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Influence of Complex Additives on

Structure, Microstructure, Phase
Transitions and Dielectric Properties of
BiScO3-PbTiO3 Ceramics
a a a a
E. D. Politova , G. M. Kaleva , A. V. Mosunov , N. V. Sadovskaya
b
& A. H. Segalla
a
Karpov Institute of Physical Chemistry , 105064, Obukha s-str.,
3-1/12, b. 6, Moscow , Russia
b
ELPA Company , Panfilovsky pr. 10, Zelenograd, 124460 , Moscow ,
Russia
Published online: 20 Sep 2013.

To cite this article: E. D. Politova , G. M. Kaleva , A. V. Mosunov , N. V. Sadovskaya & A. H.

Segalla (2013) Influence of Complex Additives on Structure, Microstructure, Phase Transitions
and Dielectric Properties of BiScO3-PbTiO3 Ceramics, Ferroelectrics, 449:1, 1-10, DOI:
10.1080/00150193.2013.822752

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 Ferroelectrics, 449:1–10, 2013
Copyright © Taylor & Francis Group, LLC
ISSN: 0015-0193 print / 1563-5112 online
DOI: 10.1080/00150193.2013.822752

Influence of Complex Additives on Structure,

Microstructure, Phase Transitions and Dielectric
Properties of BiScO3 -PbTiO3 Ceramics

E. D. POLITOVA,1,∗ G. M. KALEVA,1 A. V. MOSUNOV,1

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N. V. SADOVSKAYA,1 AND A. H. SEGALLA2

1
Karpov Institute of Physical Chemistry, 105064, Obukha s-str., 3-1/12, b. 6,
Moscow, Russia
2
ELPA Company, Panfilovsky pr. 10, Zelenograd, 124460, Moscow, Russia

Ceramic solid solutions from the region of morphotropic boundary on the base of
0.36BiScO3 -0.64PbTiO3 , modified by complex additives of Bi2 O3 and Ni2 O3 , Bi2 O3 and
MnO2 , and LiF additives in amounts up to 5 w. % have been prepared by the con-
ventional solid state reaction method. Decreasing of the phase formation temperature
accompanies by increasing in density of the doped ceramics have been revealed. Influ-
ence of additives on microstructure, dielectric, ferroelectric properties, and effects of
dielectric relaxation have been revealed.

Keywords BiScO3 -PbTiO3 ceramic solid solutions; ferroelectric phase transition; ad-
ditives

Introduction
Rather low temperature of the ferroelectric to paraelectric phase transition T C ∼600 K (Curie
temperature) determines the working temperatures of the most widely used Pb(TiZr)O3
(PZT) materials [1]. Though during last decade, a lot of efforts was aimed to the search of
new piezoelectric materials, till now their functional properties do not exceed the functional
parameters of the PZT-based materials [2].
However, for some technical applications such as automotive and aerospace applica-
tions piezoelectric materials with higher working temperatures T C and with high piezo-
electric activity are necessary [3].
Compositions close to the morphotropic phase boundary (MPB) which divides re-
gions with rhombohedral and tetragonal symmetries in the system BiScO3 -PbTiO3 (BSPT)
continue to be intensively studied last decade. Like in PZT system, they reveal high T C
values >700 K and rather high piezoelectric coefficients, so they are considered as promis-
ing for the development of new piezoelectric materials for high temperature applications
[4–12].
For the improvement of functional characteristics of piezoelectric ceramic oxide ma-
terials various cation substitutions are widely used. Additionally, the introduction of over
stoichiometric additives, mainly with low melting temperatures, in small amounts up to

Received September 25, 2012; in final form March 19, 2013.

∗
Corresponding author. E-mail: politova@cc.nifhi.ac.ru
[415]/1
 2/[416] E. D. Politova et al.

