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Synthesis and Optical Investigations on
(Ba,Sr)TiO 3 Borosilicate Glasses Doped with La
2O3
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Optics and Photonics Journal, 2013, 3, 1-7
doi:10.4236/opj.2013.34A001 Published Online August 2013 (http://www.scirp.org/journal/opj)
Synthesis and Optical Investigations on (Ba,Sr)TiO3
Borosilicate Glasses Doped with La2O3
C. R. Gautam*, Avadhesh Kumar Yadav
Advanced Glass and Glass Ceramic Research Laboratory, Department of Physics,
University of Lucknow, Lucknow, India
Email: *gautam_ceramic@yahoo.com
Received May 1, 2013; revised June 11, 2013; accepted July 16, 2013
Copyright © 2013 C. R. Gautam, Avadhesh Kumar Yadav. This is an open access article distributed under the Creative Commons
Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is
properly cited.
ABSTRACT
In this research paper we are reporting synthesis, structural and optical investigations of barium strontium titanate borosilicate glasses with addition of La2O3. Glasses were synthesized by conventional rapid melt quench method. Infrared
absorption spectra, for various (Ba,Sr)TiO3 borosilicate glass samples having glass system 64[(Ba1-xSrx)TiO3]35[2SiO2-B2O3]-5[K2O]-1[La2O3] (x = 0.3, 0.5, 0.6, 0.8 and 1.0), were recorded over a continous spectral range from
450 - 4000 cm−1. IR spectra were analyzed to determine and differentiate the various vibrational modes in the structural
changes. Raman spectroscopy of all glass samples were also carried out wavenumber range form 200 - 1500 cm−1.
These two complementary spectroscopic techniques revealed that the network structure of the studied glasses is mainly
based on BO3, pentaborate groups linked to BO4 tetrahedra and units placed in different structural groups, the BO3 units
are dominanting. The recorded IR and Raman spectra of different glasses are used to clarify the optical properties of the
prepared glass samples correlating with their structure and compositions. UV-Vis spectroscopy was carried out in range
of 200 - 800 nm. The optical band gap was found between 2.023 - 3.320 eV.
Keywords: (Ba,Sr)TiO3; Infrared Spectroscopy; UV-Vis Spectroscopy; Raman Spectroscopy
1. Introduction
Glasses are defined as inorganic product of fusion which
has been cooled to a rigid condition without crystallization without crystallization [1]. The main distinction between glass and crystals is the presence of long range
order in the crystal structure. A widespread set of very
different borate glasses with optical, magnetic, superionic conductivity and other technologically interesting
properties are currently produced. The optimization of
such properties as a function of compositions and other
synthesis parameters are required a good knowledge of
the microscopic glassy structure. For many years, glasses
containing transition metal ions have attracted attention
because of their potential applications in electrochemical,
electronic and electro-optic devices [2]. IR spectroscopy
is one of the most common spectroscopic techniques
used by organic and inorganic chemists. Simply, it is the
absorption measurement of different IR frequencies by a
sample positioned in the path of an IR beam. The main
goal of IR spectroscopic analysis is to determine the che*
Corresponding author.
Copyright © 2013 SciRes.
mical functional groups of the samples. Using various
sampling accessories, IR spectrometers can accept a wide
range of types of sample such as gases, liquids, and solids. Thus, IR spectroscopy is an important and popular
tool for structural elucidation and compound identification [3]. Raman spectroscopy is also an essential tool for
characterization of the structure, environment, and dynamics of glassy materials. Furthermore, the portability
of the technique allows for its use in on-line process monitoring [4]. In Raman spectroscopy, the nature of the
light matter interaction is not same as in IR spectroscopy
and the fundamental differences between the two processes determine the selection rules, which control Raman
or IR activity of normal mode of vibrations. Interaction
of IR radiation with a normal mode of vibration only
occurs when the electric field of radiation oscillates with
same frequency as instant dipoles caused by atomic vibrations. A normal vibration can be IR active only if a
change in the dipole moment of the vibration occurs and
is a one photon process, as only photon is absorbed [5].
