Bull. Mater. Sci.

(2023) 46:61 Ó Indian Academy of Sciences

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Structural, electrical and magnetic properties of lead-free double

perovskite multiferroic: BiSrFeCeO6

KALPANA PARIDA* and R N P CHOUDHARY

Physics Department, Siksha ‘O’ Anusandhan (Deemed to be University), Bhubaneswar 751030, India
*Author for correspondence ([email protected])

MS received 13 May 2022; accepted 16 October 2022

Abstract. In this paper, detailed studies of structural, micro-structural, dielectric, electrical and magneto-electric
characteristics of chemically synthesized a new double perovskite, BiSrFeCeO6 (strontium cerate-modified bismuth
ferrite), are reported. The basic crystal data (unit cell dimension and orthorhombic crystal system) of the compound were
obtained by analysing the room temperature X-ray powder diffraction data. Study of the surface microstructure of a
sintered pellet sample, recorded by scanning electron microscope at room temperature, reveals the formation of high-
density sample with the homogeneously and uniformly distributed grains of different size and shape. Analysis of fre-
quency-temperature dependence of dielectric parameters and nature of hysteresis loop has exhibited the ferroelectric
characteristics of the material. Studies of complex impedance and modulus components at different temperatures and
frequencies have provided electrical characteristics of grains and grain boundaries present in the material, which are
closely related to its microstructure. Thus, the correlation between the crystal structure with electrical properties and
relaxation mechanism of the prepared sample has been established. The type of dielectric relaxation process and
mechanism occurred in the compound have also been studied not only by analysis of the dielectric properties (er, tan d)
and impedance parameters, but also from the study of frequency-temperature conductivity. The existence of negative
temperature coefficient of resistance (NTCR) characteristics in the material has been confirmed from the temperature and
dc conductivity analysis. Similarly, the frequency and ac conductivity analysis show that the studied compound follows
Jonscher’s universal power law. Based on the structural, ferroelectric, magnetic and magneto-electric characteristics,
multiferroism in the new composition of bismuth ferrite has been established.

Keywords. Chemical reaction method; ferroelectric; impedance; magnetic.

1. Introduction paid on to work on lead-free bismuth ferrite BiFeO3 (BFO),

which has rhombohedral (distorted perovskite) structure,
Since the discovery of ferroelectricity in barium titanate in simultaneous anti-ferromagnetic and ferroelectric ordering
1940s, a large number of oxides of different structural for a large range of temperature (anti-ferromagnetic Neel
family including perovskite, tungsten bronze, layer struc- temperature TN = 370°C and ferroelectric Curie temperature
ture, etc. were examined to get materials with optimum TC*833°C [5]). However, from the technological applica-
physical propertied for devices. Out of all these, some lead- tions point of view, the performance of BFO is not very
based perovskite like lead titanate (PbTiO3), lead zirconate encouraging because of some inherent problems including
titanate (PbZrTiO3) was found most promising for devices, structural instability, leakage current, difficulty in getting
and thus these were widely used for device applications. single phase, low saturation magnetization/polarization, etc.
Because of the toxic nature and health hazard of lead, [6]. In order to solve the above inherent problems to opti-
severe attempts are being made to find out alternative of the mize the multiferroic properties of BFO, several approaches
lead-based materials not only for single device but also for have been attempted including varying synthesis methods,
multifunctional applications. In the last few years, much substitution of suitable elements at the Bi/Fe site [7] and
attention has been paid on to develop materials, having two fabrication of chemically synthesis method and/or com-
different conduction mechanism and phenomenon like fer- posites with the compounds of different structural family.
roelectricity and magnetism in a single phase. Such type of Though some improvement in the properties of BFO has
materials is expected to be used for a wide range of appli- been observed, there is still some scope for further work for
cation in electronic and other industries due to their the purpose. There is more attention for the discovery of
excellent ferroelectric, ferromagnetic and/or ferroelastic new perovskite materials having high TC half-metals. The
properties [1–4]. In view of this, much attention has been perovskites (ABO3) or more than one perovskite
 61 Page 2 of 9 Bull. Mater. Sci. (2023) 46:61

