Journal of ELECTRONIC MATERIALS

DOI: 10.1007/s11664-017-5328-9
2017 The Minerals, Metals & Materials Society

Structural, Optical, and Magnetic Properties of Lead-Free

Ferroelectric Bi0.5K0.5TiO3 Solid Solution with BiFeO3 Materials

NGUYEN HOANG TUAN,1 LUONG HUU BAC,2 LE VIET CUONG,3

DUONG VAN THIET,1 TRAN VAN TAM,4 and DANG DUC DUNG1,5

1.Department of General Physics, School of Engieering Physics, Ha Noi University of Science

and Technology, 1 Dai Co Viet street, Ha Noi, Viet Nam. 2.Department of Optics and Opto-
electronics, School of Engieering Physics, Ha Noi University of Science and Technology, 1 Dai Co
Viet street, Ha Noi, Viet Nam. 3.Laboratory for Micro-Nano Technology, University of Engi-
neering and Technology, VNUH, 144 Xuan Thuy street, Ha Noi, Viet Nam. 4.School of Chemical
Engineering, University of Ulsan, Ulsan 680-749, Republic of Korea. 5.e-mail:
dung.dangduc@hust.edu.vn

A solid solution of Bi0.5K0.5TiO3-BiFeO3 was fabricated by a solgel technique.

The pure Bi0.5K0.5TO3 samples exhibited weak room-temperature ferromag-
netism. The room-temperature ferromagnetism was observed in BiFeO3 solid
solution in Bi0.5K0.5TiO3. The optical band gap of Bi0.5K0.5TiO3 was reduced
from 3.22 eV to 1.39 eV with the increase in the amount of BiFeO3 solid
solution. The room-temperature ferromagnetism and band gap reduction were
attributed to the diffusion of BiFeO3 into Bi0.5K0.5TiO3 to form a solid solution.
Our work provided a simple method of realizing room-temperature ferro-
magnetism in lead-free ferroelectric materials.

Key words: Lead-free ferroelectric, Bi0.5K0.5TiO3, solid solution, solgel,

multiferroic

INTRODUCTION Recently, the injection of transition metals into

lead-based ferroelectrics such as Pb(Zr,Ti)O3(PZT)-
The development of multiferroic materials has
based or PbTiO3 materials led to the development of
attracted considerable research interest because of
multiferroic materials based on the current appli-
their several potential applications, including mem-
cation trend of integrating more functional potential
ory devices based on the combination of ferromag-
in lead-based materials. Room-temperature ferro-
netism and ferroelectricity.1 However, a scarcity of
magnetism in PbTiO3 doped with Ni, Mn, Co, and
materials in nature exists given that the conditions
Fe has been reported.811 Natural multiferroic
for being simultaneously ferroelectric and ferromag-
BiFeO3 materials in solid solution with lead-based
netic are difficult to achieve because of the usual
PbTiO3 materials exhibit enhanced magnetodielec-
atomic level mechanism.2 Therefore, obtaining mul-
tric effects. This phenomenon resulted from spin
tiferroic materials at room temperature remains a
phonon interactions.12 The magnetoelectric cou-
major challenge. Four methods can be applied to
pling was also reported in multilayer Terfenol-D/
achieve and develop multiferroic materials: (i)
PZT-based materials or NiFe2O4/PZT bilayer.13
enhancing the performances of natural multiferroic
Lead-based ferroelectric materials have recently
materials, (ii) combining ferromagnetic materials
been restricted in electronic devices because they
with ferroelectric materials as a composite or mul-
contain hazard risks and pollutants (60 wt.% Pb);
tilayer, (iii) introducing the transition metal to
however, lead-based electronic devices are still sold
ferroelectric materials as dopants, and (iv) synthesis
in the market and these materials are still
of multiferroic materials.37
researched in the laboratory. Thus, presently, the
development of multiferroic materials from lead-
free ferroelectric materials is necessary.
Among lead-free ferroelectric materials, bismuth-
(Received October 21, 2016; accepted January 18, 2017) based ferroelectric materials have been significantly

