Journal of Alloys and Compounds 546 (2013) 57–62

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Journal of Alloys and Compounds

journal homepage: www.elsevier.com/locate/jalcom

Effect of La3+ substitution on the phase transitions, microstructure

and electrical properties of Bi1xLaxFeO3 ceramics
Qiang Zhang, Xiaohong Zhu ⇑, Yunhui Xu, Haobin Gao, Yunjun Xiao, Dayun Liang,
Jiliang Zhu, Jianguo Zhu, Dingquan Xiao
Department of Materials Science, Sichuan University, Chengdu 610064, China

a r t i c l e i n f o a b s t r a c t

Article history: Multiferroic Bi1xLaxFeO3 (x = 0.00, 0.05, 0.10, 0.15, 0.20) (represented as B1xLxFO) ceramics were pre-
Received 25 June 2012 pared using the conventional solid state reaction route. The effects of La3+ doping on the density, phase
Received in revised form 14 August 2012 structure, morphology, dielectric and ferroelectric properties were investigated. Judging from X-ray dif-
Accepted 17 August 2012
fraction patterns, all the B1xLxFO ceramic samples were well crystallized in a pure perovskite phase
Available online 25 August 2012
while the crystal structure changed from rhombohedral to orthorhombic with increasing the La3+ substi-
tution. SEM observations clearly revealed that the grain size was remarkably decreased by La3+ doping. As
Keywords:
a result, the ferroelectric Curie temperature was lowered in the La-doped ceramics. However, the abnor-
La3+ doping
Bi1xLaxFeO3 ceramics
mal dielectric responses near the antiferromagnetic Néel temperature (TN) demonstrated the existence of
Multiferroics remarkable magnetoelectric coupling in the Bi1xLaxFeO3 ceramics, and the TN was shown to increase
Phase transition substantially with the increase in La3+ doping content. It was found that the dielectric permittivity of
Microstructure the ceramics was significantly increased and the dielectric loss was slightly increased with the increase
Electrical properties in La3+ content. The dielectric constant er of the Bi0.85La0.15FeO3 ceramic at 10 kHz reached as high as
1008, 20 times larger than that for pure BiFeO3. In addition, the ferroelectric properties of the B1xLxFO
ceramics were improved and the remanent polarization was increased by La3+ doping. This is probably
because the A-site doping with more stable La3+ could reduce the volatilization of Bi3+ and, thus, reduce
 0
the concentration of charged defects or defect dipole complexes, such as V O , V 000 000
Bi or ðV Bi  V O Þ in the
ceramics.
Ó 2012 Elsevier B.V. All rights reserved.

1. Introduction ration of phase pure BFO is reported to be difficult due to the

Multiferroic materials show simultaneously two or more re-
sponses among ferroelectric, (anti)ferromagnetic and ferroelastic
properties due mainly to the coupling between ferroelectric and
magnetic orders [1]. They have attracted much attention in recent
years because of their potential for new device applications in mul-
tiple state memory elements, electric field controlled ferromag-
netic resonance devices, and transducers with magnetically
modulated piezoelectricity [2–4]. The main multiferroic oxide
compounds are BiFeO3 (BFO), BiMnO3 (BMO) and ReMnO3
(Re = Y, Ho, Lu), etc. Among them, BiFeO3 is a multiferroic material
with a rhombohedrally distorted perovskite structure (space group
R3c) [5]. Its phase transition temperatures are high (TN = 640 K and
TC = 1100 K), which makes it very attractive from an application
point of view.
The BiFeO3 ceramics can be fabricated at various sintering tem-
peratures by a conventional solid-state reaction. However, prepa-
⇑ Corresponding author.
E-mail address: xhzhu@scu.edu.cn (X. Zhu).
volatilization of some reactants and phase decompositions at high
temperature and narrow temperature range of BiFeO3 phase for-
mation. Moreover, a large leakage current density is caused by
charge defects, non-stoichiometry and second phases in BFO
ceramics, which makes it difficult to gain a well-saturated ferro-
electric hysteresis loop and a low dielectric loss and thus hinders
its practical applications [6–8].
To improve the electrical properties of the BFO, several research
groups have attempted to dope with +3 valence lanthanide ions of
La3+ and Sm3+ as well as transition metal ions of Mn4+, Ti4+ and
Nb5+ at different sites of BFO [8–10]. The doping has resulted in
the reduction in the leakage current density and the improvement
in ferroelectric properties of BFO to some extent. It has been ob-
served that below 10% La doping in Bi1xLaxFeO3 ceramics main-
tains the rhombohedral structure; however, for 20% and 30% La
doping, the structures change to the orthorhombic and tetragonal,
respectively [11]. It is noticed that La doping significantly enhances
the ferromagnetic moment and reduces electric leakage due to the
broken cycloid spin structure caused by the changes in the crystal-
line structure [12]. In addition, Ho doping at A site in BiFeO3 re-