compounds belong to a huge number of oxide materials to fabricate pellets from cylindrical discs (10 mm diameter
with wide industrial applications. The double perovskites and 0.5 to 3 mm thickness), which were subjected to sin-
with a general chemical formulation of A0 A00 B00 B00 O6 are the tering process at 800°C for 8 h. Further, the analysis of
combinations of two perovskites, i.e., A0 B0 O3 and A00 B00 O3. surface micrographs obtained from scanning electron
In A0 A00 B00 B00 O6, A0 and A00 correspond to alkaline or rare- microscope (SEM) at room temperature was carried out to
earth metals cations, whereas B00 and B00 are transition metal examine the compactness as well as the microstructure of
cations [8]. It is found from the literature survey that no the developed material. For the purpose of electroding, both
attempt has been made to fabricate a double perovskite of the sides of the discs were painted with high-purity con-
BFO with another perovskite SrCeO3 in equal ratio (i.e., ducting silver paste and dried in an oven (at 140°C for 1 h).
BiSrFeCeO6), which is expected to provide some important The dielectric and impedance spectroscopy data (i.e.,
data and information on its new composition. Strontium impedance, modulus, dielectric parameters and conductiv-
cerate (SrCeO3) has a perovskite-like protype structure with ity) were obtained using impedance analyzer and LCR
high temperature proton conductor characteristics useful for meter (PSM 1735, N4L) as a function of temperature and
important potential applications. It has defect perovskite- frequency (1 kHz to 1 MHz). The field-dependent dielectric
like structure in orthorhombic phase with space group Pnma polarization (P–E) loop of the sample was recorded using
or Pbnm. As this compound has unique properties, addition loop tracer (Marine India Company). The vibrating sample
of this compound to BiFeO3 is expected to provide some magnetometer (VSM, Lake Shore-7410), with a maximum
important information about structure and physical proper- applied field of ±8 kOe, was used to measure the magnetic
ties of new composition of bismuth ferrite (BiSrFeCeO6). behaviour of the sample at room temperature. Similarly, the
The detailed literature survey shows that the effect of magneto-electric coupling coefficient of the magnetically
simultaneous addition of different non-iso valence element poled sample was obtained by M–E coupling set up (M/S
(i.e., (Sr2?/Ce4?) at the (Bi3?/Fe3?) site on structural and Marine India Company).
physical properties of BFO has not been studied and
reported by chemically prepared sample so far. Therefore,
with an objective to tailor the structural, dielectric, electri- 3. Results and discussions
cal and multiferroic properties of bismuth ferrite, we have
been motivated to fabricate and study a double perovskite 3.1 Structural and microstructural properties
oxides of a general formula A0 A00 B0 B00 O6 (A0 = Bi, A00 = Sr,
B0 = Fe, and B00 = Ce forming BiSrFeCeO6 = BiFeO3 ? Figure 1 exhibits XRD pattern of the calcined powder of
SrCeO3) which should provide a reasonably better perfor- BiSrFeCeO6 at room temperature. As the location and
mance for devices with interesting structural, dielectric and intensity of most of the diffraction peaks of pattern differ
magnetic properties. In order to have better understanding from those of ingredients used, the synthesis of new mate-
of the material, it is proposed to study structural, electrical, rial is expected. The diffraction peaks of the pattern were
dielectric and magnetic properties of the compound in dif- examined by the ‘POWD’ software [9]. Initial examination
ferent experimental conditions. of intensity and distribution of X-ray peaks suggests that the
sample has crystalline nature. To start with, the indexing of
all the peaks was carried out in different crystal system and
2. Experimental

