Research Article

Received: 25 May 2009

Accepted: 18 August 2009

Published online in Wiley Interscience: 13 November 2009

(www.interscience.wiley.com) DOI 10.1002/jrs.2494

Vibrational spectroscopic study of Sr2ZnTeO6

double perovskites
Anderson Dias,a Ganesanpotti Subodh,b Mailadil T. Sebastianb
and Roberto L. Moreirac
Sr2 ZnTeO6 ceramics were prepared by the solid-state route and their vibrational phonon modes were investigated using optical
spectroscopic techniques, for the first time. X-ray diffraction (XRD) and Raman and infrared spectroscopies were employed to
investigate the structures of these perovskite materials and the results analysed together with group-theoretical predictions.
The number and behaviour of the first-order modes observed in both spectroscopic techniques are in agreement with the
calculations for a tetragonal I4/m space group. The complete set of the optical phonon modes was determined, and the intrinsic
dielectric properties of the materials were evaluated, allowing us to discuss their potential application in microwave (MW)
c 2009 John Wiley & Sons, Ltd.
circuitry. Copyright

Keywords: double perovskites; Raman spectroscopy; infrared spectroscopy; ceramics; microwave dielectrics; crystal structure

Introduction

702

From the materials chemistry point of view, ceramics with

the perovskite structure present an incredibly wide array of
structures and phases with totally different functions, which are
directly related to the combination of chemical elements in the
basic formula ABX3 , X being usually oxygen. The multiple ion
substitution in the perovskite lattice in either the A or B position, or
in both, creates the so-called complex perovskites, which present
pairs of unlike valence cations in proportions depending on their
oxidation states and ionic radii.[1] It is well known that the final
properties of any perovskite material are highly dependent on
the nature of its constituent cations, as well as on its structural
features, including ordering and defects.[2,3] In particular, because
of their adequate dielectric responses at high frequencies, ceramic
materials such as A2 B B O6 , known as double perovskites, can
be used as dielectric resonators and filters in microwave (MW)
circuitry. Therefore, these compounds have been investigated
in the past years by many research groups in an attempt to
understand their crystal structure and dielectric behaviour as
functions of chemical substitution and physical behaviour, which
are intimately related to their performance in service.[3 5] More
recently, studies have been performed on double perovskites
containing B-site hexavalent cations, such as Mo, Re, U, W and
Te.[6 12]
According to Augsburger et al.,[9] p-elements like tellurium can
be successfully stabilized in the B sites of the perovskite structure,
once they show the required spherical symmetry and adequate
ionic sizes. Also, previous works on Te-based compositions showed
excellent MW properties with very low sintering temperatures
(<700 C).[9,13] Although a number Te-based new materials have
been reported, to the best of our knowledge, no investigation
has been carried out to explore the vibrational properties of
complex perovskites with simultaneous presence of Zn and Te
sharing their B positions. In particular, ceramics with the formula
Sr2 ZnTeO6 have not yet been investigated from the perspectives
of the behaviour of their optical phonon modes either from their

J. Raman Spectrosc. 2010, 41, 702706

crystalline structure. In order to study the potential of a given

material to MW applications (resonators or filters), the knowledge
of its polar phonon features is mandatory, since these infrared
active phonons determine the intrinsic dielectric response of
the system in the intermediate terahertz region. Recently, Dias
et al.[11] and Ayala et al.[14] studied the characteristics of the optical
phonons in Sr2 MgTeO6 and Sr2 CoTeO6 based on Raman scattering
data and found correlations between the crystalline structures
and the vibrational modes for these ceramics. In the present work,
Raman and infrared reflectivity spectra of Sr2 ZnTeO6 ceramics are
investigated in detail together with group theory calculations. The
results allow us to contribute to the debate on the crystalline
structure and MW dielectric properties of this ceramic system.

