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Synthesis and Characterization of MgO- doped SrTiO3 Ceramics

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Journal of The Australian Ceramic Society Volume 52[1], 2016, 95 – 101 95

Synthesis and Characterization of MgO- doped SrTiO3

Ceramics
K. Chandra Babu Naidu*, T. Sofi Sarmash, M. Maddaiah, P. Sreenivasula Reddy, D. Jhansi Rani
and T. Subbarao

Materials Science Lab, Department of Physics, S K University, Anantapuramu – 515 003, A. P, India

E-mail: chandrababu954@gmail.com

Available online at: www.austceram.com/ACS-Journal

Abstract
The micro structural, dielectric and electrical properties have been studied for magnesium doped strontium titanate
ceramics synthesized via conventional solid state reaction method which were calcined at 1150 0C for 9hr and
sintered at 1300 0C for 3hrs respectively. The high dielectric constant (εr) and low loss tangent (tanδ) were noticed at
RT (room temperature) as 88.1 (0.1 kHz), 45.4 (5 MHz) and 0.0067 (0.1 kHz) respectively for dielectric
applications. The strong relaxation dynamics in loss factor was observed at higher temperatures for lower
frequencies particularly. AC and DC-conductivity variations with temperatures were performed and the activation
energies (Ea) were calculated using the lnσ Vs 1/T plots. Apart from the samples were characterized using XRD,
FESEM, and EDAX for structural, surface morphological, elemental analysis respectively. (MgO)0.1 doped
(SrTiO3)0.9 showed seebeck coefficient of 467.4 µV/K as the slope of curve for the thermoelectric applications.

Keywords: Dielectric Constant, Scanning Electron Microscopy, Electrical Properties, Calcination.

