R E SE A R CH A N D D E V ELO PM EN T | Perovsk i te

Synthesis and Characterization of

Bismuth Ferrite-Nickel Ferrite
Nanocomposites
S. Mukherjee1
Abstract: A chemical route was used to synthesize perovskite bismuth ferrite and spinel nickel
ferrite of bismuth ferrite-nickel ferrite nanocomposites. The precursors mixed were made to
undergo thermal analyses to observe the crystallization temperature. Then the precursor samples
were heated at 550, 600 and 700 °C for 4 h, followed by XRD analyses to determine phase formation.
Crystallite size, strain analyses by the Williamson-Hall plot and planes of orientations were noted
from XRD analysis. It was observed that 600 °C was the optimum temperature for phase
development. Morphology analyses exhibited an agglomerated mass of particulates, while
individual phase particulates were polygonal and irregularly shaped. EDX analysis confirmed the
elemental compositions of the sample synthesized, while FTIR analysis confirmed the presence of
M–O octahedral and tetrahedral coordinations of the M–O bonds formed.

Keywords: perovskite, spinel, crystallization, morphology, phase, M–O coordinations

1. Introduction product property is more interesting than pare varying proportions of the per-
Bismuth ferrite is a single phase multiferroic the sum properties that are present in the ovskite-spinel bismuth ferrite-nickel ferrite
material, which has a distorted octahedral composite but remain absent in individual composite by chemicals using standard pre-
structure. It exhibits weak magnetism due to phases. For composite materials, the magne- cursors based on nitrate salts, citric acid,
the spin cycloid magnetic moment, while toelectric effect is a product tensor property ammonium hydroxide followed by phase
oxygen vacancies are noted due to Fe3+ to Fe2+ and has been found to be applicable for analysis, bonding analysis from FTIR spec-
reductions. Due to these vacancies current devices such as switches, actuators, magnetic tra and morphology by SEM. EDX confirms
leakage occurs, limiting its application for field sensors, electronic memory devices, t he element a l c omp o sit ion of t he
device fabrication. To reduce the current microelectronics, spintronics and others [2, composite.
leakage, doping of rare-earth and transi- 3]. The artificial magnetoelectric effect is
tional metal ions is carried out at A and B based on product properties, and composites
sites of the perovskite bismuth ferrite. Multi- that are multiferroic have much better appli- 2. Experimental
ferroics are a certain category of materials cations than s­ ingle-phase ones. [3] To date,
that possess multiple ferroic orders like fer- several composite materials have been used 2.1 Synthesis of bismuth-ferrite
roelectricity, ferromagnetism and ferrotor- for magnetoelectric and multiferroic devel- and nickel-ferrite
roidicity, either in single phase or as compos- opment s , l i ke Ni Fe 2 O 4 –BaTiO 3 [4], Bi-nitrate and Fe-nitrate (1:1 molar ratio, AR
ites [1]. Composite materials based on ceram- Ni 0. 8 Zn 0. 2 Fe 2 O 4 –Ba 0.6 Sr 0.4 TiO 3 [5], (x) grade) were mixed properly with optimum
ics are of vital importance in modern science Co 0.5Zn0.5Fe2O 4+(1-x)PLZT [6], multilayer deionized water after being weighed individ-
and applications. The amount of phases composites of PZT/Ter fenol-D [7], ually. 2 moles of citric acid was then added,
within the composite matrix plays a vital role BiFe0.5Cr0.5FeO3–NiFe2O4 [8] CuFe2O4-PZT and the resultant was mixed properly. Ethyl-
in the development of the required proper- [9], BiFeO3-PT [9, 16], NiFe2O 4 -PZT [10], ene glycol was then added to the resultant
ties, since a composite executes sum proper- BaTiO3–CoFe2O4 [11], BiFeO3–CoFe2O4 [11, mixture, which acts as a chelating agent in
ties or product properties. Individual phases 13, 14, 15] an BiFeO3 BaTiO3 [12]. Currently, volumetric ratio of 60:40 with the citric acid
provide the weighted sum of the contribu- limited research is available on the bismuth mix solution. The final mix solution
tions proportional to the volume fraction of ferrite-nickel ­ferrite-based composite. The obtained was stirred with a magnetic stirrer
phases giving rise to the sum properties. The present experimental research aims to pre- for about 1–2 h for homogeneity. After being