Experimental
Sr2 ZnTeO6 ceramics were prepared by a solid-state ceramic route.
High-purity SrCO3 and TeO2 (99 + %, Aldrich Chemical Co.) were
used as starting materials. Stoichiometric amounts of the powder
mixtures were ball-milled in distilled water as medium using yttriastabilized zirconia balls in a plastic container for 24 h. The slurry
was dried, ground well, heated at a rate of 2.5 C/min and kept
at 700 C for 4 h. A slow heating rate was given for the oxidation
of Te4+ to Te6+ , which occurs under specific thermodynamic

Correspondence to: Anderson Dias, Departamento de Qumica, ICEB II, Sala 67,
UFOP, Ouro Preto, MG 35400-000, Brazil.
E-mail: anderson dias@iceb.ufop.br

a Departamento de Qumica, Universidade Federal de Ouro Preto-UFOP, Ouro

Preto, MG 35400-000, Brazil
b Materials and Minerals Division, National Institute for Interdisciplinary Science
and Technology, Trivandrum 695 019, India
c Departamento de Fsica, Universidade Federal de Minas Gerais-UFMG, C. P.
702, Belo Horizonte, MG 30123-970, Brazil

c 2009 John Wiley & Sons, Ltd.

Copyright

Results and Discussion

(400)

Intensity

440
620
511

60

2/degrees

531

400
420

222
311

74.4 75.0 75.6 76.2 76.8

80

100

120

140

2/degrees
Figure 1. XRD pattern for the Sr2 ZnTeO6 ceramics sintered at 1125 C for
2 h. Insets: high-resolution data for the peaks (400) and (620). Notice the
complex structure of the peaks (fitted by Gaussian curves), owing to the
lowering of symmetry besides K 1 and K 2 reflections.

Figure 2. Microstructure (SEM) of the Sr2 ZnTeO6 samples sintered at

1125 C for 2 h.

Fig. 1 and were tentatively indexed on the basis of the International

Centre for Diffraction Data (ICDD) file #16-0549, assuming a
cubic structure, as previously made in other similar Te-based
ceramic systems.[11] The bulk density of Sr2 ZnTeO6 ceramics with
additions of B2 O3 was greatly enhanced and attained a maximum
at 1125 C (96.1% of the theoretical density). Figure 2 presents
the microstructure of 0.2 wt% B2 O3 added Sr2 ZnTeO6 material
sintered at 1125 C for 2 h. As can be observed, the materials
have uniform distribution of grains with sizes varying from 1 to
4 m. The stability of complex perovskite structures can be well
explained with the use of tolerance factors (t).[1] For the materials
studied here, the tolerance factors can be determined by:

c 2009 John Wiley & Sons, Ltd.

Copyright

RSr + RO


t =

RZn + RTe
+ RO
2
2

(1)

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703

Crystalline, single-phase Sr2 ZnTeO6 perovskites were produced

after conventional solid-state processing at 1125 C without any
secondary phases or impurities. The XRD results are displayed in
J. Raman Spectrosc. 2010, 41, 702706

40

331

111

20

(620)