The polycrystalline BiSrFeCeO6 was produced by a

chemical reaction technique using high-purity ingredient,
viz. bismuth nitrate (Bi (NO3)35H2O), strontium nitrate
(SrNO3)2, iron (III) nitrate nano hydrate (FeNO3)39H2O
and ceric ammonium nitrate, Ce(NH4)2(NO3)6 (M/s Loba
Chemicals, India) in appropriate stoichiometric ratio. A
clear solution of strontium, iron, bismuth and ceric ammo-
nium nitrate was made with deionized water. This solution
was dried out at 120°C for 6 h. The obtained dried powder
was subjected to annealing and calcination at 750°C for 4 h.
The fine powder of the lump, obtained from calcination and
annealing, was achieved through grinding. The phase of the
resultant powder was examined by analysing the XRD
(X-ray diffraction) data collected at room temperature with
´
CuKa radiation (k = 1.5405 Å) with small scan angle. The
X-ray powder diffractometer (D8 Advance; Bruker) was
used for this purpose. The fine powder compound was used Figure 1. X-ray diffraction pattern of BiSrFeCeO6.
Bull. Mater. Sci. (2023) 46:61 Page 3 of 9 61

three-unit cell configurations. On the basis of the best fit 3.2 Microstructural studies of BiSrFeCeO6
(i.e., minimum difference between the observed and cal-
culated value of Bragg angle and inter planar distance of Figure 2a shows SEM micrograph of the chemically syn-
each peak of the pattern), crystal system and unit cell were thesized sample. The micrographs reveal a homogeneous
selected. The least-squares unit cell dimensions of the nonuniformly distributed crystallites/grains of varying size
material are found to be; a = 4.110 (2) Å, b = 13.907 (2) Å [linear dimension (0.3–0.8 lm)]. The agglomeration of
and c = 24.226 (2) Å (standard deviation in parentheses). As grains with a porosity is observed in sample. Figure 2b
most of the peaks have exactly been indexed with the above represents the energy dispersive X-ray (EDX) pattern,
determined unit cell dimensions (a, b, c) with orthorhombic which shows the presence of different elements (Bi, Sr, Fe,
crystal structure, it has been proved that this sample is a Ce and O) in the sample confirming the formation of desired
single-phase compound. Similarly, the study of the basic compound BiSrFeCeO6. The estimated amount of these
crystal structure and the corresponding data suggests that elements present in the prepared sample, in term of weight
the developed material has single-phase with orthorhombic % and atomic %, has been given in table 2. The presence of
structure [10]. Figure 1 shows the X’pert high score match elements and estimated amount of these elements in EDX
of the compound BiSrFeCeO6 with parent compound clearly confirms the formation of the BiSrFeCeO6 com-
SrCeO3 (Ref: jcpds-01-083-1156). All the peaks with dobs, pound without the presence of foreign elements and in
dcal and (h k l) values are given in table 1. The crystallite required stoichiometric ratio. Figure 2c shows the elemental
size (D) has been estimated by Scherrer’s formula with the mapping of BiSrFeCeO6. It can be said that the present
full-width half-maximum (b) of the diffraction peak; double perovskite sample is characterized with uniform
D = b1kk (k = X-ray wavelength (0.15406 nm), distribution of elements over the entire cross-section of the
cosh
2 sample with proper stoichiometric ratio, as evident in the
h = diffraction angle, k = 0.89). The average crystallite element mapping. The formation of the required compound
size (D) of the sample, estimated from some of the intense is confirmed from the compositional analysis.
peak’s u, is found to be 13 nm [11].