Therefore, IR spectra give addition information than
Raman spectra by which the symmetries of normal
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C. R. GAUTAM, A. K. YADAV
2
modes of vibration of molecules and crystal lattices are
determined [6-8]. Addition of various alkali modifiers,
A2O (A: Li, Na, K, Rb, Cs), to the borate glasses brings
drastic changes in the structural units. The structure of
alkali borates glassy matrix is a complex three-dimensional network of boron and oxygen composed of larger
structural units. The added modifier can act in two different ways: by forming four-coordinated boron ( BO 4 )
and by forming non-bridging oxygen (NBO). These two
structural units are described by reaction given bellow:
2 BO
2 BO 2A
A2O
2 BO3
2 BO 4 2A
A2O
3
3
(1)
residual stresses due to temperature gradient, which is
produced by rapid cooling. The glasses were cooled to
room temperature within the furnace after annealing. Nomenclature of prepared glass samples contains six letters
(BSTKL and T) and four digit groups (5, 1 and 0.3 to 1.0
digit numbers). First three letters BST refers to barium
strontium titanate borosilicate. The term 5 K designates
the 5% of K2O while term L indicates, whether La2O3 is
used as donar dopants and the numeric term before L
denotes molecular percentage of La2O3. The last numeric
number denotes the content of strontium or composition,
x value.
(2)
The existence of four coordinated boron in alkalidoped borate glasses has been studied extensively for a
wide variety of modifiers through various spectroscopic
techniques such as IR, Raman, NMR, and NQR spectroscopy [9,10]. Recently, our group reported few publications on structural, crystallization and dielectric studies
of (Pb,Sr)TiO3 borosilicate glass and glass ceramics.
These studies shows very high dielectric constant and
La2O3 was act as nucleating agent as well as network modifier [11-13]. More recently, we are reported on results
of structure, crystallization kinematics of (Ba,Sr) TiO3
borosilicate glasses. These glasses are technologically
important for making optical active devices due to high
refractive index and their glass ceramics shows the sluggishness of the crystallization in glass matrix due to doping of La2O3 [14,15].
2. Experimental Procedure
2.2. Infrared Spectroscopy
The powdered glass samples were mixed with KBr powder and pressed as pellets. Then, these pellets are used as
samples for recording the IR spectra. The IR spectra of
BST borosilicate glasses are carried out using JASCO
FT/IR-5300 in the wave number range 450 - 4000 cm−1
at room temperature.
2.3. Raman Spectroscopy
The powdered glass samples are used as in the wave
number range from 200 - 1500 cm−1. Micro Raman setup,
Renishaw, UK, equipped with a grating of 1800 lines/
mm and Olympus (model MX-50) A/T was attached with
spectrometer which focuses laser light into sample and
collect the scattered at 1800 by scattering geometry. The
15.4 nm Ar+ laser was used as an excitation source and
GRAM-32 software for data collection.
2.1. Sample Preparation
2.4. UV-Vis Spectroscopy
High purity analytical reagent grade chemicals BaCO3
(Himedia 99%), SrCO3 (Himedia 99%), TiO2 (Himedia
99%), SiO2 (Himedia 99.5%), H3BO3 (Himedia 99.8%),
K2CO3 (Himedia 99.9%), La2O3 and (Himedia 99.9%)
were used for the preparation of various glass samples
having glass system 64[(Ba1-xSrx)TiO3]-30[2SiO2-B2O3]5[K2O]-1[La2O3] (x = 0.3, 0.5, 0.6, 0.8 and 1.0). Appropriate amounts of raw materials, as per the composition
of glasses, were properly weighed and mixed in an agate
mortar using acetone as mixing medium and dried the
powder. The glass batches of 20 grams were melted in a
high-grade alumina crucible in open air atmosphere using
a programmable electric furnace. The melting temperatures for different compositions were in the range 1050˚C
- 1450˚C. The melt was maintained at the melting temperature in the furnace for 10 minutes for refining and
homogenization. The melt was poured into an aluminum
mould and pressed by a thick aluminum plate then immediately transferred in to a preheated muffle furnace for
annealing at temperature 450˚C for 3 hours to remove the
UV-visible absorption spectroscopy is a very useful technique to characterizing the optical and electronic properties of different materials such as thin films, filters, pigments and glasses. Measurement of the optical band gap
of glass sample is carried out using the data within range
200 - 800 nm obtained by spectrophotometer. UV-vis
spectroscopy of the samples was carried out using UVvisible spectrophotometer (Varian, Carry-50Bio). It measures the percentage of radiation in the different regions
such as ultra-violet (200 - 400 nm) and visible (400 - 800
nm) regions that is absorbed at each wavelength within
ultra-violet and visible regions. Optical transitions are
basically two types, direct and indirect transitions. In
these transitions, the electromagnetic radiations interact
with the electrons in the valence band and which reaches
to conduction band by gaining fundamental band gap.