1. INTRODUCTION was increased up to 30,000 [5]. Owing to the

Strontium titanate is a ternary oxide of cubic perovskite
structure with lattice parameter of 3.9076 A0 at RT.
Enormous studies have been done on SrTiO3 because of
its electrical properties and applications [1]. Therefore
SrTiO3 has got recognition as a candidate material for
the applications of phase shifters, oscillators, capacitors
needed circuitry systems, filters, resonators, DRAMs
and sensors [2]. SrTiO3 (ST) exhibited good dielectric,
electrical and defect structural properties. At RT
undoped ST showed a dielectric constant of 250 [3].
However, when impurities are added up to the pure ST,
there may be either enhancement or reduction in the
dielectric and electrical properties and probably change
may be occurred in the diffraction lines. Moreover
dielectric constant was apparently diminished at RT due
to the introduction of MgO into ST lattice nevertheless
decreases the loss factor (tanδ).
The electrical conductivity is directly proportional to
the oxygen partial pressure according to the equation σ
α P1/m O2 [4].Where ‘m’ depends upon the type of
semiconductor i.e. either n-type or p-type
semiconductors. The incipient ferroelectric strontium
titanate retains its paraelectric behavior up to 0 K. At
lower temperatures i.e. below 3 K the dielectric constant
incorporation of MgO into the ST, evidently dielectric
constant was decreased while loss factor increased due
to occupation of Sr+2 site by Mg+2 and good
enhancement in the dielectric constant while decrement
in loss factor because of occupation of Ti+4 site by Mg+2
[6]. Due to substitution effect distinct properties have
been changed, since the ionic radius of Mg+2 (0.120nm)
is smaller than Sr+2 (0.144nm) [7], the first
approximation for the occupation of Mg+2 is Ti+4 site in
ST lattice. In the literature almost low-temperature
dielectric properties have been studied and in this
investigation the author intended to study dielectric
properties from RT to higher temperatures.
As far as micro structural properties are concerned, due
to the addition of magnesium into ST lattice, there could
be no change in the structure. For all kinds of
compositions (x=0.1-0.9) with respect to SMgT, similar
peaks at similar positions were observed except few
additional diffraction lines which correspond to MgTiO3
phases at x=0.15 composition. But for STMg at y=0.15
composition various MgO peaks were observed [8, 9].
The lattice parameter of undoped ST was reported as
0.3906 nm [10]. As just described in O. Okhay et al [11]
some rich grains were observed in TEM studies which
 Naidu et al.
connect to ilmenite structure of MgTiO3. In respect of
electrical properties ac-activation energies were
reported as 0.117-0.142eV at different frequencies [8]
and these are in consistent with pure ST [12]. Moreover
for a particular concentration of (MgO)0.1 doped
(SrTiO3)0.9 the structural dielectric (dielectric constant
and loss factor), and electrical properties (thermo
electric properties, ac and dc- conductivity properties)
were studied in this paper using XRD, FESEM, EDAX
and HIOKI 3532-50 LCR HiTESTER.
2. EXPERIMENTAL PROCEDURE
In order to prepare MgO doped SrTiO3 powder particles
the raw materials were taken as SrCO3 (99.5% purity),
TiO2 (99.54% purity) and MgO (99.9% purity). These
starting materials were mixed in their Stoichiometric
ratio to form (MgO)0.1 doped (SrTiO3)0.9. The resultant
compound is initially ball milled for nearly 12hrs using
Retsch PM200 ball miller and later calcined at a
temperature of 11500C for 9 hrs. Furthermore the
samples were pressed into pellets by applying the
pressure of 10 Tons and were sintered at 13000C for
3hrs in conventional furnaces which can able to go up to
1400 0C temperature. The resultant powder particles and
sintered pellets polished with silver paste of thickness
0.125cm and radius 0.61cm were characterized using
XRD (BRUKER X-Ray Powder Diffract Meter, CuKα)
at room temperature, FESEM, (AMETEK system) and
HIOKI 3532-50 LCR HiTESTER (Japan) for structural,
surface morphological, elemental and dielectric
properties analysis respectively. For the dielectric
properties measurements, the sintered pellets sputtered
with silver paste on both sides without contacting the
edges were kept in platinum electrodes of LCR
controller of temperature range from RT to 600 0C
operated at the frequencies from 42Hz- 5MHz having
the heating rate of 0.50C/min.
3. RESULTS AND DISCUSSIONS
The crystalline structure of Mg doped ST was
evaluated by XRD analysis at RT using Bruker X-Ray
Powder Diffract Meter .The CuKα radiation of wave
length 1.54056 A0 was used for recording X-ray
diffraction pattern. Ni filter was used as the
monochromator. The machine was operated with 30 mA
beam current and 40kV of power. Fig.1 depicts the
XRD pattern of undoped ST and Mg doped ST (referred
as STMg in fig.1). It can be seen that the two
compounds exhibit cubic crystalline structure having
single perovskite phases with the exception of few
additional phases corresponding to the presence of
MgTiO3 phases [13] of hexagonal ilmenite structure
[14]. These phases (MgTiO3 and MgO) are because of
the cationic substitution effect. Since ionic radius is
taken into consideration (radii of Ti4+<Mg2+<Sr2+) [15].
96
Huge increment in the intensity of diffraction line was
obtained due to the increment of structure factor (F) at
2-theta angle 32.490 having 17427 counts and similar
miller indices (h k l) were noticed as (100), (110),
(111), (200), (210), (211), (220) and (310) of undoped
ST. As reported in A. Tkach et al [8] the packing degree
of A and B ions in the ST lattice can be described by
measuring tolerance factor (T) and fractional tolerance
factors (T1 and T2 ) [16] using following formula.
T= ,
.
.
T1 = (1)
T2 =
Where RA= radius of A-site ion, RB= radius of B-site
ion, RO= radius of oxygen ion and a= lattice parameter.
T1 and T2 provide the stability of the compound. If T1 or
T2<1, two ions fluctuate in their sites while for T1 or
T2>1 it attributes closely packed nature of two ions
together. Pure ST exhibited tolerance factor as 1.0016
and for the present samples when Mg occupies B-site of
ST, T, T1 and T2 were reported in sequence as 0.9474,
1.03241 and 1.09006. These are in close agreement with
literature values. Charge compensation mechanism is
obeyed in this case while charge imbalance is produced
if Mg occupies A-site of ST [8]. The lattice constants of
MgO (4.213 A0) are much larger than that of undoped
ST (3.905 A0) [17] and there is a large mismatch
between them. However, the lattice parameters (a, b, c
and α, β, γ) were achieved as a=b=c= 3.8897A0 and α=
β= γ=900 and are in consistent with literature data.
Hence it is confirmed that the structure of present
compound is cubic. Based on lattice parameters
obtained the practical value of unit cell volume
(59.05x10-24 cm3) was calculated which is comparable
to the unit cell volume of undoped ST as reported in
JCPDC file 35-734. Furthermore the average crystalline
size (DP= 106.3 nm) using Scherer formula [18], average
dislocation density (ρ=5.95x1013(m-2)) and average
elastic strain (Estrain= 0.0325) were established
according to the following equations. XRD profile data
is represented in Table 1.
Dp =
(2)
Where k is a constant and is equal to 0.9, θ is diffraction
angle, λ=0.154056 nm (CuKα) and β is full width half
maxima.
ρ= and Estrain= (3)
Journal of The Australian Ceramic Society Volume 52[1], 2016, 95 – 101 97