studied because they exhibited strong ferroelectric
properties caused by the stereochemical activity of
the Bi lone electron pair.1417 Among them, the
ferroelectric materials Bi0.5K0.5TiO3 (BKT),
Bi0.5Na0.5TiO3, and Bi0.5(Na,K)0.5TiO3 are widely
studied because of the comparatively strong ferro-
electric properties as compared with PZT-based
materials.18 Therefore, the integration of the ferro-
magnetism in these materials is a candidate for other
functions of electronic devices. Recently, we obtained
room-temperature ferromagnetism in Fe-doped BKT
nanocrystal.19 In addition, our theoretical calcula-
tions predicted that the reduction of band gap is due
to the presence of conduction bands of iron, and the
ferromagnetism in Fe-doped BKT samples resulted
from the exchange splitting between spin sub-bands
through crystal field theory.19 Moreover, we also
reported possible room-temperature ferromagnetism
in Ni-doped lead-free BKT nanocrystal.20 Thus,
realizing room-temperature ferromagnetism in
lead-free ferroelectric materials is a possible method
to achieve environmentally friendly multiferroic
materials.
BiFeO3 is one of the rare multiferroic materials. The
bulk BiFeO3 materials exhibit G-type antiferromag-
netism with the Neel temperature of 650 K, and a
ferroelectric transition of the Curie temperature of
approximately 1103 K.21 The BiFeO3 shows weak
ferromagnetic properties because of the spiral spin
structure with G-type antiferromagnetism. If this
spiral spin structure is suppressed, the weak ferro-
magnetism results from the DzyaloshinskiiMoriya
interaction.2225 The modified BiFeO3 and other lead-
free ferroelectric materials were found to enhance the
magnetism, piezoelectric, ferroelectric, and dielectric
properties. The enhancement of multiferroic proper-
ties and tunable magnetic behavior was exhibited by
the (1 x)BiFeO3-xBi0.5Na0.5TiO3 (x = 00.6) solid
solution.26 The enhancement of the piezoelectric con-
stant was obtained in BiFeO3-modified lead-free
Bi0.5(Na,K)0.5TiO3 materials.27 Morozov et al. reported
that the polarization and strain response of BKT were
enhanced via solid solution with BiFeO3.28 The mul-
tiferroic properties of (1 x)Bi0.5K0.5TiO3 + xBiFeO3
(BKT-xBFO; x = 0.6, 0.7, and 0.8) ceramics was also
investigated.29 However, these studies only focused on
the large range of BiFeO3 solid solution, and the
magnetic properties are only discussed in terms of
modified BiFeO3 by adding BKT.
In this work, the room-temperature ferromagnetism
in BiFeO3 solid solution in BKT materials was
reported. The diamagnetic property competes with
the weak ferromagnetic property in undoped BKT
samples. The ferromagnetic signal was enhanced as
the amount of BiFeO3 contents increased to the final
compensation of ferromagnetic with paramagnetic
properties. The optical band gap energy of samples
decreased from 3.22 eV to 1.39 eV for undoped lead-
free BKT and 30 mol.% BiFeO3 solid solution in BKT,
respectively. The observed room-temperature ferro-
magnetism and reduction of optical band gap energy
Tuan, Bac, Cuong, Van Thiet, Van Tam, and Dung
resulted from the random substitution of Fe3+ ions in
BiFeO3 into the crystal lattice of the host BKT as a solid
solution.
EXPERIMENT
Pure BKT and solid solution (1 x)BKT + xBFO
(x = 5, 10, 15, 20, 25, and 30) samples were synthe-
sized by the solgel technique. The raw materials
used consisted of bismuth nitrate pentahydrate
(Bi(NO3)25H2O), potassium nitrate (KNO3),
tetraisopropoxytitanium (IV) (C12H28O4Ti), and iron
(III) nitrate (Fe(NO3)39H2O). Acetylacetone
(CH3COCH2COCH3) and acetic acid (CH3COOH)
were selected as solvents. First, bismuth nitrate
pentahydrate and potassium nitrate were dissolved
in acetic acid and distilled water. After stirring
vigorously for 1 h, a transparent homogeneous sol
was formed. Then, acetylacetone was introduced
into a prepared solution after adding tetraiso-
propoxytitanium (IV). After stirring vigorously for
2 h, a thin yellow homogeneous sol was formed.
Then, iron(III) nitrate was added. The solutions
were stirred for approximately 45 h at room tem-
perature. Then, the sol was heated at 100C to
prepare dry gels. The dry gels were ground and
calcined at 400C for 2 h and sintered at 800C for
3 h. Potassium was added to excess at approxi-
mately 10 mol.% to prevent potassium loss during
the gel and sintering processes. The crystalline
structures of the samples were characterized by
x-ray diffraction (XRD). The vibrational and rota-
tional modes in samples were characterized by
Raman spectroscopy. The optical properties were
studied by ultravioletvisible (UVVis) spec-
troscopy. The magnetic properties were character-
ized by using vibration sample magnetometer at
room temperature.
RESULTS AND DISCUSSION
Figure 1a shows the XRD patterns of pure BKT
and BKT-xBFO as solid solution at room tempera-
ture. The peaks were indexed as the tetragonal
structure of BKT phase for all samples, indicating
that BiFeO3 materials were well-dissolved in BKT
materials to form a single phase, which was fol-
lowed by the crystal structure of host BKT materi-
als. The impurity phase could not be detected
through XRD measurement. An enlarged compar-
ison of the location of (110) diffraction peaks in the
range of 30 to 35 show that the peak positions of
the samples slightly shifts toward lower 2h values
as the BiFeO3 amount is increased, as shown in
Fig. 1b. The result indicated that the lattice param-
eter of the samples tends to expand with the
increase in the amount of BiFeO3 solute in the
BKT solution. If we considered the HumeRothery
rules,30 then Bi3+ and Fe3+ ions of BiFeO3 materials
may prefer random distribution to the lattice site of
the host BKT structure, where the Bi3+ tended to
Structural, Optical, and Magnetic Properties of Lead-Free Ferroelectric Bi0.5K0.5TiO3 Solid
Solution with BiFeO3 Materials

