
5700
7955
8960
6650
7470
8355
8970
2500
8730
εmax at TC
1 kHz
1 kHz
1 kHz
1 MHz
1 kHz
1 kHz
1 kHz
10 kHz
1 kHz
100 kHz
Frequency
713 Page 6 of 8
G. Panomsuwan, H. Manuspiya
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A comparative study of dielectric and ferroelectric properties of sol–gel-derived B
­ aTiO3…
Page 7 of 8 713
Fig. 5 P–E loops measured at room temperature of a BTO-1150 and b BTO-1350
was no significant change in dielectric constant for both
BTO ceramics as the frequency increased from 100 Hz to
1 MHz along temperature range investigated, indicating
their frequency independent behavior or non-relaxor ferroelectric response.
and BTO-1350 is mainly attributed to the difference in the
grain size and dense in microstructure. It can conclude that
BTO-1350 is more suitable for ferroelectric device applications than BTO-1150 owing to its ferroelectric domain
switching behavior with low loss.
3.4 Ferroelectric properties
To further evaluate the ferroelectric behavior of sintered
BTO ceramics, the measurements of P–E loops were carried
out at room temperature, as shown in Fig. 5. The P–E loop
of BTO-1150 revealed an ellipse shape with an unsaturated
polarization, which is the characteristic feature of a lossy
hysteresis loop [42, 43]. It implies that BTO-1150 possessed
high leakage current or low resistance possibly due to its low
dense microstructure and the presence of porosities. Unlike
in fine-grained BTO-1150, the P–E loop of BTO-1350
showed a hysteresis loop with well-saturated polarization
at the applied voltage greater than ± 3000 V. This feature is
a clear evidence of ferroelectric domain switching in BTO1350. With an applied voltage of ± 4000 V, the remnant
polarization (Pr) of BTO-1350 reached 20.6 μC/cm2, while
the coercive fields (Ec) was 4.8 kV/cm. The Ec of BTO-1150
was found at 25.5 kV/cm, which is much greater than that of
BTO-1350. It is known that Ec refers to an external electric
field required for polarization reversal in ferroelectric materials. Therefore, it can suggest that a larger energy or higher
external electric field is required to reorient the domain walls
in BTO-1150, as compared to BTO-1350. High density of
grain boundaries and defects of fine-grained BTO-1150 can
cause the pinning effects on the movement of domain walls,
thus inducing high Ec values. For the BTO-1350 having
coarse grains, low density of grain boundary has a dilution
effect, resulting in a weak influence on its ferroelectric properties. The difference in the P–E loops between BTO-1150
4 Conclusions
The BTO nanopowders were successfully synthesized
via sol–gel method followed by subsequent calcination at
800 °C. The synthesized BTO powders exhibited a cubic
structure with the particle size of less than 100 nm. The
BTO-1150 and BTO-1350 had an average grain size of
about 1 and 12 µm, respectively. They showed a tetragonal
structure with high tetragonality (c/a) of 1.0105. The frequency dependence on dielectric properties of BTO-1150
and BTO-1350 revealed the relaxation behavior at high frequency above 1 MHz. The dielectric constant of BTO-1150
was less sensitive to change with temperature than BTO1350. The T–C phase transition or TC occurred at 125 °C for
both BTO ceramics. Room-temperature dielectric constant
of fine-grain BTO was higher than that of coarse-grained
BTO due to the grain size effect. A well-defined P–E hysteresis loop was observed only for BTO-1350 with coarse
grain size. In contrast, a lost hysteresis loop was observed for
BTO-1150 owing to its large leakage current. Our results in
this work can serve as a useful information and reference on
the dielectric and ferroelectric properties of sol–gel-derived
BTO bulk ceramics as well as a helpful guideline to the
researchers in this field.
Acknowledgements This work was financially supported by Kasetsart
University Research and Development Institute (KURDI) and Research
Grant for New Scholar from Thailand Research Fund (MRG-6180095).
13
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713 Page 8 of 8
G. Panomsuwan, H. Manuspiya
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13
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