0925-8388/$ - see front matter Ó 2012 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.jallcom.2012.08.067
58 Q. Zhang et al. / Journal of Alloys and Compounds 546 (2013) 57–62
duces the leakage current, enhances the ferroelectric switching
characteristic, and explains the stereochemical activity of Bi lone
pairs [13,14]. It has been observed that in Sm doped BiFeO3 the
spiral spin modulation peculiar to pure BiFeO3 was suppressed in
the orthorhombic phase, leading to the weak ferromagnetic prop-
erties [15]. The Sr doping at A site results in oxygen non-stoichiom-
etry and with the increase in Sr concentration SrFeO3 phase is
accompanied by decrease in magnetization [16]. Similar behavior
has also been observed in Ca, Ba doped BiFeO3 samples without
any enhancement in magnetization [17]. It is generally accepted
that the perovskite phase can be stabilized and the electrical prop-
erties can be enhanced in BiFeO3 ceramics by adding various do-
pants, like Er3+, La3+, Sm3+, Nb5+ and so on, because their radii are
similar, and they stabilize the perovskite phase that helps to de-
crease Bi3+ volatilization and the number of oxygen vacancies
[18,19]. Although a great deal of work has been devoted to doped
BFO, there are very few reports on systematic investigation of
phase transitions, microstructure and electrical properties in La
doped BFO ceramics. Especially, the effects of La3+ doping on the
ferroelectric and antiferromagnetic phase transitions, temperature
dependent dielectric responses and magnetoelectric coupling of
BFO ceramics still lack consistency and are not fully understood
[20–22].
In the present work, we explored the phase evolution, micro-
structure development and density variation of Bi1xLaxFeO3
(BLFO) ceramics. Moreover, a systematic study has been carried
out on the dielectric, ferroelectric and magnetoelectric coupling
properties of La doped BiFeO3 ceramics.
2. Experimental details
Samples of Bi1xLaxFeO3 (x = 0.00, 0.05, 0.10, 0.15, 0.20) were prepared by the
conventional solid state reaction method. High purity Bi2O3 (99.99%), Fe2O3
(99.99%) and La2O3 (99.99%) were carefully weighed in stoichiometric proportions
and thoroughly mixed for about 5 to 6 h using high purity isopropyl alcohol as a
medium. The resulting power was preheated at 700 °C for 2 h using a furnace,
the temperature of which can be controlled to an accuracy of ±1 °C. The calcined
material was once again ground thoroughly prior to pressing and sintering at
850 °C for 2 h. The samples were thinned down to 1.5 mm thick, and high temper-
ature silver paste was applied on their two major surfaces as electrodes for electri-
cal measurements. The X-ray diffraction pattern of the samples was recorded at
room temperature using X-ray power diffractometer with CuKa radiation
(k = 0.154178 nm) in a wide range of Bragg angles 2h (20–80°) at a scanning rate
of 2°/min. The microstructure and surface morphology were characterized by scan-
ning electron microscopy (JEOL JSM-5900LV). The heat flow versus temperature
curve was determined using a differential thermal analyzer (DTA) (Netzsch
STA449C Jupiter). Dielectric constant and the loss tangent measurements were car-
Fig. 1. X-ray diffraction (XRD) patterns for the Bi1xLaxFeO3 (x = 0.00–0.20) ceramics.
ried out in the frequency range from 100 Hz to 1 MHz by using an impedance ana-
lyzer (HP4294A). The hysteresis loops of polarization (P) as a function of applied
electric field (E) (P–E loops) were determined using a Radiant Precision Ferroelectric
Measurement System (RT2000 Tester, USA).
3. Results and discussion
3.1. Structural analysis
BiFeO3 is known to possess a rhombohedrally distorted perov-
skite structure described by the space group R3c [23]. The room-
temperature XRD patterns of the La doped BiFeO3 ceramics sin-
tered at 850 °C for 2 h in air atmosphere are shown in Fig. 1. All
the diffraction peaks of BiFeO3 were indexed. All doped specimens
exhibit a perovskite structure, but there is a small amount of sec-
ond phase in the pure BFO sample. It has been reported that impu-
rity phases are usually formed along with a BiFeO3 phase in the
solid state reaction process [24]. These phases were identified
mainly as Fe-rich Bi2Fe4O9 phase. It is observed here that doping
with La eliminated the second phase impurity, indicating that the
addition of La3+ ions can hinder the formation of a second phase
[25]. More importantly, it is found that the structure is rhombohe-
dral for x 6 0.10 and orthorhombic for x P 0.15 of B1xLxFO ceram-
ics. Detailed analysis of the XRD patterns reveals the structural
modifications with the increase in La content. XRD peaks (0 0 6),
(2 0 2) and (1 1 3) at about 2h = 39° become broad and the (1 1 3) al-
most disappears at x = 0.20. Besides, the intensity of the (1 0 4) and
(1 1 0) peaks in BLFO ceramics becomes weak and the splitting of
these peaks around 2h = 32° decreases, indicating a reduction in
the rhombohedral phase. The change from rhombohedral to ortho-
rhombic symmetry is almost complete near x = 0.20.
3.2. SEM analysis
The surface morphologies of the Bi1xLaxFeO3 ceramics sintered
at 850 °C for 2 h are shown in Fig. 2. It can be seen from the figure
that the microstructure is homogeneous and few distinct pores ex-
ist in the grain boundary for all samples with the average grain size
of 2.0–5.0 lm. Pure BFO has relatively large grains whereas La
doped BFO exhibited dense structure with small grain size. On
the other hand, it is shown in Fig. 2(b–e) that as the La content is
increased, the average grain size is remarkably reduced for the La
doped BFO ceramics, showing a dense and uniform distribution
of grain sizes with lower density of pores. All the doped pellets
 Q. Zhang et al. / Journal of Alloys and Compounds 546 (2013) 57–62 59