422

44.8 45.2 45.6 46.0 46.4

2/degrees

200

conditions.[15] The mixed powders were calcined at 1000 C for

4 h, ground into fine powders and divided into different batches for
optimizing the sintering temperature. Due to the poor sinterability
of Sr2 ZnTeO6 , 0.2 wt% B2 O3 (Aldrich Chemical Co.) was added as
sintering aid and mixed thoroughly to the powders in distilled
water and dried. They were subsequently mixed with 4 wt% of
polyvinyl alcohol (molecular weight 22 000, BDH Lab Suppliers,
England) and again dried and ground well. Cylindrical pucks of
about 1011 mm height and ca 20 mm diameter were made by
applying 150 MPa pressure. These compacts were then fired at
600 C for 30 min to expel the binder before sintering at 1125 C
for 2 h. The densities of the sintered materials were determined by
the Archimedes method.
The crystal structure and the phase purity of the sintered samples
were studied by X-ray diffraction (XRD) using Cu K radiation
( = 0.15418 nm) in a Rigaku-Geigerflex 2037 diffractometer,
with the BraggBrentano geometry, in the 2 range 10140
(step 0.05 2, 1 s/step). Besides, higher resolution data for using
in investigations concerning deviations from cubic symmetry
were collected at 4 s/step of 0.02 2 , in special ranges around
chosen peaks. In these measurements, because of imperfect
monochromaticity, the data contain the contribution of the
K 2 line, which was then considered in the data analysis. The
sintered samples were thermally etched for 20 min at 1100 C, and
the microstructures were analysed by using a scanning electron
microscope (SEM: JSM 5600 LV, Tokyo, Japan).
Micro-Raman scattering spectra were collected in backscattering configuration by using an Olympus confocal microscope
attached to a Horiba/Jobin-Yvon LABRAM-HR spectrometer (objective 100), equipped with 600 and 1800 grooves/mm diffraction
gratings. The 632.8 nm line of a HeNe laser (effective power of
6 mW at the sample surface) was used as the exciting line and
a Peltier-cooled charge-coupled device (CCD) as detector of the
scattered light. An edge filter was employed for stray light rejection, i.e. Rayleigh scattered light. The wavenumber resolution
was better than 2 cm1 and the accumulation times were typically ten collections of 20 s. The obtained spectra were divided
out by the BoseEinstein thermal factor[16] before being fitted
by a sum of Lorentzian lines. Infrared reflectivity measurements
were performed in a Fourier transform spectrometer (Bomem DA
8-02) equipped with a fixed-angle specular reflectance accessory
(external incidence angle of 11.5 ). In the mid-infrared region
(5004000 cm1 ), we used an SiC glowbar lamp as the infrared
source, a Ge-coated KBr beamsplitter and an LN2 -cooled HgCdTe
detector. In the far-infrared range (50600 cm1 ), we used the
same source, but a 6-m coated Mylar hypersplitter and a liquidHe-cooled Si bolometer. The samples surfaces were polished to an
optical grade (0.25 m) prior to the measurements. A gold mirror
was used as reference. The data were collected under vacuum
(104 bar) with a spectral resolution of 2 cm1 . The reflectivity
spectra were evaluated by means of standard KramersKronig
analysis and adjusted by an oscillator model. A generalized fourparameter oscillator model was used rather than the classical
model to achieve a good fit with minimum number of physically
meaningful oscillators.

220

Vibrational spectroscopic study of Sr2 ZnTeO6

A. Dias et al.

Raman Intensity

where RSr , RZn , RTe and RO are the ionic radii of Sr, Zn, Te and
O ions, respectively.[1,11,17] Shannons ionic radii[17] are frequently
employed to determine the tolerance factors. For Sr2 ZnTeO6 ,
the tolerance factor is 0.985, which is at the borderline between
cubic (untilted) and distorted pseudo-cubic (tilted) structures.
Based on previous results of Dias et al.,[11] which showed how to
distinguish between cubic or pseudo-cubic symmetries in similar
Sr-containing double perovskites, high-resolution XRD analyses
were then carried out around the particular peaks (400) and
(620). The corresponding diffractograms are displayed in the
insets of Fig. 1, where characteristic splittings of the XRD peaks
are seen after peak deconvolution (the experimental data were
fitted by Gaussian curves for easier visualization), demonstrating
unequivocally a lowering of symmetry in these ceramics. The
observed peak splitting together the high tolerance factor (close
to 1) suggests a slight tetragonal distortion of the cubic lattices
for our materials, as has been verified in other double perovskites
containing tellurium or indium.[11,18] As will be shown later, these
observations are confirmed by the analysis of our spectroscopic
data. The MW dielectric properties of the Sr2 ZnTeO6 ceramics were
investigated using the resonance method at 5 GHz (details on the
experimental setup are described in Ref. [11]). The material has
dielectric constant of 16.5, quality factor of 8500 and temperature
coefficient of the resonant frequency of 77 ppm/ C at the
optimized sintering conditions of 1125 C/4 h.
Room-temperature Raman analysis was carried out in Sr2 ZnTeO6
materials, and the results are displayed in Fig. 3 (open squares).
As can be seen, the spectrum is dominated by four strong bands
centred at 147, 430, 573 and 767 cm1 , together with other
weaker though well-defined bands which will be discussed later.
Such a profile with four intense Raman bands is characteristic
of ordered 1 : 1 complex perovskites with cubic or pseudo-cubic
structures.[19,20] Compared to their MgTe analogues, the bands
of the Sr2 ZnTeO6 ceramics are slightly downshifted.[11] This is
as a consequence of the larger Zn ions compared to Mg ions,
which leads to an expanded unit cell with larger ionic distances