42 Interceram 5 | 2019www.interceram-review.info
Author muth ferrite and Ni−Fe hydroxides were mine the stretching and vibration of the
mixed in the molar ratio of 0.6:0.4 and M–O bonds responsible for the composite
DR. SOUMYA MUKHERJEE  0.4:0.6, respectively, in an agate motor. The synthesis.
( smmukherjee3@gmail. finely ground mixture was then heated in a
com), is presently Assistant tube furnace at temperatures of 550, 600 and
Professor, Department of
700 °C for 4 h in normal air atmosphere. 3. Results and discussion
Metallurgy, Kazi Nazrul Uni-
versity Asansol. His major
Figure 1 depicts the thermal analysis car-
areas of interest are elec- 2.2 Characterization techniques ried out over the mixed precursor of bis-
tronic materials, compos- The thermal analysis was carried out with a muth ferrite-nickel ferrite of equimolar
ites, ceramic synthesis by DSC-TGA analyzer (Perkin Elmer) on pre- ratio. DSC-TGA was carried out up to
various chemicals, solid cursors (a mix of dry powder after 330 °C and 750°C at a 10 K-heating rate. Minor weight
state processes and others. Ni-Fe hydroxides precipitates after drying) in changes and the endothermic trough at
His teaching topic interests
the range from room temperature to 750 °C 110–160 °C were due to the removal of
include metal working,
physical metallurgy, me-
with a heating rate of 10 K/min in the pres- water and some chelating agents used for
chanics of materials, mate- ence of nitrogen atmosphere. The results aid complexation. The prominent weight
rials engineering, thermo- the identification of the heat treatment change and an exothermic peak coupled
dynamics of materials and required for crystallization in annealing fur- with an endothermic trough at around 160–
others. naces. XRD was carried out on the annealed 250 °C was due to the breaking of chelating
sample to identify the phases and also to agents and the formation of metal oxides
determine strain; the Williamson–Hall plot from the respective precursor salt. Drastic
method was utilized. Morphology analyses weight changes occurred until 200 °C,
were carried out by scanning electron which was primarily due to the loss of
microscopy to observe the microstructure of hygroscopic water molecules. From 200 °C
the synthesized samples, while the elemental onwards the loss in weight was due to the
analysis was carried out by EDX to confirm elimination of crystallization water, the
the composition. M–O octahedral and tetra- intermediate reaction that occurs for chela-
hedral coordinations were observed to deter- tion and its breakdown to form ferrites.

DSC-TGA of sample BFO-NFO

7.0
stirred to obtain a homogeneous solution, it
Tcrystallization 426 °C
was kept in an alumina crucible and heated
in a pot furnace to 330 °C for about 45 min 6.8
until powdery masses appeared. The powder
mass was then crushed, and sintering was
carried out at 450 °C for 2 h to form BiFeO3 0
6.6
(bismuth ferrite).
Weight change
Heat flow

A co-precipitation chemical route was

undertaken with Ni-nitrate, Fe-nitrate in 1:2
6.4
molar ratio, and both were dissolved individ-
ually in deionized water. Then two solutions
of nitrates were mixed and mildly heated at
60–70 °C for 40 min to accelerate dissolu- 6.2
tion. NH4OH was added drop-wise to the
mixed nitrate solution to precipitate Fe−Ni
hydroxide. Complete filtration was obtained 6.0
after 24 h, and the resulting wet precipitate
-20
was heated mildly at 80–90o C for 3–4 h to
0 100 200 300 400 500 600 700 800
dry it completely and to obtain a brown
coloured ultra-fine powder of Ni-Fe hydrox- Temperature (°C)
ides. To synthesize the bismuth ferrite-nickel Figure 1 DSC-TGA of bismuth ferrite-nickel ferrite up to 750 °C with a heating rate of 10 K/min
ferrite composite, dried powder mass of bis- (© Mukherjee)