∼5 w. % is considered as an efficient approach for both the optimization of sintering and

regulation of electrical properties of piezoelectric ceramics. It has been revealed that bis-
muth and manganese oxides additives stimulate increasing of electroresistance, decreasing
of dielectric loss, and allow regulation of ferroelectric domain switching and fatigue effects
[13–18].
It was shown that introduction of excess Bi2 O3 intensified liquid-phase sintering and
compensates the Bi2 O3 -loss providing the increase in polarization and piezoelectric coef-
ficients d33 from 354 up to 408 pC/N in 0.37BiScO3 -0.63PbTiO3 ceramics doped by 5 at%
Bi [14, 16].
Earlier, we studied the influence of both A- and B-cation substitutions and of the
MnO2 , Bi2 O3 and other additives on phase composition, microstructure, phase transitions
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and piezoelectric properties of ceramics in the (1-x)BiScO3 -xPbTiO3 systems, with x =

0.60–0.66; A – Nd; B – Lu, Yb, Er, Y [19–22].
It was shown that the over stoichiometric additives provided the decrease of total
conductivity and dielectric loss more than one order at high temperatures, and increase of
d33 and kt piezocoefficients. Additionally, influence of Cr2 O3 additives on crystal structure,
dielectric and piezoelectric properties of compositions (1-x)BiScO3 -xPbTiO3 with x = 0.63,
0.635, 0.64, was studied [23].
Effects of dielectric relaxation originated from oxygen ionic transport were revealed
in some ceramics sintered at high temperatures. The increase of piezoelectric coefficients
d33 and kt up to 400 pC/N and 0.50, respectively, was observed in ceramics with x = 0.64.
In this work, influence of complex additives Bi2 O3 and Ni2 O3 , Bi2 O3 and MnO2 , and
LiF additive with low melting temperature on phase content, density, microstructure and
dielectric properties of ceramics on the base of the 0.36BiScO3 -0.64PbTiO3 solid solution
was studied.

Experimental Procedure
Ceramic solid solutions based on the composition 0.36BiScO3 -0.64PbTiO3 (BSPT) were
doped with complex additives: Bi2 O3 (3 w. %) and Ni2 O3 (0.5 w. %) (I), Bi2 O3 (3 w. %)
and MnO2 (0.5 w. %) (II), with LiF (1 w. %) (III) and LiF (5 w. %) (IV). The samples were
prepared by the two-step solid state reaction method using Bi2 O3 , Sc2 O3 , PbO and TiO2
oxides (“pure” grade) as starting reagents. Stoichiometric mixtures of the homogeneized
oxides were calcined at 973 K (7 h), then the samples were regrounded, over stoihiometric
additives were added, and pressed pellets were sintered at temperatures 1223 K, 1273 K,
1298 K and 1323 K (2 h) and slowly cooled to the room temperature.
Phase composition and crystal structure parameters were determined using the X-ray
diffraction (DRON-3M with CuKα -beam, ProfitVZ software). Microstructure of the samples
was checked by scanning electron microscopy (SEM) (JEOL JSM-7401F, Analysis Station
JED-2300). Dielectric properties were studied by dielectric spectroscopy (Agilent 4284 A,
1 V) in the temperature range of 300–1000 K at frequencies 100 Hz–1 MHz.

Results and Discussion

According to X-Ray diffraction data, dense single phase ceramic samples I and II were
prepared at Ts = 1223 – 1323 K (Fig. 1). It is clear that complex additives Bi2 O3 with
Ni2 O3 and MnO2 intensified the phase formation process as the dense single phase initial
BSPT 0.36/0.64 samples were prepared at higher sintering temperatures Ts = 1423 K.
Introducing of 1–5 w. % of LiF provides the decrease of sintering temperatures as well.
 Influence of Complex Additives [417]/3

The dense samples III and IV were prepared at Ts = 1223 – 1323 K, and at Ts = 1273 –
1298 K, respectively.
The influence of additives on the structure of solid solutions was proved. Initial BSPT
samples comprised the mixture of tetragonal and orthorhombic phases. Introduction of
rather small amounts of additives stimulates the shift of the compositions I and II to the
region of MPB with rhombohedral structure, while the shift the compositions III and IV
to the region with tetragonal structure (Fig. 1, insert). Small displacements of diffraction
peaks also indicate the small changes of the unit cell parameters of the samples I–IV.
The effects of additives on sintering temperature and density of ceramics were checked.
It is necessary to mark different influence of the additives and sintering temperature on
the density of the samples I–IV. Shrinkage of the sample I increases from the value of
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8.6% at sintering temperature Ts = 1223 K up to the value 11% at the temperatures Ts =