Fig. 1. (a) XRD patterns of pure BKT and BKT-xBFO solid solution with various BiFeO3 concentrations; and (b) the magnification of XRD peaks
in the range of 30 to 35 of pure BKT and BKT-xBFO with various BiFeO3 concentrations.

Fig. 2. (a) Surface morphology images of pure BKT and of BKT-xBFO materials: (b) 5 mol.%, (c) 10 mol.%, (d) 15 mol.%, (e) 20 mol.%, (f)
25 mol.%, and (g) 30 mol.%.

randomly substitute at the A site (Bi or K site) of the
BKT structure and Fe3+ preferred to randomly
substitute at the Ti4+ site to form single-phase
materials. Note that the ionic radius with six-fold
coordination of Ti4+ (0.061 nm) is smaller than that
of Fe3+ (0.064 nm).31 Thus, the use of Fe3+ ions as
substrate at the Ti site resulted in the expansion of
lattice parameters as observed in XRD diffraction.
The result was consistent with recent observation in
lattice distortion in Fe-doped BKT or Bi0.5Na0.5TiO3
materials.19,32 In other words, the single-phase
BiFeO3 solid solution in BKT materials, following
the crystal structure of BKT, was well-prepared by
the solgel method.
Figure 2a shows the surface morphology of
undoped BKT samples. The undoped BKT samples
exhibited a grain size of approximately 30 nm which
was consistent with our recent observation.33 The
surface morphology changed when BiFeO3 solute in
BKT formed a solid solution. Figure 2bf shows the
surface morphology of BKT-xBFO with concentra-
tions of BiFeO3 materials of 5 mol.%, 10 mol.%,
15 mol.%, 20 mol.%, 25 mol.%, and 30 mol.%. The
grain sizes increased by approximately 100200 nm
as the concentration of BiFeO3 increased. Zhou
et al. reported that the grain size of Bi0.5Na0.5TiO3-
BKT materials increased by the addition of
BiFeO3.34 Given the presence of oxygen vacancies
in the oxide systems, as Fe3+ ions enter into the six-
fold coordinator B site of the perovskite structure to
substitute for Ti4+, mass transport during sintering
is beneficial.34 Thus, we suggested that the
increased grain size in the case of BiFeO3 solid
solution in BKT results from oxygen vacancies
promoting grain growth.
Figure 3a shows room-temperature Raman spec-
tra of pure BKT and BKT-xBFO as solid solution
with various concentrations. The Raman bands for
pure BKT and BKT-xBFO samples are relatively
broad because of the disorder on the A site and from
 Tuan, Bac, Cuong, Van Thiet, Van Tam, and Dung