3.3 Dielectric characteristics

3.3a Frequency dependent dielectric parameters: Figure 3a

and b shows the frequency and temperature dependence
of er and tan d of BiSrFeCeO6.
Table 1. Comparison of dobs and dcal for different (h k l) planes These dielectric parameters are strongly dependent on
of BiSrFeCeO6. polarization, frequency, temperature and experimental
conditions. The high value of relative dielectric constant at
dobs dcal I/I0 h k l
low frequency is due to the existence of all the different
3.9430 3.9417 12 1 1 0 types of polarizations, such as ionic, atomic, dipolar and
3.7494 3.7482 13 1 1 2 electronic in the material. On increasing frequency, these
3.3396 3.3419 21 0 4 2 polarizations slowly vanish and finally only electronic
3.1367 3.1344 100 1 0 5 polarization remains at very high frequency ([1010 Hz),
2.9616 2.9590 41 0 1 8 accordingly, the value of er decreases (with increasing fre-
2.7801 2.7815 87 0 5 0 quency) and finally becomes constant at high frequency. As
2.4746 2.4742 8 1 2 7 can be seen in figure 3a, temperature also has significant
2.2656 2.2630 15 1 5 2 effect on dielectric constant. Therefore, at low frequencies
2.1523 2.1531 8 1 5 4 and high temperatures, we have observed high value of
2.0732 2.0804 9 1 5 5
dielectric constant. Similar trend is observed in frequency
1.9939 1.9916 13 2 0 3
1.9640 1.9644 25 2 2 1
and temperature dependence of dissipation factor (tan d).
1.9178 1.9177 41 1 5 7 The presence of bismuth and iron of the studied compound
1.8475 1.8474 10 0 1 13 could be one of the reasons for the high value of tangent
1.7561 1.7565 11 0 6 9 loss at low frequencies and high temperatures. At high
1.6845 1.6848 14 1 1 13 temperatures and in the low-frequency region, the value of
1.6334 1.6335 30 2 0 9 er gradually decreases with the increase in frequency.
1.5994 1.5984 25 0 7 9 Hence, the low-frequency region displays dispersion, which
1.5654 1.5644 10 2 5 5 is a normal characteristic of all the dielectrics. In the high-
1.3864 1.3867 10 0 6 14 frequency limit, the value approaches to a small constant
1.3539 1.3541 8 2 2 13 value. The grain boundary is either being short circuited (up
1.2415 1.2419 14 1 9 10
to 150°C) or has a relatively low contribution. At low fre-
1.2116 1.2115 10 0 5 18
quencies, the dielectric constant is maximum because of the
 61 Page 4 of 9 Bull. Mater. Sci. (2023) 46:61

Figure 2. (a) SEM image, (b) EDX pattern and (c) element mapping of BiSrFeCeO6.

thus reaches at a stable point, which shows the nature of

Table 2. Weight % and atomic % from EDX spectra. polar dielectric. This type of trends suggests polarization is
based on domain switching [12].
Element Weight % Atomic %

OK 16.21 59.53
3.3b Temperature-dependent dielectric parameters: Fig-
Fe K 9.40 9.89 ure 4a exhibits the variation of relative dielectric constant
Sr L 16.50 11.06 (er), of BiSrFeCeO6, with temperature at selected
Ce L 23.49 9.85 frequencies. The dielectric constant slowly increases up to
Bi M 34.41 9.67 about 200°C, increases very fast to have maximum at
Total 100.00 around 300°C and then decreases fast showing a peak. The
dielectric peak decreases fast with increase of frequency
without shift in peak position indicating its association with
IBLC, which can be explained by Maxwell Wagner
existence of oxygen vacancy, grain boundary and interfacial mechanism [13]. It is found that the substitution of high
dislocation, etc. So, the value of dielectric constant and amount (50%) of co-doping (Sr, Ce) at the (Bi, Fe) sites of
dielectric loss decreases with increase of frequency, and BiFeO3, the relative dielectric constant of the parent
Bull. Mater. Sci. (2023) 46:61 Page 5 of 9 61

Figure 3. Variations between (a) er and (b) tan d vs. frequency at selected temperatures of BiSrFeCeO6.

Figure 4. Variations of (a) er and (b) tan d with temperature at selected frequencies of BiSrFeCeO6.

compound (BFO) drastically increases from 340 transition of bismuth ferrite (BiFeO3) is about 380°C, an
(temperature = 300°C, frequency = 100 kHz) to 1500 in anomaly observed near 300°C may corresponds to the same
chemical reaction technique carried out at the same anti-ferromagnetic (TN) transition. Since the ferroelectric
frequency and temperature [14]. Similarly, the tangent loss transition (Tc) of bismuth ferrite multiferroic is very high
decreases (figure 4b) with increase in frequency as of the ([850°C), it was not possible to observe this phase transition
relative dielectric constant and exhibit a peak around 225°C. in experimental temperature range. The shift of peak is
The peak temperature is found to shift towards higher frequency and temperature dependent. The peak shifts
temperature with increase in frequency, implying towards high temperature side on increasing the frequency,
temperature-dependent relaxation processes [15]. The again, showing the characteristics of relaxor with thermally
dielectric constant is found to increase many folds and the originated relaxation mechanism of the material. The reason
dielectric loss of bismuth ferrite decreases sharply on doping for higher value of dissipation factor (as compared to that of
Sr, Ce at its Bi/Fe sites. The high value of dielectric constant room or low temperatures) at low frequency and high
and the low value of tangent loss can potentially be employed temperature could be the same as above. The values of
in electronic devices. Figure 4a shows that at room dielectric and tangent loss of this sample are very much
temperature dielectric constant starts increasing with rise comparable to those of the other reported materials of this
of temperature at all the mentioned frequencies and reaches type [16]. On further increase of temperature, tangent loss
its highest value at a particular temperature and then decrease increases very fast. This increase may be associated with
showing a dielectric anomaly. As the anti-ferromagnetic space charge, defect or some impurities.
 61 Page 6 of 9 Bull. Mater. Sci. (2023) 46:61