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R E SE A R CH A N D D E V ELO PM EN T | Perovsk i te

Moreover, the dried coprecipitate form of mined by using Braggs law of diffraction ence of both phases indicated the formation
Ni−Fe salts undergoes a reaction to form a while keeping ion correspondence with the of composite. With a change in the molar
spinel phase. The crystallization tempera- JCPDS card No PDF#01-074-2016, PDF#01- fraction of perovskite-spinel, it was observed
ture is noted to be about 426 °C from the 074-2013 for the respective perovskite-spi- for all cases that perovskite exhibits a much
DSC-TGA analysis. The peak is noted to be nel phase of the composite. The scan rate of more prominent presence and sharp peaks
exothermic in nature, as is evident from the 5 °/min was carried out within a scan range in comparison to the spinel phase. Nickel
nature of the heat flow. This also indicates of 10–80 °. The phase analysis revealed high ferrite phase was observed to be more prom-
the onset of the phase evolution for the intense sharp peaks without any hump or inent with an increase in temperature. Peak
composite material. discontinuity. Moreover, broad peaks were position and nature were found to be in cor-
Figure 2 to Figure 4 depict the XRD not observed during the scan either. Sharp respondence with the findings of the previ-
spectra of the phases formed after anneal- intense peaks for both perovskite bismuth ous work of Soumya Mukherjee et.al. [17,
ing at three different temperatures for a ferrite and spinel nickel ferrite phases were 18]. The crystallite size is evaluated using
fixed soaking period. Phases are deter- noted for all samples. The prominent pres- Scherrer’s equation t = 0.9λ/βcosθ, where t is

0.4 BFO-0.6 NFO 550 4hrs 0.6 BFO-0.4 NFO 550 4hrs

BFO BFO

BFO BFO
BFO
Intensity (a.u.)

Intensity (a.u.)

BFO
NFO
BFO
NFO NFO BFO
NFO BFO BFO
BFO
NFO
NFO
NFO NFO

10 20 30 40 50 60 70 80 10 20 30 40 50 60 70 80
Angle (2θ) Angle (2θ)
Figure 2 XRD spectra of 0.4BFO-0.6NFO and 0.6BFO-0.4NFO after a 4 h soaking period at 550 °C (© Mukherjee)

0.4 BFO-0.6 NFO 600 4hrs 0.6 BFO-0.4 NFO 600 4hrs
BFO

BFO

NFO
Intensity (a.u.)
Intensity (a.u.)

BFO
NFO NFO
NFO

BFO NFO BFO

NFO
BFO BFO
BFO
BFO NFO
BFO

10 20 30 40 50 60 70 80 10 20 30 40 50 60 70 80
Angle (2θ) Angle (2θ)

Figure 3 XRD spectra of 0.4BFO-0.6NFO and 0.6BFO-0.4NFO after a 4 h soaking period at 600 °C (© Mukherjee)

44 Interceram 5 | 2019www.interceram-review.info
 0.4 BFO-0.6 NFO 700 4hrs 0.6 BFO-0.4 NFO 700 4hrs

BFO
BFO

BFO

Intensity (a.u.)
BFO/NFO
Intensity (a.u.)