These transitions occur in both crystalline and amorphous semiconductor materials. These transitions are related with Mott and Davis relation. For photon energies
just above fundamental edge, the relation between ab-
Copyright © 2013 SciRes.
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C. R. GAUTAM, A. K. YADAV
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sorption coefficient (α) and photon energy is given below
[16,17]:
hν E g hν
n
(3)
where A is a constant related to the extent of the band
tailing, n = 1 2 for allowed direct transition, n = 2 for
allowed indirect transition, hυ is the photon energy and
Eg is the optical band gap energy of the material. The absorption coefficient, α, was calculated at different photon
energies by using the relation, α = A d , where A is the
absorbance and d the thickness of the samples. The optical band gap, Eg, was calculated by extrapolating the lin12
12
ear parts of the curves to hν 0 of curve hν
verses hυ and extrapolating for the glass samples.
2.5. Density Studies of Glass Samples
The density strongly depends on the composition and
structure of the samples Density of the glass samples
were determined by liquid displacement method of Archimedes principle [18]. Distilled water was used as the
liquid medium. Density of glass and glass ceramic samples were calculated using the formula:
W2 W1
W4 W1 W3 W2
(4)
ρ = Density (gram/cc);
W1 Weight of empty specific gravity bottle (gram);
W2 Weight of specific gravity bottle with sample
(gram);
W3 = Weight of specific gravity bottle with sample
and distill water (gram);
W4 = Weight of specific gravity bottle with distill water (gram).
Figure 1. IR spectra of BST borosilicate glass samples: (a)
BST5K1L0.3; (b) BST5K1L0.5; (c) BST5K1L0.6; (d) BST
5K1L0.8 and (e) ST5K1lL1.0.
3. Results and Discussion
3.1. Infrared Spectroscopy
The IR spectra for various glass samples of BST borosilicate glasses doped with La2O3 are shown in Figure 1.
IR spectra of all glass samples consist of various absorption bands in different regions lies between wavenumbers
450 - 4000 cm−1. These bands are influenced by doping
the variation in content of Ba/Sr ratio because the positions of some absorption bands are shifted due to compositional variations. Wavenumbers of different absorption
peaks for all the glass samples have been listed in Table
1. The first absorption band lies in wavenumber range
3440 - 3470 cm−1. The position of this broad band
slightly shifted towards lower wavenumber side with
increasing the concentration of Sr. This absorption band
occurs due to molecular water inside the glassy network
[19]. Absorption bands were observed in the wavenumber range 2853 - 2924 cm−1 and these absorption bands
Copyright © 2013 SciRes.
are attributed to formation of hydrogen bonding [20-22].
These bands are almost unaffected by the variations of
Ba/Sr ratio. An IR spectrum of these glass samples also
shows diffused absorption bands in wavenumbers range
2340 - 2365 cm−1. The doublet splitting was observed in
this band and attributed to -OH bonding vibrations which
are formed at non-bridging oxygen sites and hydroxyl
groups are usually present in borate glasses. The presence of -OH groups may due to the KBr pellet technique
used to record IR spectra [23]. There are few absorption
bands in the wavenumber range 1275 - 1739 cm−1 are observed due to the asymmetric stretching relaxation of the
B-O bonds of trigonal BO3 units. Such types of vibrational modes were observed within wavenumbers range
from 1200 - 1750 cm−1 [24,25]. The band at 1560 cm−1
was absent in all glass samples except glass samples
BST5K1L0.5 and BST5K1L0.6. The bands near wavenumber 1737 cm−1 are present only in barium rich glass
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Table 1. Peak positions in IR spectra of glass samples in the system 64[(Ba1-xSrx)TiO3]-35[2SiO2.B2O3]-5 [K2O]-1[La2O3].
Wavenumber of different absorption peaks (cm−1)
Glass samples code
1
2
4
3
5
a
b
6
7
8
9
BST5K1L0.3
3470
2924
2853
2365
2342
-
1343
983
707
467
BST5K1L0.5
3480
2923
2853
2365
2340
1560
1332
984
707
467
BST5K1L0.6
3450
2923
2853
2365
2348
1560
1340
992
719
479
BST5K1L0.8
3450
2923
2853
2365
2342
-
1332
991
719
467
ST5K1L1.0
3440
2924
2854
2364
2346
-
1356
992
707
464
Table 2. Peak positions in Raman spectra of different glass
samples in the glass system 64[(Ba1-xSrx) TiO3]-30[2SiO2.