Fig. 2. SEM micrographs of the Bi1xLaxFeO3 (x = 0.00–0.20) ceramics with (a) BLFOx=0.00, (b) BLFOx=0.05, (c) BLFOx=0.10, (d) BLFOx=0.15, (e) BLFOx=0.20 sintered at 850 °C for 2 h.

have a relatively high density around 95%. Obviously this solid
phase sintering technique used in this work has positive effects
on densification. However, it is still a great challenge to prepare
undoped BFO ceramics with high purity phase and high density
[26]. Rare earth ions are known to suppress the grain growth in
perovskite, which is probably attributed to their lower diffusivity
[27]. Therefore, open porosity could not be observed easily and
the microstructure with well-grown grains is more homogenous
for the La doped ceramics, especially in the case of 15% doping,
and thus the doped ceramics have a higher density.
3.3. Thermal analysis
Fig. 3 shows the DTA curves for the Bi1xLaxFeO3 (x = 0.00–0.10)
power samples during the heating process by primarily focusing on
the temperature range from 650 to 900 °C. The existence of ferro-
electricity and the corresponding Curie temperature (TC) for these
samples were determined using DTA. For the sake of clarity a base
line is subtracted from the data and the resulting data are plotted.
Endothermic peaks signifying the first-order phase transition could
be identified in the heating cycle. The transition revealed by the

Fig. 3. DTA measurements for the Bi1xLaxFeO3 (x = 0.00–0.10) power samples.