NFO
BFO BFO
NFO BFO
BFO
BFO NFO NFO
NFO

BFO NFO

10 20 30 40 50 60 70 80 10 20 30 40 50 60 70 80
Angle (2θ) Angle (2θ)
Figure 4 XRD spectra of 0.4BFO-0.6NFO and 0.6BFO-0.4NFO after a 4 h soaking period at 700 °C (© Mukherjee)

the crystallite size, λ is the wavelength From the above plots (Figure 5) it can be intrinsic stretching vibration of the metal at
1.54 Å, β is the full width half mean and θ is observed that the crystallite size increases the tetrahedral site is in the range of 620–
the angle. It is noted that broadening occurs with the sintering temperature, while the lat- 550 cm-1, and that for the metal at the octa-
with a decrease in crystallite size causing tice strain decreases. Increasing the molar hedral site lies in the range of 450–385 cm-1.
prominent lattice strain in the material fraction of perovskite bismuth ferrite in the The stretching vibration observed at 450 cm-1
matrix. Thus, the total line broadening is composite further decreases the resulting is characteristic of inverse spinel nickel fer-
due to both the crystallite size and lattice strain of the matrix, while the reverse hap- rite. The strong absorbance peaks at 650–
strain. pens when increasing the spinel mole frac- 750 cm-1 are due to the Fe–O stretching and
tion of the composite matrix. bending vibration, which is characteristic of
β=0.9λ/tcos(θ) + ηtanθ The FTIR spectral analysis of the synthe- perovskite compounds. The absorption
or sized composite is shown in Figure 6. Previ- spectra obtained was found to be in corre-
βcosθ= 0.9λ/t + ηsinθ (1) ous experimental research showed that the spondence with the experimental findings

The above equation is known as William-

son-Hall equation. By plotting versus sinθ,
we can find the lattice strain (η) from the
Table 1 Crystallite size and lattice strain for 0.4BFO-0.6NFO at different temperatures (© Mukherjee)
slope of the graph and the crystallite size (t) Temperature 2θ [degrees] Crystallite size Crystallite size from Lattice strain [%]
[°C] from Scherrer’s Williamson-Hall
from the intercept. The line broadening due formula [nm] equation [nm]
to lattice strain is proportional to tanθ as per 550 32.06 55.06 53 0.17
the mathematical formulation. 600 32.18 68 77 0.015
From the Williamson–Hall plot (Figure 5) 700 31.72 76.6 82 0.013
more accurate determination of the crystal-
lite size is carried out along with the strain
measurement. The change in the annealing
temperature along with the composition Table 2 Crystallite size and lattice strain for 0.6BFO-0.4NFO at different temperatures (© Mukherjee)
plays a significant role in the strain calcula- Temperature 2θ [degrees] Crystallite size Crystallite size from Lattice strain [%]
tion. The strain developed is possibly due to [°C] from Scherrer’s Williamson-Hall equa-
formula [nm] tion [nm]
the presence of the two phases, their interac-
550 31.64 51 50.2 0.105
tion, growth and others factors. Table 1 and
Table 2 demonstrate comparative crystallite 600 32.02 68 78 0.015
size dimensions comparing between the 700 32.12 77 79.2 0.009
Scherrer’s and Williamson-Hall plots.

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R E SE A R CH A N D D E V ELO PM EN T | Perovsk i te

0.4BFO-0.6NFO 550 4hrs 0.6BFO-0.4NFO 550 4hrs

0.3
0.3
y = -0.207x + 0.276
0.25
0.25 R2 = 0.243
y = -0.348x + 0.263 0.2
0.2
R2 = 0.206
0.15
0.15

βcos θ
βcosθ

0.1
0.1
0.05
0.05
0
0 0 0.1 0.2 0.3 0.4 0.5 0.6
0 0.1 0.2 0.3 0.4 0.5 0.6
sin θ sin θ

0.4BFO-0.6NFO 600 4hrs 0.6BFO-0.4NFO 600 4hrs

0.2125 0.228
0.212 0.226
0.2115 y = -0.208x + 0.203 y = 0.038x + 0.210
0.224
R2 = 0.535 R2 = 0.244
0.211 0.222
βcos θ