B2O3]-5[K2O]-1[La2O3].
Glass sample code
Raman band positions (cm−1)
1
2
3
4
BST5K1L0.3
977
812
675
248
BST5K1L0.5
979
829
708
285
BST5K1L0.6
980
836
698
275
BST5K1L0.8
979
833
720
281
ST5K1L1.0
981
803
670
248
samples. This band was present due to the diborate linkage, B-O-B, in the borate glassy network. In this linkage
both boron atoms are tetrahedrally coordinated with triborate super structural units [27,28]. In these glass samples no absorption peak at 806 cm−1 was observed and it
confirms the absence of boroxol ring in glassy network.
The bands at low frequencies are observed in the IR
spectra of all glass samples and can be attributed to vibration of metal cation such as Ba2+ and Sr2+. The similar
bands were also present in IR spectra of PbO-B2O3
glasses and attributed to the vibrations of Pb2+ cations
[29]. Hence network-modifying behavior is observed in
which these ions enters the interstices of the network.
This is supports to our results, and network-modifying
behavior of BaO and SrO are observed.
3.2. Raman Spectroscopy
Figure 2. Raman spectra of BST borosilicate glass samples:
(a) BST5K1L0.3, (b) BST5K1L0.5, (c) BST5K1L0.6, (d)
BST5K1L0.8 and ST5K1lL1.0.
samples. A nonlinear trend for band near 1332 cm−1 was
observed. A broad absorption band at around 983 cm−1 is
attributed to a stretching vibration of B-O-Si linkage [26].
A weak absorption band is observed within the wavenumber range 707 - 719 cm−1 in IR spectra of all glass
Copyright © 2013 SciRes.
Raman spectra of different BST borosilicate glass samples doped with La2O3 are shown in Figures 2(a)-(e) and
the peak positions of Raman bands have been listed in
Table 2. Each Raman spectra indicate four different
kinds of peaks. Raman pattern of glass sample BST5K1L
0.3 is shown in Figure 2(a). It shows four broad and
overlaped peaks at different wavenumbers 248, 675, 812
and 977 cm−1. The Raman band at wavenumber 977 cm−1
was occured due to B-O− stretching in orthoborate units
[30]. The peak at 675 cm−1 is the characteristic of B-O-B
stretching in metaborate rings [31,32] while peak at wavenumber 812 cm−1 occurs due to symmetric breathing vibrations of boroxol rings [33,34]. Raman bands of glass
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C. R. GAUTAM, A. K. YADAV
sample BST5K1L0.5 shows four bands at various wavenumbers 285, 708, 829 and 979 cm−1 respectively (Figure 2(b)). The Raman band near 829 cm−1 is attributed to
B-O-B stretching in pyroborate units [31,32]. Figure 2(c)
depicts the Raman spectra of glass sample BST5K1L0.6
and showing three distinct peaks with different intensities
at wavenumbers 275, 698, 836 and 980 cm−1. These Raman bands were also present in glass samples BST5K1L
0.8 and ST5K1L1.0 with slight shifting in their wavenumbers (Figures 2(d)-(e)). The non linear variations
were observed with changing the Ba/Sr ratio in glassy
matrix. When the content of Sr was increased from 0.6 to
0.8 or 1.0, the band at 836 shifted towards lower wavenumber side. This may be due to non uniform variation
in symmetry and dipole moment during the measurements. The weak Raman peak were observed their spectra due to metalic cations towards low wavenumber side.
The assignment of IR and Raman bands in the spectra of
different glass samples are summarized in Table 3.
3.3. UV-Vis NIR Spectroscopy
UV-visible absorption spectra of various (BaSr)TiO3 borosilicate glass samples have shown in Figure 3. The
band gap, Eg for BST borosilicate glasses have been
listed in Table 4.
There is not any sharp increase in absorption at energies closed to the band gap that manifests itself as an
absorption edge in the UV-visible absorption spectra and
it is indicating the amorphous nature of glass samples. It
is observed that absorption edges shifted towards higher
wavelength side with to increasing concentration of SrO.