3.4 Impedance spectroscopy studies 3.5 Modulus analysis

Figure 5a illustrates the variation of Z0 (real component of The variation of electric modulus components of complex
impedance Z) with frequency for BiSrFeCeO6 (BSFCO) at modulus (M0 and M00 ) of BiSrFeCeO6 with frequency has
selected temperatures. The decrease of Z0 with increase in been shown in figure7 at selected temperatures. From
temperature for the entire frequency range indicates figure 7a, it can be seen that the value of M0 in the low-
occurrence of semiconductor (NTCR = negative tempera- frequency range tends to zero. Also, the frequency range at
ture coefficient of resistance) behaviour in a BSFCO cera- which the M0 value reduces to zero, increases with the
mic sample. The samples exhibit normal dielectric increase in temperature. In figure 7b, it is noticed that with
behaviour of decreasing Z0 with increase in frequency. increase in temperature, the M00 maximum relaxation peaks
Figure 5b presents frequency dependent Z00 (imaginary shift towards the high-frequency region, which suggests the
component of Z) of BiSrFeCeO6 at different temperatures. temperature dependence of dielectric relaxation.
The shift in the asymmetric peak broadening in the high-
frequency region with rising of temperature has been
observed. From the above graphs, the existence of thermally 3.6 Conductivity analysis
activated electrical relaxation process in the material can be
understood [17]. At high frequencies, all the Z00 spectra for The ac conductivity is plotted in figure 8a and b as a
different temperatures unites. The asymmetric broad peak function of frequency and temperature, respectively, for
points to a distribution of relaxation times. BiSrFeCeO6. The formula, rac = xereotand (where, x is the
Figure 6a–c shows the complex impedance spectrum of angular frequency of the ac source, tan d is the dielectric
BiSrFeCeO6 corresponding to the impedance data taken at loss and eo is the dielectric permittivity in vacuum), has
various temperature and frequency. The corresponding been used to calculate the ac conductivity of the sample
resistance and capacitance of grains and grain boundary of [18]. The nature of the ac conductivity plots can be
BSFCO have been compared in table 3. From the Nyquist described by Jonscher’s power law as given below [19]:
plots, it has been concluded that NTCR behaviour exhibits rt ¼ rdc þ Bxn
due to the decreases of grain resistance with increasing
temperature, which suggests that the Nyquist plots have the where n is a dimensionless exponent with 0\n\1, r(x) is
radius of the arcs. The Debye type of relaxation can be the ac conductivity at the angular frequency x, rdc is the dc
described with the help of constant phase element (i.e., conductivity, rt is the total conductivity and B is the con-
CPE), which can be connected to the parallel RC network in stant that depend on the intrinsic material property and
the proposed circuit [16]. In the present study, distorted temperature. At the low frequencies and low temperatures,
semicircular arcs have been obtained in the Nyquist plot at the value of rac rises gradually, and at high temperature, rac
all the experimental temperatures. For example, the becomes almost frequency independent. The activation
depressed angle of the semicircular plot corresponding to energy of the sample is found decreasing from 0.33 to
150°C below the Z00 axis, which is a measure of relaxation 0.27 eV on increasing frequency from 10 kHz to 1 MHz. In
time distribution, is found to be 3.6°. The existence of non- this high frequency region, the calculated ac conduction
Debye type of relaxation is a consequence of non-uniform activation energies are found to be smaller than that of the
grains and structural distortions [17]. low-frequency region. This is possibly because of the dif-
ference in mechanism of conductivity. At low frequencies,
instead of relaxation/orientation mechanism, the conduc-
tivity is considered by mobility or transportation over long
distances. The relaxation/orientation process requires higher
energy when compared with the energy requirement for the
mobility of the charge carriers over longer distances. The
calculated activation energy at the high temperatures can be
related to the residual cations in the grain boundary and the
formation of association among the oxygen vacancies or
thermal motion of the oxygen vacancies [20].