60 Q. Zhang et al. / Journal of Alloys and Compounds 546 (2013) 57–62
Fig. 4. Variations of dielectric constant (a) and loss tangent (b) of the Bi1xLaxFeO3
(x = 0.00–0.20) ceramics as a function of frequency at room temperature.
plots is the ferroelectric – paraelectric phase transition tempera-
ture TC. The value is obtained to be 829.1 °C for x = 0.00 (pure
BFO), which matches well with the reported value 830 °C for pure
BiFeO3 [28]. As the doping contents of La increase, the TC changes
significantly from 818.1 °C (x = 0.05) to 812.7 °C (x = 0.10). The de-
crease in TC of La substituted BFO may be attributed to site disorder
and structural deflection generated due to substitution. It is usually
expected that A-site doping is responsible for the modified ferro-
electric behavior and B-site substitution causes the magnetic
ordering in BFO [29]. Such a TC shift observation gives further evi-
dence that the enhanced ferroelectricity seen later for BLFO sam-
ples is not due to any impurity phase formed, but due to changes
in the internal structure of the basic BFO formation.
3.4. Dielectric analysis
Fig. 4 shows the dielectric constant (er) and loss tangent (tan d)
of the Bi1xLaxFeO3 as a function of frequency for those five sam-
ples at room temperature. For all the samples investigated, a
smooth curve has been obtained. In BFO, low-frequency dispersion
in both er and tand spectra indicates the presence of dc conductiv-
ity [30,31]. The room temperature er values at 100 kHz of the sam-
ples are, respectively, 80 (x = 0.00), 225 (x = 0.05), 105 (x = 0.10),
560 (x = 0.15) and 100 (x = 0.20), indicating that La3+ substitution
is indeed helpful in improving the dielectric properties of BFO
ceramics. The dielectric constant for all the samples decreases with
increasing frequency, as can be expected from a conventional
dielectric relaxation process. It can be seen that doping with La in-
creases the dielectric constant of BiFeO3, which reaches a maxi-
mum at a La content x = 0.15. As a result, the dielectric constant
er of the Bi0.85La0.15FeO3 ceramic at 10 kHz reaches as high as
1008, 20 times larger than that for pure BiFeO3. It is believed that
the occurrence of crystal structure change from rhombohedral to
orthorhombic and the increased density in the Bi1xLaxFeO3 ceram-
ics are helpful in improving their dielectric properties. The ceramic
at x = 0.15 has a nearly orthorhombic structure and the highest
density, thus giving rise to the maximum dielectric constant. Sim-
ilar to the dielectric constant, the dielectric loss also decreases
smoothly with increasing frequency, which is consistent with the
results reported by Pradhan et al. [6]. It can be seen that doping
with La also increases the dielectric loss of BiFeO3, which reaches
a maximum at a La content x = 0.15. Nonetheless, it is worth men-
tioning that both er and tan d are rather stable over the relatively
high frequency range investigated, particularly in the frequency
range between 500 and 1000 kHz.
Fig. 5 shows the variations of the dielectric constant (er) and loss
tangent (tan d) with the temperature at 10 kHz for the Bi1xLaxFeO3
ceramics. The relatively high resistivity and controlled leakage cur-
rent in La-substituted BiFeO3 allowed er and tan d to be determined.
Here, the dielectric constant of the Bi1xLaxFeO3 ceramics increases
significantly with an increase in temperature up to 350 °C. The typ-
ical dielectric constant and loss tangent at 10 kHz for x = 0.15,
x = 0.20 are 1200, 1188 and 0.03, 0.04, respectively, and those for
x = 0.05, x = 0.10 are comparatively lower. These values obtained
are comparable to those reported for doped BiFeO3-based materi-
als. Moreover, the increase in dielectric constant up to 350 °C is
not related to the ferroelectric transition, since the ferroelectric-
paraelectric phase transition temperature is much higher
(TC = 830 °C) [12], but related to the antiferromagnetic Néel tem-
perature (TN). It can be deduced from Fig. 5 that the TN increases
substantially with the increase in La doping content. These anom-
alies in the dielectric constant and loss tangent as a function of
temperature observed near the TN demonstrate the existence of
remarkable magnetoelectric coupling in the Bi1xLaxFeO3 ceramics
[20,32]. It is suggested that the structural modification from rhom-
bohedral to orthorhombic caused by La3+ doping destructs the spin
cycloid of BiFeO3, and thus enhances the magnetic and magneto-
electric coupling properties [12,33,34]. It is noteworthy that the
dielectric loss is still high for Bi1xLaxFeO3 ceramics, which may
be due to space charge polarization present in ceramics at high
temperature and low frequency [35]. In addition, an important
contribution to the losses is given in bulk ceramics by other types
of defects associated to the grain boundaries, resulting in a com-
plex impedance behavior [36].
3.5. P–E analysis
Fig. 6 shows the room-temperature polarization versus elec-
tric field ferroelectric hysteresis loops (P–E loops) for the Bi1x-
LaxFeO3 (x = 0.05–0.20) ceramics, measured at a frequency of
50 Hz. It is known that BFO is a hard material and hence the
P–E curves get constricted. We never really approach full satura-
tion so that the polarization values generally remain low and the
curves that we observed are obtained only in the sub-coercive
field region. It is also known that well saturated ferroelectric
loops in pure BFO are difficult to obtain due to the high coercive
field and high leakage currents. And the high leakage of BFO is
known to be attributed to the existence of oxygen vacancies
and Fe2+, both of which can form impurity phase in the band
gap of BFO [37]. Recently, oxygen vacancies rather than Fe2+, is
found to make more contribution towards the high leakage cur-
rents, which could dramatically decrease the breakdown voltage
[38,39]. In our case, the shape of P–E loops of the BLFO ceramics
is improved due to La doping. Furthermore, a rectangular-like
loop with relatively large 2Pr is observed in the Bi1xLaxFeO3
(x = 0.05–0.20) ceramics. The remanent polarization and coercive
field for the Bi1xLaxFeO3 (x = 0.050.20) ceramics are 1.98, 2.02,
 Q. Zhang et al. / Journal of Alloys and Compounds 546 (2013) 57–62 61