For pure Sr glass sample of composition, a drastic increase in its absorption edge at increasing the content of
SrO and which shows red shift due 580 nm, which shows
the translucency inside glass sample. The indirect optical
band gap of BST borosilicate glasses are determined by
using Davis and Mott relation as discussed in section 2.4.
The plot of hυ versus (αhυ)1/2 shown in Figure 4. The
optical band gap was found to be lie in range of 2.023 -
5
3.320 eV. The similar results were also reported on BaTiO3 by Suzuki [35]. The band gap decreases with increasing the concentration of SrO. This shows the composition dependence of optical band gap [36,37]. The
pure Sr content glass sample has lowest band gap value
2.023 eV. This sudden difference for band gap value may
be due to the variation of non-bridging oxygens. The
shift of the absorption edge to a higher wavelength or
decrease of Eg with increasing SrO content may be due to
more porous nature of Sr rich glass samples than that of
Ba rich glass samples, and also increased the oxygen
amount inside the samples. Hence, an increase in the formation of bridging oxygen (BO4 units) and which makes
the sample more semiconducting [38].
3.4. Density Studies
The density of BST borosilicate glasses was found between 2.55 - 2.84 gm/cc. It decreases with increasing
concentration of SrO in the BST borosilicate glasses
while it increases with increasing the concentration of
La2O3. This may be due to high density of Ba (3.51 g/cc)
and Sr (2.61 g/cc). Almost linear trend was observed in
the density of glasses following equation y = 3 − 0.46x
and this was shown in Figure 5. The values of density of
BST borosilicate glasses have been listed in Table 4.
4. Conclusion
Perovskite bulk transparent BST borosilicate glasses
were prepared successfully by rapid melt quench method.
The IR and Raman bands were found to be composition
dependent. IR spectra of BST borosilicate glass samples
shows that borate is major network former in this glass
system and it is also confirmed by Raman spectroscopic
studies. The vibrations due to metallic cations (Ba2+ and
Sr2+) are also play important role as a network modifier
at lower wavenumber sides in their IR as well as Raman
spectra. The optical band gap shows slight dependence
on compositions and it was found lowest for the glass
sample ST5K1L1.0 (2.023 eV).
Table 3. Assignment of infrared and Raman bands in the spectra of different glass samples.
Wave number (cm−1)
IR assignments
IR
Raman
471 - 523
248 - 285
Vibrations of metal cations such as Ba2+, Sr2+
722 - 828
670 - 720
bonding of B-O-B linkages (diborate linkage)
1035
803 - 812
stretching vibration of B-O-Si linkage
1200 - 1635
820 - 836
2292 - 2376
977 - 981
asymmetric stretching relaxation of the B-O bond of
trigonal BO3 units
-OH bonding
Raman assignments
Vibrations of metal cations are observed
B-O-B stretching in metaborate rings or B-O-B stretching
in metaborate chains
Symmetric breathing vibrations of
boroxol rings
B-O-B stretching in pyroborate units
B-O− stretching in orthoborate units
2700 - 3000
-
Hydrogen bonding
-
3391 - 3435
-
Molecular water
-
Copyright © 2013 SciRes.
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C. R. GAUTAM, A. K. YADAV
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Table 4. Optical band gap and density of glass samples in
the system 64[(Ba1-xSrx).TiO3]-35[2SiO2.B2O3]-5[K2O]-1[La2
O3].
Compositions (x)
Glass codes
Optical band
gap (eV)
Density
(gram/cc)
0.3
BST5K1L0.3
3.320
2.84
0.5
BST5K1L0.5
3.315
2.80
0.6
BST5K1L0.6
3.311
2.775
0.8
BST5K1L0.8
3.307
2.6
1.0
ST5K1L1.0
2.023
2.55
5. Acknowledgements
Figure 3. UV-visible absorption spectra of all BST borosilicate glass samples.
The authors are gratefully acknowledged to the University Grant Commission (UGC), New Delhi, (India) for
financial support under the major research project F. No.
37-439/2009 (SR).
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Figure 4. Davis and Mott plot of hυ versus (αhυ)1/2 of glass
sample (a) BST5K1L0.3, (b) BST5K1L0.5, (c) BST5K1L0.6,
(d) BST5K1L0.8 and (e) ST5K1lL1.0.
Figure 5. Variation of density vs content of Sr.
Copyright © 2013 SciRes.
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