0.2105
βcos θ

0.22
0.210 0.218
0.2095 0.216
0.209 0.214
0 0.1 0.2 0.3 0.4 0 0.1 0.2 0.3 0.4
sin θ sin θ

0.4BFO-0.6NFO 700 4hrs 0.6BFO-0.4NFO 700 4hrs

0.182 0.185
0.181 0.184 y = 0.018x + 0.175
R2 = 0.668
0.18 0.183
y = 0.027x + 0.168
0.179 0.182
R = 0.503
2
0.178
0.181
0.177
βcos θ
βcos θ

0.18
0.176
0.175 0.179
0.174 0.178
0.173 0.177
0 0.1 0.2 0.3 0.4 0.5 0 0.1 0.2 0.3 0.4 0.5 0.6
sin θ sin θ
Figure 5 Williamson–Hall plot for BFO-NFO composites of different ratios at three different temperatures for fixed hours of the soaking period (© Mukherjee)

by Soumya Mukherjee et al. on the synthe- different temperatures of 550, 600 and obtained after annealing at 550 °C for 4 h
sized sample of bismuth ferrite-nickel ferrite 700 °C for a 4 h soaking period is shown in were found to be segregated with more
[17, 18]. All these peaks were found in all the Figure 7 to Figure 12. For all cases, agglom- porosity. The agglomerate particle size was
samples, confirming the presence of the eration was noticed with few intercon- estimated to be about 400–500 nm for
BFO-NFO composite. It was observed that nected pores. The agglomerates had an 0.4BFO-0.6NFO composites, while for the
the intensity of the absorptive peaks at 500 irregular polygonal to spade-like shape. 0.6BFO-0.4NFO sample it was about
and 750 cm-1 increases due to an increase in Few grains are noted to have a spherical 400 nm, as shown in Figure 7 and Figure 8.
particle size with an increase in the sintering shape too. The morphology of the synthe- Annealing at 600 °C for 4 h led to samples
temperature from 550 to 700 °C. sized sample was found to be in corre- with an interconnected structure with poros-
The SEM morphology of the synthe- spondence with experimental findings of ity in between the connecting ridges. The
sized samples after heat treatment at three the author in previous articles. Samples agglomerate size was found to be between

46 Interceram 5 | 2019www.interceram-review.info
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R E SE A R CH A N D D E V ELO PM EN T | Perovsk i te

0.4BHO-0.6NFO 550 4hrs 0.4BHO-0.6NFO 700 4hrs

0.40 0.5
0.35
0.4
0.30
0.25 0.3
% Absorbance

% Absorbance
0.20
0.2
0.15
0.10 0.1
0.05
0.0
0.00
-0.05 -0.1
0 1000 2000 3000 4000 5000 0 1000 2000 3000 4000 5000
Wavenumber (cm-1) Wavenumber (cm-1)

0.6BHO-0.4NFO 700 4hrs 0.6BHO-0.4NFO 550 4hrs

0.4 0.4

0.3 0.3
% Absorbance

% Absorbance

0.2 0.2

0.1 0.1

0.0 0.0

-0.1 -0.1
0 1000 2000 3000 4000 5000 0 1000 2000 3000 4000 5000
Wavenumber (cm-1) Wavenumber (cm-1)

Figure 6 FTIR spectroscopy of the bismuth ferrite-nickel ferrite composite of two different molar ratios obtained at two different temperatures of 550 and
700 °C after 4 h of soaking in similar conditions (© Mukherjee)

Figure 7 SEM morphology of 0.4BFO-0.6NFO composites after a 4 h soaking period at 550 °C by a chemical route (© Mukherjee)

600 and 650 nm for both composites, as The morphology was observed to have a slight honeycomb structure in a certain por-
shown in Figure 9 and Figure 10. slight change at about 700 °C, exhibiting a tion of the material matrix with an increase

48 Interceram 5 | 2019www.interceram-review.info
Figure 8 SEM morphology of 0.6BFO-0.4NFO composites after a 4 h soaking period at 550 °C by a chemical route (© Mukherjee)