Fig. 3. (a) Room-temperature Raman spectra of pure BKT and BKT-xBFO with various BiFeO3 concentrations, (b) The magnification of Raman
spectroscopy in the range of 150450 cm 1 of pure BKT and BKT-xBFO with various BiFeO3 concentrations.

Fig. 4. (a) UVVis absorption spectra and (b) the dependence of (ahm)2 on hm of pure BKT and BKT-xBFO with various BiFeO3 concentration.
The inset in Fig. 4(b) shows the optical band gap values as a function of the BiFeO3 amount.

overlapping Raman modes, making it difficult to
distinguish from different modes. The BKT materi-
als fabricated by the solgel technique shows six
scattering modes, located at roughly 150 cm 1,
201 cm 1, 276 cm 1, 332 cm 1, 529 cm 1, and
633 cm 1, where the low-frequency band is associ-
ated with the KO bonds, whereas the higher-
frequency bands could probably be assigned to
vibrations of the TiO6 octahedral.35 Moreover, Hou
et al. pointed out that a weak band at 157 cm 1 is
associated with the KO vibrations, whereas the
strong band centered on 284 cm 1 (of A1 symmetry
and assigned to a TiO6 octahedra) is the dominating
feature in the BKT Raman spectrum, and the high-
frequency bands of BKT at 523 cm 1, 632 cm 1, and
827 cm 1 were assigned to vibrations of the TiO6
octahedra.36 In addition, the high-frequency Raman
bands in oxides are dominated by vibrations involv-
ing mainly oxygen displacements and can often be
interpreted in terms of polyhedral vibrations.36
However, a BiO bond would be located at very
low frequencies and was not observed in our exper-
imental conditions because of the high mass of the
bismuth atom.3537 The role of lattice vibration of
BiFeO3 solid solution in BKT samples are shown in
the magnification of Raman spectroscopy in the
range of 150450 cm 1, as shown in Fig. 3b. In
addition, the appearance of a left-shifted shoulder in
the 260 cm 1 and 350 cm 1 peaks are related to
an increase in the distortion of the TiO6(FeO6)
octahedral with an increase in Fe concentration.
The decrease of the ionic radii, when Fe ions
substituted for Ti ions, naturally leads to distortion
of the structural framework, and polyhedron distor-
tion in oxides is known to result in a low-frequency
shift.37 The results were in agreement with the
recently reported effect of lattice vibration in ferro-
electric materials caused by the transition metal
defect in lead-based ferroelectric PbTiO3 materi-
als.811 Our results were also consistent with a
recent report for Bi0.5Na0.5TiO3 solid solution with
BiCrO3.38
Structural, Optical, and Magnetic Properties of Lead-Free Ferroelectric Bi0.5K0.5TiO3 Solid
Solution with BiFeO3 Materials
Figure 4a shows the optical absorption spectra of
undoped BKT and BKT-xBFO solid solution samples
with various BiFeO3 concentrations. The undoped
BKT samples show the single-band absorbance while
the complex band absorbance was obtained for BKT-
xBFO samples. The appearance of absorbance peaks
at approximately 485 nm in BKT-xBFO samples was
suggested for Fe3+ local states, which resulted from
Fe3+ ions preferring to substitute at the Ti site of the
host BKT lattice during solid solution formation. The
appearance of local-state Fe3+ in BKT-xBFO samples
was consistent with a recent study on Fe-doped BKT
materials.19 However, single Fe3+ ions were unlikely
substituted at the Ti site in the BKT crystal struc-
ture; two board absorbance bands in the range of
approximately 6001200 nm were obtained in
BiFeO3 solid solution in BKT samples. Both experi-
mental and theoretical investigations predicted that
the BiFeO3 samples exhibited major absorption from
approximately 2.50 eV to 2.81 eV, corresponding to
the energy gap, and the minor absorption begins at
1.18 eV resulting from the FeO6 octahedral of the d
orbital of Fe splitting into three-fold degenerate t2g
and e.g. bands.19,39,40 In addition, Liu et al. pointed
out that the minor absorption occurs when the