105

140

175

and, therefore, to general weaker ionic bonds. Completing the

spectroscopic analysis, infrared reflectivity spectrum of Sr2 ZnTeO6
materials is presented in Fig. 4 (open squares). The visual inspection
of the spectra shows at least six well-defined bands for these
samples, indicating an average non-cubic symmetry for the
Sr2 ZnTeO6 materials, as will be discussed below. A careful
analysis of Fig. 4 reveals the presence of other weaker bands
and shoulders in the reflectivity spectrum, which can be revealed
only after adequate fitting procedures. In view of that, a group
theoretical investigation was undertaken in order to get a better
understanding of the crystal structure and its consequence on the
samples vibrational features.
The ideal simple perovskite is cubic, belonging to the Pm3m
space group, but tilting of the oxygen octahedra occurs very often,
owing to structural instabilities linked to a mismatch in the sizes
of the cations. It is worth mentioning that there are no active
first-order Raman phonons and only three infrared active modes
for the ideal Pm3m group. Concerning the complex perovskites of
the general formula A2 B B O6 , cubic structures will be presented
by materials with tolerance factors close to or greater than 1.
In such cases, the ideal cubic structure can still be assumed by
totally disordered systems (B site with average occupation of two
cations). However, the most interesting and frequent cases are
shown by ordered, yet untilted lattices with Fm3m symmetry (O5h ,
No. 225, Glazers notation a0 a0 a0 ).[21] This configuration allows a
classification of the normal modes at the Brillouin zone centre as
 = Ag + Eg + F1g + 2F2g + 5F1u + F2u . The symmetry analysis of the
irreducible representations above indicates that four modes are
Raman active (Ag , Eg , 2F2g ), and another four modes are infrared
active (4F1u ).[22] For our Sr2 ZnTeO6 ceramics, XRD data showed
that an Fm3m structure is not adequate to describe its structure,
because it is not compatible either with the splitting of the (400)
and (620) XRD peaks or with the number of observed modes in
Raman and infrared spectra. Indeed, a lower symmetry structure
with a small distortion from the cubic one appears to be more

210

Wavenumber/cm-1

390
420
450
Wavenumber/cm-1

150

300

450

600

750

900

Wavenumber/cm-1

704

Figure 3. Micro-Raman spectrum for the Sr2 ZnTeO6 complex perovskites

in the spectral region 40900 cm1 . Experimental data are in open squares,
while the fitted curve is the black line. Grey lines represent the phonon
modes adjusted by Lorentzian curves.

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Figure 4. Measured (closed squares) and adjusted (solid black line) infrared
reflectivity spectra for the Sr2 ZnTeO6 ceramics.

c 2009 John Wiley & Sons, Ltd.

Copyright

J. Raman Spectrosc. 2010, 41, 702706

Vibrational spectroscopic study of Sr2 ZnTeO6

plausible to describe the XRD and spectroscopic data. A2 B B O6
double perovskites with tetragonal distortion belong very often to
the I4/m space group.[23] In the present case, we believe that this
structure could describe our data, since it holds for other similar
materials.[11,18,19]
Assuming this tetragonal structure, Sr2 ZnTeO6 materials could
5
, No. 87,
be described as belonging to the I4/m space group (C4h
0
0