Table.1 Shows the XRD profile data of MgO doped when counts plotted against the energy (keV), it clearly
SrTiO3 showed the presence of magnesium, titanium, strontium
and oxygen elements with their concentrations. This
2θ d- FWH (h k Dp(n ρx1013( Estrain expressed a fact that not only XRD analysis identifies
spac M l) m) m-2) the presence of second phases but also FESEM and
e EDAX can perform the same thing. Fig 3 depicts
(A0) EDAX spectrum of Mg doped ST ceramics. The
22.8 3.88 0.087 (10 102.8 9.46 0.01 average grain size (Ga) was calculated as 4.83µm, using
42 97 6 0) 59 the following formula [19].
32.4 2.75 0.070 (11 129.8 5.94 0.04
.
92 34 8 0) 75 Average grain size Ga = (4)
40.0 2.24 0.075 (11 125.3 6.37 0.01
49 96 0 1) 25 Where L= the total test line length, M= the
46.5 1.94 0.081 (00 118.2 7.16 0.00 magnification, N= total number of intercepts which the
6 90 3 2) 94 grain boundary makes with the line.
52.4 1.74 0.139 (01 71.2 0.197 0.02
39 35 5 2) 93
57.8 1.59 0.094 (11 107.2 8.7 0.04
65 23 1 2) 87
67.9 1.37 0.104 (02 101.6 9.69 0.06
08 92 7 2) 08
77.2 1.23 0.119 (01 94.3 0.112 0.03
6 39 8 3) 57

Fig.2 shows FESEM images of MgO doped

SrTiO3

Fig.1 Shows the XRD Spectrum of MgO doped SrTiO3

ceramics (MgTiO3 and. MgO)
The surface morphology was analyzed by field emission
scanning electron microscopy. Fig.2 shows the FESEM
images of Mg doped ST sintered at 13000C which are
made at the different spots having 10,000X
magnifications and in 500µm, 4µm range. In the images
almost spherical shape grains containing
inhomogeneous distribution along with grain
boundaries have been observed. Discrete rich grains
have been seen which are corresponding to the presence
of MgTiO3. Sintering effect is responsible for the grain
growth of present sample. In EDAX spectrum also
Fig.3 Shows EDAX Spectrum of MgO doped SrTiO3
The dielectric properties have been studied by means of
LCR meter (HIOKI 3532-50 HiTESTER). Dielectric
constant of Mg doped ST sintered at 13000C as a
function of temperature (303K-673K) at the selected
frequencies of 0.1 kHz- 5MHz is plotted in fig.5. Clear
evidence has been given by Olena Okhay et al [22] as
owing to the substitution of Mg on both sites of
strontium and titanium, it substantially decreases the
permittivity as well as dielectric loss at lower
temperatures and are lower than the undoped ST.
 Naidu et al. 98

Various kinds of dopants to ST such as magnesium,

manganese, chromium and iron were used to decrease 1400
the loss factor (tanδ) [23].
1200
0.1kHz
Table.2 Shows EDAX data of MgO doped SrTiO3 1kHz

Dielectric constant
1000
1MHz
800 3MHz
5MHz
600

400

200

0
303 353 403 453 503 553 603 653
Temperature(K)