1298–1323 K. The shrinkage of the samples II doped by the complex additive Bi2 O3 -MnO2
slightly changes from 8.5% for Ts = 1223 K till 8.7% at higher sintering temperatures of
Ts = 1273–1323 K practically independently on sintering temperature.
Another type of influence of the additive and sintering temperature was observed in
ceramics doped by LiF. The shrinkage of the samples III and IV doped by LiF and sintered
at Ts = 1273 K reached 12–13%, however, it decreases with further Ts increasing. So, the
highest enhancement of the shrinkage of the sample was observed for samples I (11%), and
for samples III and IV (12–13%) sintered at Ts = 1273 K.
Microstructure of the doped samples was studied using the SEM method. The average
size of grains varies from ∼1 μm to ∼10–20 μm in ceramic samples I sintered at 1223
and 1323 K, respectively (Fig. 2). Ceramics 1 prepared at Ts = 1223 К have sharp grain
boundaries while those prepared at Ts = 1323 К are characterized by melted boundaries
that determined the manifestation of the liquid phase sintering mechanism.
Ceramics II are characterized by the homogeneous microstructure with the average
grain size ∼5 ÷ 10 μm. In ceramics III sintered at Ts = 1298 K growth of grains up to

Figure 1. X-ray diffraction patterns of the samples II (a) and IV (b) sintered at 1298 K: 0.36BiScO3 -
0.64PbTiO3 modified by Bi2 O3 (3 w. %) and MnO2 (0.5 w. %) (a) and by LiF (5 w. %) (b). In inserts
peaks with h2 + k2 + l2 = 4 for samples I–IV sintered at 1298 K are shown (Color figure available
online).
 4/[418] E. D. Politova et al.
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Figure 2. SEM images of surfaces of the 0.36BiScO3 -0.64PbTiO3 (BSPT)-based ceramics I–IV
sintered at 1223 К – 1323 К: I (3 w. % Bi2 O3 and 0.5 w. % Ni2 O3 , Тs = 1223 К, 2 h) (a), II (3 w. %
Bi2 O3 and 0.5 w. % MnO2 , Ts = 1298 К, 2 h) (b), III (1 w. % LiF, Ts = 1298 К, 2 h) (c), IV (5 w. %
LiF, Ts = 1273 К, 2 h) (d). White bars – 10 μm. (Continued)
 Downloaded by [Memorial University of Newfoundland] at 01:17 10 November 2013

Figure 2. (Continued)
Influence of Complex Additives
[419]/5
 6/[420] E. D. Politova et al.