3.7 Multiferroic properties

The double perovskite compound BiSrFeCeO6 shows

multiferroics properties possessing more than one ferroic
Figure 5. Variations between (a) Z0 and (b) Z00 (inset) vs. order. To confirm the multiferroics nature of the sample, we
frequency at selected temperatures of BiSrFeCeO6. have performed the P–E hysteresis loop, M–H hysteresis
Bull. Mater. Sci. (2023) 46:61 Page 7 of 9 61

Figure 6. Variations between Z0 and Z00 at (a) 25–100°C and (b) 150–250°C. (c) The deviation angle at 150°C of
BiSrFeCeO6.

Table 3. Calculated values of Rg (grain resistance), Cg (grain capacitance), Rgb (grain boundary resistance) and Cgb (grain boundary
capacitance) at different temperatures.

Temp.
(oC) Model Rg (X) Cg (Faraday) Rgb (X) Cgb (Faraday)

25 (RC) (RQC) 2.468E?04 3.991E–010 1.561E?04 1.000E–025

50 (RC) (RQC) 3.240E?02 6.856E–010 1.824E?04 6.252E–019
100 (RC) (RQC) 2.819E?03 3.667E–010 1.484E?03 8.445E–020
150 (RC) (RQC) 7.219E?02 3.143E–010 2.252E?02 1.000E–020
200 (RC) (RQC) 3.293E?02 3.089E–010 9.420E?01 2.982E–018
250 (RC) (RQC) 3.122E?02 1.733E–010 8.314E?06 2.072E–010

Figure 7. Variations of (a) M0 and (b) M00 with frequency for BiSrFeCeO6 at different temperatures.
 61 Page 8 of 9 Bull. Mater. Sci. (2023) 46:61

Figure 8. AC conductivity of BiSrFeCeO6 as a function of (a) frequency and (b) temperature.

Figure 9. (a) P–E hysteresis loop, (b) M–H hysteresis loop and (c) magneto electric voltage coefficient of
BiSrFeCeO6.

loop and M–E coupling measurement at room temperature. The appearance of P–E hysteresis loop indicates the ferro-
Figure 9a explains the polarization hysteresis loop of the electric property in the sample. As shown in figure 9a, well
tested sample at room temperature. This graph suggests that developed but lossy ferroelectric hysteresis loop is observed
polarization is dependent of electric field and frequency. for BSrFeCeO6.
Bull. Mater. Sci. (2023) 46:61 Page 9 of 9 61

The magnetic hysteresis (M–H) loop (figure 9b) of this drives), devices in optoelectronics, actuators, microwave
sample has been recorded at room temperature using VSM electronics, transducers and stress sensors).
(vibrating sample magnetometer) to find the ferromagnetic
nature of the sample. The saturation magnetization of the
studied sample is found to be 0.4 emu g–1. The evaluated Acknowledgements
magneto electric coupling coefficient, generated by cou-
pling of electric and magnetic order parameters, is pre- We are grateful to Dr Satyabati Das, IIT, Bhubaneswar,
sented in figure 9c. Initially the tested sample was Odisha, and Dr Perumal Alagarsamy, Professor in Physics,
electrically poled as well as magnetically poled for M–E IIT Guwahati, Assam, India, for their kind help in
coefficient evaluation. Due to polling, it gets the saturation experiments and analyses work.
in charge and spin alignment which is essential for effective
interaction between the poled sub-lattices. The magneto
electric coupling coefficient (aE ) can be evaluated from the
given equation [21]: References
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