Fig.4 Shows the Dielectric constant Vs Temperature

Plots of MgO doped SrTiO3 ceramics

In this investigation also similar reports were obtained

but they are at higher temperatures. As far as the exact 1.2
0.1kHz
results are concerned, at frequencies 0.1 kHz and 5 1kHz
1
MHz when temperature approaches to RT, εr values are 1MHz
loss tangent(tanδ)

obtained as 88.05 and 45.43 respectively. This reveals 0.8 3MHz

the fact that at lower frequencies only dielectric 5MHz
response is high while it is low for the higher range 0.6
frequencies due to lagging of polarization mechanism
behind the applied field. Obviously, in fig.4 between the 0.4
temperatures of 303K- 413K (at 0.1 kHz), a moderate
0.2
increase of permittivity (εr) and an abrupt enhancement
of εr at 413K- 563K range was observed. When 0
temperature approaches to 673K, εr is achieved as
30 80 130 180 230 280 330 380
1178.9 and 57.67 at 0.1 kHz and 5 MHz respectively. Temperature(0C)

The loss factors were noted as 0.0067 and 0.1621 at 0.1 Fig.5 Shows Loss tangent Vs Temperature Plots of
kHz and 5 MHz respectively (at RT). But for the similar MgO doped SrTiO3
frequencies at 673K tanδ values were obtained
sequentially as 1.048 and 1.022.Hence, it is confirmed 80000000
that as increasing the temperature, loss has increasing
trend. The temperature dependence of dielectric loss is 70000000 0.1kHz
depicted in fig5. Mean while, tanδ spectrum of Mg 1kHz
60000000 1MHz
doped ST attributed to the ferroelastic domain wall 3MHz
Impedance(Ω)

dynamics around the cubic to tetragonal phase 50000000 5MHz

transformation [24-26] at 0.1 kHz and 1 kHz. At higher 40000000
temperatures 503K and 453K two strong peaks owing to
30000000
relaxation dynamics were noticed for lower frequencies.
20000000
Fig.6 depicts the temperature dependence of impedance
10000000
(Z) and it established a fact that the higher is the
temperature; the lower is the impedance for smaller 0
frequencies. The moderate Z-values were achieved at 30 80 130 180 230 280 330 380
higher frequencies. Temperature(0C)

Fig.6 Shows the Impedance Vs Temperature Plots of

MgO doped SrTiO3
Journal of The Australian Ceramic Society Volume 52[1], 2016, 95 – 101 99

Temperature dependence of Seebeck coefficient thermally activated and hence this can be governed by
(thermoelectric power) of MgO doped ST ceramics the Arrhenius equation.
sintered at 13000C is shown in fig. 8. The Seebeck
coefficient is positive and increases with increase of %
σ =σ0 exp ( ) (6)
temperature revealing that holes are being introduced by #&

Mg addition. In Dy doped ST electrons were introduced

Where K=8.6X10-5eV, σ0= pre exponential factor, and
as just reported in J.LIU et al [27]. However, at high
T= absolute temperature.
temperatures the seebeck coefficient showed a constant
In general σac can be calculated by the following
trend and later decreased with an overall slope of
equation.
467.4µV/K. Because of addition of MgO there is a
moderate decrease in the slope of present sample than
σac= ε0εrω tanδ (7)
undoped ST. The carrier concentration (n) was
calculated for the MgO doped ST pellets of thickness
Where εr =dielectric constant, ε0=8.9X10-12 F/m, ω=2πf
0.125cm and radius 0.61cm as 0.031X1022 cm-3 using
and tanδ= loss tangent. Fig. 11 depicts the variation of
the following equation.
ac –conductivity with reciprocal of temperature and
!" reveals almost a linear relation between lnσac and
n= X exp ( ) (5) 1000/T. The slopes of the curves attribute activation
#
energies and were achieved as 0.22eV, 0.32 eV and
Where N=1022cm-3 (Density of states), V=0.15 cm3 0.54 eV at 0.1 kHz, 1 kHz and 5 kHz frequencies
# respectively. These were in close agreement with
(Volume of the sample), = 86.4 µV/K and S=seebeck
$ activation energies of undoped ST [28]. But for the
coefficient
higher frequencies i.e. at 5 MHz Ea was obtained as
12000 0.008eV. This explicitly establishes a fact that
conductivity increases with increasing frequency and
10000
becomes independent of temperature at high
frequencies. At lower frequencies the conductivity
Thermoemf (µV)