Fig. 5. Variations of dielectric constant (a) and loss tangent (b) of the Bi1xLaxFeO3 (x = 0.05–0.20) ceramics as a function of temperature at 10 kHz.

Fig. 6. Polarization versus electric field ferroelectric hysteresis loops (P–E) for Bi1xLaxFeO3 (x = 0.05–0.20) ceramics at room temperature.

2.04, 2.20 lC/cm2 and 2.88, 2.95, 3.02, 5.08 kV/cm, respectively.
However, the observed polarization value is much smaller than
the reported values similarly without saturation [40], which
might be attributed to different applied voltage and difference
in lattice distortion by different doping elements. In this case,
the ferroelectric behavior starts to become less clear because
the electrical response is dominated by the conduction effects.
The effects of La doping on BFO is to increase the spontaneous
and residual polarization of the system [41]. Partially saturated
P–E loop could be observed for La doped BFO (x = 0.15–0.20).
However, during the measurement, application of higher fields
was restricted due to conductivity of the samples [42].
Experiments are in progress to improve further the density of
the sample so as to reduce greatly the conductivity.
62 Q. Zhang et al. / Journal of Alloys and Compounds 546 (2013) 57–62
4. Conclusions
In summary, the Bi1xLaxFeO3 (x = 0.00–0.20) ceramics were
prepared by a rapid solid state reaction method. XRD patterns indi-
cated that all the ceramics had stable perovskite structure, and
with the increase of La doping contents the crystal structure
started to change from rhombohedral to orthorhombic. SEM obser-
vations indicated that all the samples had relatively good compact-
ness, few distinct pores and the average grain size of 2.0–5.0 lm. A
reduction of the ferroelectric Curie temperature TC has been ob-
served in the La doped samples in comparison to the pure BiFeO3.
The abnormal dielectric responses observed near the antiferromag-
netic Néel temperature (TN) demonstrate the existence of remark-
able magnetoelectric coupling in Bi1xLaxFeO3 ceramics, and the TN
is confirmed to increase substantially with the increase in La dop-
ing content. The electrical properties could be improved by the La
addition and larger dielectric constant is observed for La-doped
samples. Moreover, La3+ substitution in BFO helps in the formation
of single phase, reduces the volatilization of Bi3+, improves the
dipolar ordering, and reduces the concentration of charged defects,
thereby enhancing the ferroelectric properties. Based on these re-
sults, we conclude that La3+ is a potential candidate to be substi-
tuted in BFO multiferroic material systems, which certainly helps
to enhance multiferroic properties and possible multifunctional
applications.
Acknowledgments
The authors acknowledge the financial support from the Na-
tional Natural Science Foundation of China (Grant No. 61071017),
the Program for New Century Excellent Talents in University of
China (Grant No. NCET-10-0582), the Doctoral Fund of the Ministry
of Education of China (Grant No. 20100181120021), the Fund for
Returnees to Launch S&T Researches by Ministry of Education of
China (Grant No. 20111568-8-8), the Program for Outstanding
Young Scientific and Technological Leader of Sichuan Province
(Grant No. 2011JQ0021), and the Program for Distinguished Young
Scholar of Sichuan University (Grant No. 2011SCU04A05).
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