[21]
Glazers notation a a c ). This tetragonal symmetry is derived
from the prototype Fm3m cubic structure by an antiphase tilt
of ZnO6 and TeO6 octahedra in the basal plane along the [001]
direction of the cubic cell. In this structure, Sr atoms occupy 4d
sites of S4 symmetry, Zn and Te ions occupy 2a and 2b sites of C4h
symmetry and the oxygen atoms are in 4e and 8h sites (C4 and Cs
symmetries, respectively). Then, by using the site group method of
Rousseau et al.,[22] one obtains the following decomposition of the
phonon modes in terms of the irreducible representations of the
C4h point group:  = 3Ag + 5Au + 3Bg + Bu + 3Eg + 6Eu . Excluding
the acoustic (Au + Eu ) and silent modes (Bu ), we would expect nine
Raman active (3Ag , 3Bg , 3Eg ) and nine infrared modes (4Au , 5Eu ) for
this structure. Bearing in mind the above factor group calculations,
careful fitting of the Raman spectra of Sr2 ZnTeO6 samples were
carried out. The theoretical curves are displayed in Fig. 3 as solid
black lines, besides nine Lorentzian grey lines, in perfect agreement
with the theoretical predictions. Table 1 presents the adjustment
parameters to the best fit of the Raman spectrum, i.e. wavenumbers
(cm1 ) and full width at half-maxima (cm1 ). This result presents
strong evidence that Sr2 ZnTeO6 perovskite would belong to the
5
) space group.
tetragonal I4/m (C4h
Now, the results from infrared reflectivity measurements will be
discussed. The spectrum displayed in Fig. 4 was analysed by using
the four-parameter semi-quantum model,[24] with a nonlinear
least-squares program.[25] Within this model, the infrared phonon
contributions to the complex dielectric function () can be
described by:
() =

N

2j,LO 2 + i j,LO
j=1

2j,TO 2 + i j,TO

114.2
141.8
155.6
166.4
413.9
422.4
432.1
568.5
765.9

15.5
4.3
10.2
19.5
7.3
6.9
6.6
20.3
23.8


j =

(2k,LO 2j,TO )

k

2j,TO
(2k,TO 2j,TO )

(4)

k=j

From these values, the static dielectric constant in the MW limit

(j,TO ) is obtained by adding the oscillator strengths over all
modes according to the equation:
r = +

N


(5)

j=i

The values of r and for the double perovskite are given in

Table 2, together with the phonon dispersion parameters. Now,
the intrinsic unloaded quality factor Qu extrapolated to the MW
region (j,TO ) can be calculated as the reciprocal of the
dielectric loss tangent (tan ), i.e.
tan =

tan j =

 j j,TO

r 2j,TO
j

(6)

The obtained values for the individual and overall losses are also
presented in Table 2. At 10 GHz, Sr2 ZnTeO6 ceramics presented
intrinsic Qu f of 85 THz and r = 14.1. These values are
quite adequate for applications as MW devices relatively high
quality factor (high selectivity) and high dielectric constant and

j,TO

j,TO

j,LO

j,LO

105 tan j /

147.2
187.7
198.0
243.6
258.4
372.7
441.0
668.3
705.3

12.5
18.4
36.7
48.2
79.2
13.4
41.3
30.2
44.1

161.7
197.0
237.3
255.2
260.0
440.6
460.1
701.2
760.3

9.7
65.1
67.3
57.6
15.5
53.3
20.5
37.6
14.6

4.342
3.458
0.329
0.105
0.007
1.760
0.002
0.628
0.046

17.863
12.826
2.188
0.606
0.063
1.208
0.003
0.301
0.029

= 3.41

r = 14.1

 tan j / = 35.0 105

The positions () and damping constants ( ) are given in cm1 .

c 2009 John Wiley & Sons, Ltd.

Copyright

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705

Positions (, cm1 ) and full width at half-maxima ( , cm1 ) were

obtained from the adjustment of the experimental data by Lorentzian
lines.

J. Raman Spectrosc. 2010, 41, 702706

(3)

Table 2. Dispersion parameters calculated from the fit of the infrared

reflectance spectrum of Sr2 ZnTeO6

Table 1. Observed Raman modes for the Sr2 ZnTeO6 ceramics

1
2
3
4
5
6
7
8
9



 () 1 2


R = 

 () + 1 

The best fit of our experimental reflectivity data by Eqns (1) and (2)
are presented in Fig. 4 as the solid black curve, and the obtained
dispersion parameters (positions and widths of the TO and LO
infrared branches) are listed in Table 2. We note that nine infrared
modes were discerned for the Sr2 ZnTeO6 ceramics, in perfect
agreement with the predicted number of modes for materials
with the assumed tetragonal structure.
Once the dispersion parameters for the polar phonons are
determined, we can calculate the intrinsic phonon contribution to
the MW dielectric properties of the material. First, we calculate the
oscillator strengths of the individual jth TO modes (Table 2) by:

(2)

where is the electronic polarization contribution, and

j,LO (j,TO ) and j,LO ( j,TO ) are the frequency and damping of
the jth longitudinal (transverse) optical polar modes, respectively.
N is the number of polar phonons. At quasi-normal incidence, the
dielectric function is related to the optical reflectivity R by the

Band

Fresnel formula:

A. Dias et al.
are in good agreement with the dielectric response of other
double perovskites.[11,18,19] However, we should remember that
for ceramic materials the intrinsic Qu f values are usually higher
than the actual MW ones, because some important dielectric
losses of extrinsic origin (impurities, polar species, microstructural
defects, etc.) must be added up to the phonon ones.[26] Despite
this, the intrinsic quality factor value allows a good evaluation
of the processing conditions for a ceramic material once single
crystals have very low extrinsic contributions.
Let us now discuss the tetragonal structure proposed for
our Sr2 ZnTeO6 ceramics. Howard et al.[27] have applied group
theoretical tools to study ordered double-perovskite structures by
considering different combinations of octahedral tilting, starting
from the cubic Fm3m structure. This structure is a result of the
doubling of the ideal perovskite by imposition of rocksalt 1 : 1
ordering. From this Fm3m space group, tilting of the BO6 octahedra
are allowed, resulting in eleven structures of lower symmetry, as a
result of the cation ordering in combination with the corner-linked
tilting of the octahedral units. Groupsubgroup relationships were
established, which could be applied to explain the experimentally
observed results of the present work, as discussed below.
Sr2 ZnTeO6 perovskites present a tolerance factor nearly unity,
which means that a cubic phase would be expected. Many
other complex perovskites with tolerance factors near unity
(or traditionally considered cubic) were recently revisited, and
distorted structures were determined.[11,14,18,19,28] Indeed, in some
recent works, Dias et al.[11,14,19] and Ayala et al.[14] showed that
although XRD and other techniques indicate cubic or nearly
cubic structures for a number of double perovskites, Raman
spectroscopic analysis was able to resolve the structures as actually
tetragonal. Within the framework of the Glazer[21] description,
the I4/m structure derives from Fm3m (a0 a0 a0 ) by a single
rotation of the BO6 octahedra about one of the four-fold axes,
lowering the symmetry to tetragonal (a0 a0 c ). This structure
presents nine Raman active and another nine infrared active
phonon modes,[19] in complete agreement with our findings for
the Sr2 ZnTeO6 ceramics. We believe that the small tetragonal
distortion in these materials is similar to that observed in
Sr2 MgTeO6 ,[11] Ba2 MgTeO6 ,[11] Sr2 CoWO6 [14] and Ba2 YNbO6 ,[19]
i.e. the octahedral tilting is too small to be detected by XRD
or even more sophisticated techniques such as neutron and
electron diffraction. However, the anti-phase distortions appear
to be sufficiently large to be detected by Raman and infrared
spectroscopies, giving rise to the degeneracy and breaking of the
symmetries of the normal modes and leading to a larger number
of observed fundamentals.

close to unity (usually considered cubic). The materials present the

tetragonal I4/m structure with small deviations from the common
cubic Fm3m structure, which occurs very often in perovskites with
ordered lattice arrangements with 1 : 1 ratio.
Acknowledgements
The Brazilian authors acknowledge the financial support from
CNPq (Conselho Nacional de Desenvolvimento Cientfico e Tec

nologico),
FINEP (Agencia
de Inovaca o) and FAPEMIG (Fundaca o
de Amparo a` Pesquisa do Estado de Minas Gerais). G. Subodh
is grateful to CSIR (Council of Scientific and Industrial Research),
India for a junior research fellowship. We also thank Alexandre M.
Moreira for his help in XRD experiments.

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[24]

Sr2 ZnTeO6 ceramics were prepared as single-phase materials, and

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J. Raman Spectrosc. 2010, 41, 702706