8000
increases with increase of temperature due to thermal
6000
activation process and this must be related to hopping of
4000 charge carriers which are bound in the localized states
while conductivity decreases with increasing
2000 frequencies because of hopping of free charge carriers
0
[29].
273 319 365 412 459 502
0.004
Temperature difference(K)
0.1kHz
0.0035
Fig.7 Shows the Thermo emf Vs Temperature 1kHz
AC-conductivity(FHz/m)

0.003 1MHz
Difference Plots of MgO doped SrTiO3 3MHz
0.0025 5MHz
30
0.002
25
Seebeck coefficient(μV/K)

0.0015
20 0.001
15 0.0005

10 0
303 353 403 453 503 553 603 653
5 Temperature(K)

0
303
Fig.8 Shows the Seebeck coefficient Vs Temperature
Plots of MgO doped SrTiO3
Fig. 9 shows the ac conductivity as a function of
frequency at various temperatures. As the temperature
goes on increasing, the dielectric relaxation becomes
353 403 453 503 553
Fig.9 shows the ac-conductivity Vs Temperature Plots
Temperature(K)
of MgO doped SrTiO3 ceramics
DC-conductivity (σdc=L/RA) of MgO doped SrTiO3
was performed and it exhibited the exponentially
increasing trend with respect to the temperature from
RT to 673K. Apart from this lnσ Vs 1000/T plot has
also been performed in fig.12.
 Naidu et al. 100

ceramic material was found as 0.787eV using the

0 following formula. From the fig.11 it can be observed
3.30 2.83 2.48 2.21 1.99 1.81 1.66 1.53 that up to 550K there was a gradual increase owing to
the hopping mechanism and later an abrupt increase was
-5
because of linear hopping mechanism.

%
-10 σdc =σ0 exp ( ) (8)
#&
lnσac

-15
0.1kHz 4. CONCLUSIONS
1kHz In conclusion of this work (i) (MgO)0.1 doped
-20 1MHz (SrTiO3)0.9 prepared via solid-state reaction method
3MHz
5MHz
showed good enhancement in the dielectric constant
rather than the dielectric constant of Sr0.9Mg0.1TiO3 or
-25 1000/T(1/K) SrMg0.1Ti0.9O3 ceramics when compared with
literature.(ii) Thermoelectric properties were
Fig.10 shows the lnσac Vs 1000/T plots of MgO doped investigated from room temperature up to 673K and
SrTiO3 showed insulating nature with increasing
temperature.(iii) It is observed that the compound
exhibits cubic crystalline structure having single
0.0000006 perovskite phases with the exception of few additional
phases corresponding to the presence of MgTiO3 phases
0.0000005 of hexagonal ilmenite structure and MgO phases.(iv)
The ac- activation energies were achieved as 0.22eV,
dcconductivity (mho/cm)

0.0000004
0.32 eV and 0.54 eV at 0.1 kHz, 1 kHz and 5 kHz
0.0000003 frequencies respectively. But for the higher frequencies
i.e. at 5 MHz Ea was obtained as 0.008eV and this
0.0000002 reveals a fact that conductivity increases with increasing
0.0000001
frequency and becomes independent of temperature at
high frequencies. The dc- activation energy (Ea) of
0.0000000 MgO doped SrTiO3 ceramic material was found as
0.787eV.
250 300 350 400 450 500 550 600 650 700
Temperature (K)

Fig.11 shows the dc-conductivity Vs Temperature ACKNOWLEDGEMENTS

Plots of MgO doped SrTiO3 ceramics This work was financially supported by a project of
University Grants Commission (UGC)-NEW DELHI,
INDIA. Also thanks to Vellore Institute of Technology
-14 (VIT), Tamilanadu, and Prof. K. R. Gunasekhar from
-16
IISC-Bangalore for supporting in characterization
works such as XRD and FE-SEM of my samples and
-18 giving their valuable suggestions.
ln sigma

-20

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