electron is excited from the t2g band to the e.g. band.39
Thus, we suggested that the present BiFeO3 phase as
solid solution in BKT changed the band structure
resulting from the present exchange splitting of Fe
under a crystal field. Clearly, the solid solution of
BiFeO3 into BKT results in its band gap red shift,
indicating that the optical band gap (Eg) was reduced.
The effect of BiFeO3 solid solution in BKT samples on
the band gap was further calculated using the plot of
(ahm)2 versus photon energy hm, as shown in Fig. 4b,
where a, h, and m are absorbance coefficient, the
Planck constant, and the frequency, respectively.
The inset of Fig. 4b shows the band gap values as a
function of BiFeO3 amount. The optical band gap is
3.31 eV for pure BKT and was decreased to 1.93 eV
for 30 mol.% BiFeO3 solid solution in BKT. The
reduction of the optical band gap was suggested by
the substitution of Fe ions at the Ti site in a BKT
crystal structure in BKT-xBFO materials. The reduc-
tion of optical band gap energy was also recently
obtained in single-transition elements such as Fe-
and Ni-doped BKT or Mn-doped Bi0.5Na0.5TiO3 mate-
rials.19,20,41 Recently, a theoretical prediction was
formulated stating that the substitution transition
ions at the Ti site in BKT or Bi0.5Na0.5TiO3 results in
the reduction of the band gap caused by the presence
of conduction bands in the majority spin state.19,42
The intrinsic defect and/or surface defect influencing
the optical band gap was observed in BKT.33 The
difference between Fe3+ state and Ti4+ state created
the oxygen vacancies which also possibly affects the
optical band gap energy caused by the presence of a
local state near the conduction band.43 Thus, we
suggested that the reduction of optical band gap in
BKT-xBFO originated from the presence of a local
defect, with oxygen vacancies caused by the
unbalanced charge of Fe3+ ion dopants with Ti4+ ions
contributing to the phenomenon.
Furthermore, the effect of BiFeO3 solid solution
BKT materials on the magnetic properties was
observed by determining the magnetic moment ver-
sus magnetic field at room temperature. Figure 5
shows the magnetic hysteresis (M-H) loops of the
pure BKT and BKT-xBFO samples at room temper-
atures. The hysteresis loop with an anti-S shape is
observed for BKT samples. The inset of Fig. 5 shows
the M-H loops of pure BKT samples after subtracting
the diamagnetic component. Thus, the magnetism of
undoped BKT samples are a competition between
ferromagnetism and diamagnetism. The origin of
weak ferromagnetism in BKT is still unknown. The
diamagnetic nature of BKT provided the evidence of a
Ti4+ state with a d0 electron, which was similar to the
behavior recently observed for Ti-based perovkiste
materials such as BaTiO3 or Bi0.5Na0.5TiO3.19,33,41,44
Recently, the theoretical calculation for various
perovskite materials, such as Bi0.5Na0.5TiO3,
PbTiO3, BaTiO3 , or SrTiO3 was predicted to be
observed in the ferromagnetism of those materials
resulting from a self-defect such as Ti or O vacan-
cies.4548 In addition, the experimental results also
demonstrated that the non-magnetic nanosized
oxides were ferromagnetic, resulting from the
exchange interactions between localized electron
spin moments and oxygen vacancies at the surface
of the nanoparticles.49 We recently reported that the
self-defect and/or surface effect of BKT nanoparticle
possibly influences the band structure.33 Thus, we
suggested that the weak room-temperature ferro-
magnetism in BKT nanoparticle resulted from the
influence of a self-defect and/or surface effect.
Interestingly, the anti-S shape of pure BKT
samples changed to an S shape which was obtained
in BKT-xBFO solid solution. The result indicated
Fig. 5. Magnetic hysteresis (M-H) loops of the BKT and BiFeO3 solid
solution in BKT samples at room temperature. The inset in Fig. 5
shows the M-H curves of pure BKT nanocrystal after the diamagnetic
component substrate.