∼20–40 μm was observed. Ceramics IV sintered at Ts = 1273 K have the highest density,
with the size of grains varying from 4 μm to ∼10 μm. Besides, small crystallites with
submicron size ∼100 nm were revealed in the samples IV, which may be related to the
presence of small amount of admixture phase.
It is worse noting the difference in the sintering mechanisms of the ceramics studied.
Though the liquid phase sintering comprises the main sintering mechanism in ceramics
doped with Bi2 O3 and LiF having low melting temperatures of 1098 and 1123 K, accord-
ingly, it is necessary to take into account the possibility of dissolving the additives in solid
solutions as well.
Additionally, during the sintering in the presence of excess of Bi2 O3 the compensation
of Bi- or Pb-oxides losses takes place. However, in the case of incomplete compensation
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of losses or in the case of substitution of the A-site cations by Li1+ cations, the creation of
oxygen vacancies in perovskite is inevitable. On the contrary, the introduction of MnO2 and
Ni2 O3 additives favors to the suppression of the oxygen vacancies formation. Moreover,
the change of relative content of tetragonal and orthorhombic phases in composition close
to the MPB observed may lead to the enhancement of mechanical strains influencing the
sintering process as well. From the other side, the presence of small amounts of admixture
phases may prevent further grain growth. The essential difference in the average grain sizes
of ceramics I and III sintered at the same temperature, illustrates this effect.
Dielectric measurements revealed the 1st order sharp ferroelectric phase transitions
marked by peaks in dielectric permittivity and corresponding minima in dielectric loss
versus temperature curves at temperatures near 700–800 K (Figs. 3, 4).
At the room temperature ∼300 K the values of dielectric permittivity ε for doped
samples are in 1.5–2 times lower than ε value of the undoped sample (Fig. 3a), that
obviously relates to lower conductivity of the doped ceramics.
The εmax value measured at f ∼1 MHz reaches ∼20,000 near the T C for the doped
samples II which is comparable to the εmax value of the undoped BSPT samples. However,
the samples I, III and IV revealed the εmax value in 2–3 times lower than the not modified
samples.
The value of dielectric loss of modified samples I and III and IV is higher, then that of
the undoped composition at room temperature (Fig. 3b). At temperatures of 500–950 K the
modified ceramics, except of samples II, revealed lower loss than the initial ones, and at
temperatures near T C the samples II revealed dielectric loss more than 2 orders lower than
that of initial ones.
Small shift of the T C values to 720 K in the samples I and to 700 K in the samples II
was observed in the modified ceramics in accordance with the small changes of the unit
cell parameters. In the samples III and IV besides the maxima of dielectric permittivity at
TC = 730 K additional anomalies were observed at higher temperatures ∼760–770 K. This
correlates with the X-ray data that point to the change of the relative contents of the phases
in the modified BSPT compositions close to the MPB. The enhancement of the transition
temperature correlates with the shift of the tetragonal constituent of compositions to the
phase diagram region characterized by higher TC values.
In the doped ceramics I–IV decrease of total electroconductivity σ was observed at
room temperature, while at temperatures near TC , σ value did not change in the samples
I though in doped ceramics II–IV slight decrease of total electroconductivity σ was also
observed (Fig. 3c).
It is necessary to mark, that in ceramics I, III and IV the effects of dielectric relaxation,
typical for the undoped BSPT samples were observed (Fig. 4). This effect is suppressed
practically completely in the samples II. This confirms the common conclusion on the
 Influence of Complex Additives [421]/7
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Figure 3. Dielectric permittivity and dielectric loss versus temperature curves (a, b), and total
electroconductivity versus reciprocal temperature (c) curves of initial ceramics 0.36/0.64 sintered
at Тs = 1423 К, 2 h (1); doped ceramics I sintered at Ts = 1323 К, 2 h (2); ceramics II (3),
ceramics III (4), and ceramics IV (5) sintered at Ts = 1298 К, 2 h. Measuring frequency f = 1 kHz
(cooling) (Color figure available online).

origin of relaxation anomalies connected with the presence of vacancies in the oxygen
sublattice, caused by the losses of lead or bismuth oxide at high sintering temperatures. It
is well known, that in the process of oxygen-ion transport in ferroelectric ceramic, polar
dipoles relaxing in the ac- electric field are usually formed [23, 24]. The decrease of
 8/[422] E. D. Politova et al.
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Figure 4. Dielectric permittivity versus temperature curves of initial ceramics 0.36/0.64 sintered at
Тs = 1423 К, 2 h (a); doped ceramics I sintered at Ts = 1323 К, 2 h (b); ceramics II (c), ceramics III
(d), and ceramics IV (e) sintered at Ts = 1298 К, 2 h. Measuring frequencies f = 1, 3, 10, 30, 100,
300, 1000 kHz (cooling).

total σ , revealed in modified samples II at high temperatures, may be explained by the

manifestation of both the effects of trapping of conduction electrons at the manganese sites
and of reducing ionic conductivity due to the formation of manganese ion–oxygen vacancy
defect complexes [15].

Conclusions
The influence of complex additives Bi2 O3 and Ni2 O3 , Bi2 O3 and MnO2 , and LiF with low
melting temperature in amounts up to 5 w. % on the phase formation, density, microstructure
and dielectric properties of ceramics on base of 0.36BiScO3 -0.64PbTiO3 composition
was studied. It was confirmed that proper choice of the over stoichiometric additives and
 Influence of Complex Additives [423]/9

optimization of thermal treatment conditions allowed to prepare dense single phase ceramics
with controllable size of grains. The 1st order ferroelectric phase transitions marked by
peaks in dielectric permittivity and minima in dielectric loss versus temperature curves
were observed at temperatures near 700 K. The enhancement of ferroelectric properties
and suppression of dielectric relaxation was revealed in ceramics II modified by Bi2 O3 and
MnO2 additives.

Acknowledgments
The work is supported by the Russian Fund for Basic Research (Grant 12-03-00388).
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