Figure 9 SEM morphology of 0.4BFO-0.6NFO composites after a 4 h soaking period at 600 °C by a chemical route (© Mukherjee)

Figure 10 SEM morphology of 0.6BFO-0.4NFO composites after a 4 h soaking period at 600 °C by a chemical route (© Mukherjee)

68th Volume  5 | 2019 Interceram 49

R E SE A R CH A N D D E V ELO PM EN T | Perovsk i te

Figure 11 SEM morphology of 0.4BFO-0.6NFO composites after a 4 h soaking period at 700 °C by a chemical route (© Mukherjee)

Figure 12 SEM morphology of 0.6BFO-0.4NFO composites after a 4 h soaking period at 700 °C by a chemical route (© Mukherjee)

in densification for the 0.4 BFO-0.6 NFO O were only noticed by confirming the com- tification by XRD. A Williamson-Hall plot
composites. A valley-like formation with pound formation from phase analysis and was made to note the exact crystallite size
deep impressions was noted. The densest M-O coordination studies carried out by and strain developed for the sample. The
structure morphology was noted for the 0.6 FTIR spectral analysis. Thus, the EDX spec- strain was found to decrease with temper-
BFO-0.4 NFO composites after a 4-h soaking tra of only two samples with the highest ature and spinel phase amount into a com-
period. The particulate size was estimated to annealing temperature are shown for posite matrix, while the perovskite phase
be about 700 nm for both samples. The prob- reference. increased the strain of the composite. M–O
able cause is an increase in atomic diffusion, coordination was noted from FTIR analy-
leading to the formation of a compact struc- sis, showing the intrinsic stretching vibra-
ture with thermal activation acting as the 4. Conclusions tion of the metal at the tetrahedral site to be
driving force. From thermal analyses the crystallization within 620–550 cm-1 and that for the metal
The EDX spectra of all composites exhib- temperature for composite phase develop- at the octahedral site in the range of 450–
ited a similar nature of the elemental peaks ment was noted to be about 426 °C. 385 cm-1. Morphology analysis exhibited an
and show only the elements comprising the Depending on thermal analyses, heat treat- agglomeration with an irregular polygonal
composites. EDX spectra are shown in both ment of precursors was carried at 550, 600 to spade shape along with interconnected
Figure 13 and Figure 14. Peaks of Bi, Fe, Ni, and 700 °C for 4 h, followed by phase iden- pores. EDX confirms the presence of

50 Interceram 5 | 2019www.interceram-review.info
 Bi Spectrum 6

Fe
Element Mass-% Atomic-%
O
OK 16.04 56.15
Fe
Ni Fe K 24.82 24.90
Bi Fe Ni Ni K 4.50 4.30
Bi Ni Bi
Bi M 54.65 14.65

0 1 2 3 4 5 6 7 8 9 10 Total 100
Full Scale 528 cts Cursor: 0.000 keV keV

Figure 13 EDX spectra of 0.6BFO-0.4NFO composites synthesized after annealing at 700 °C for 4 h (© Mukherjee)

Bi Spectrum 3

Element Mass- % Atomic-%

Fe
OK 21.45 61.29
O
Fe Fe K 27.57 22.57

Ni Bi Ni K 8.92 6.94
Bi Fe Ni
Ni Bi
Bi M 42.05 9.20

0 1 2 3 4 5 6 7 8 9 10 Total 100
Full Scale 528 cts Cursor: 0.000 keV keV
Figure 14 EDX spectra of 0.4BFO-0.6NFO composites synthesized after annealing at 700 °C for 4 h (© Mukherjee)

requisite elements required for composite [7] Dong, S., Cheng, J., Li, J.F., Viehland, D.: Enhanced [14] Liao M., Zhong X.L., Wang J.B., Zhou Y.C., Liao H.:
magnetoelectric effects in laminate composites of ­Effects of CoFe2O4 content on the properties of
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