that the ferromagnetism of BKT-xBFO samples was
strongly enhanced. The coercive field (HC) and
remanence magnetization (Mr) were estimated to
be approximately 100 Oe and 0.8 memu/g, respec-
tively, which confirm the typical ferromagnetism
even at room temperature. The HC value of BKT-
xBFO samples was consistent with previously
reported values for transition metal-doped ferro-
electric materials such as HC100 and 80 Oe for Fe-
and Mn-doped Na0.5Bi0.5TiO3, respectively.32,41 The
results were also consistent with previously
reported studies for HC values of Fe- and Ni-doped
BKT whose values are approximately 70 Oe and
120 Oe, respectively.19,20 However, the M-H curves
of BKT-xBFO samples did not show the saturation
at a high magnetic applied field which was sug-
gested to contribute to the paramagnetic and/or
antiferromagnetic components. Note that the crys-
tal structure of BKT-xBFO followed the BKT struc-
ture, which resulted from the random distribution
of Bi3+ and Fe3+ ions of BiFeO3 diffused to the host
lattice of BKT to form a solid solution. Thus, the
isolated Fe3+ ions contributed to the paramagnetic
component to magnetization of samples. In addition,
the oxygen vacancies (h) were caused by the
unbalance charge between Fe3+ and Ti4+, resulting
in interaction of Fe3+ ions with Fe3+ through oxygen
vacancies like Fe3+-h-Fe3+, called the F center,
which was proposed by Coey et al.50 The interaction
exchange between two Fe3+ ions via the F center,
where the F center is similarly bound to a magnetic
polaron, leads to ferromagnetic coupling.50,51 Thus,
Fe3+-h-Fe3+ superexchange interaction will be anti-
ferromagnetic in nature, which is also the origin of
unsaturation magnetization at the applied high
magnetic field. Thus, we suggested that the
enhanced room-temperature ferromagnetism of
BKT-xBFO, compared with undoped BKT materi-
als, resulted from the interaction of Fe3+ through
oxygen vacancies caused by the random distribution
of Fe3+ cations in the host lattice structure of BKT,
and the magnetization was possibly contributed
from both self-defect and surface effects.
CONCLUSION
The ferromagnetic properties of lead-free ferro-
electric BKT materials were improved via solid
solution with BiFeO3. The optical band gap of
undoped BKT materials reduced from 3.22 eV to
1.39 eV for 30 mol.% BiFeO3 solid solution in BKT
materials. The undoped BKT samples exhibited
weak room-temperature ferromagnetism because
of the competition between ferromagnetism and
diamagnetism resulting from self-defect and/or sur-
face effect. Room-temperature ferromagnetism was
achieved in BKT-xBFO, resulting in the competition
between ferromagnetism and paramagnetism
caused by the interaction between two Fe3+ ions
through oxygen vacancies and isolated random
Fe3+in the host lattice structure of BKT. We expect
Tuan, Bac, Cuong, Van Thiet, Van Tam, and Dung
our work to provide a simple method to obtain room-
temperature ferromagnetism in the integration of
more functional lead-free ferroelectric materials.
ACKNOWLEDGEMENTS
This research was funded by the basic research of
Hanoi University of Science and Technology under
Code T2016-PC-222.
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Structural, Optical, and Magnetic Properties of Lead-Free Ferroelectric Bi0.5K0.5TiO3 Solid
Solution with BiFeO3 Materials
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