Open Journal of Inorganic Non-metallic Materials, 2012, 2, 47-54
doi:10.4236/ojinm.2012.24005 Published Online October 2012 (http://www.SciRP.org/journal/ojinm)
Synthesis, IR and Raman Spectroscopic Studies of
(Ba,Sr)TiO3 Borosilicate Glasses with Addition of La2O3
Chandkiram Gautam1*, Avadhesh Kumar Yadav1, Vijay Kumar Mishra2, Kunwar Vikram2
1
Department of Physics University of Lucknow, Lucknow, India
Department of Physics, Banaras Hindu University, Varanasi, India
Email: *gautam_ceramic@yahoo.com
2
Received July 1, 2012; revised August 6, 2012; accepted September 1, 2012
ABSTRACT
A series of glasses were prepared by rapid melt quench method in the glass system (65 − x)[(Ba0.6Sr0.4)TiO3]30[2SiO2-B2O3]-5[K2O]-x[La2O3] (x = 0, 1, 2, 5 and 10). X-ray diffraction of glass samples were carried to check its
amorphousity. Density of glass samples were measured using Archimedes principle. The refractive index of these glass
samples lies between 2.39 to 2.80. Optical properties of these glass samples were studied using Infrared (IR) and Raman
spectroscopic techniques. IR measurements were done over a continous spectral range 450 - 4000 cm–1 to study their
stucture networking systematically while Raman spectra were recorded over a continous spectral range 200 - 2000 cm–1.
IR spectra of all glass samples showed number of absorption peaks. These absorption peaks occurs due to asymetric
vibrational streching of borate by relaxation of the bond B-O of trigonal BO3. The Raman spectra of all glass samples
exhibited different spectral bands and intensity of these bands changes drastically. The network structure of these glass
samples is mainly based on BO3 and BO4 units placed in different structural groups.
Keywords: Glasses; X-Ray Diffraction; Inferared Spectroscopy and Raman Spectroscopy
1. Introduction
Glasses in the system PbO-B2O3-SiO2 and PbO-Al2O3B2O3-SiO2 have different applications, such as thick film
technology ink constituents, mixed oxide dielectrics
(MODs) and host for fluorescence centers in optical devices. These glasses are chemically stable over a wide
composition range and have a desirable electrical resistivity. The lead borosilicate glasses are used as radiation
hard glasses [1]. Vibrational spectroscopy has been used
for long time to investigate the structure of glasses and
the identification of the main structural groups [2-4].
Infrared spectroscopy has very useful technique because
it provides a means to determine local structure of building units which constitutes the glassy network [5]. Borates and borosilicate glasses containing boron oxide
have been widely used for optical lenses with high refractive index and low dispersion characteristics [6]. The
oxide glasses have wide applications in the fields of electronics, nuclear and solar energy technologies and
acoustic-optic devices [7-11]. Glasses based on boron
oxide exhibit structural chemistry of structure. Boron is
commonly found in the glasses in the form of triborate
and tetraborate units [12]. Alkali borate glasses are best
glass forming systems for demonstrating the effectiveness of the spectroscopic technique in the glass science
*
Corresponding author.
Copyright © 2012 SciRes.
[13]. IR spectra of (Pb,Sr)TiO3 borosilicate glass system
show sharp and diffuse absorption peaks. These peaks
occur due to different vibrational mode of the borate
network and asymmetric stretching relaxation of the B-O
bond of trigonal BO3 units. Vibrational spectra of PbOBi2O3-B2O3 glasses show the formation of broad bands.
IR studies of ZnO-PbO-B2O3-SiO2 glasses shows absorption bands due to bond breaking between the trigonal
elements BO3 and allowing the formation of BO4 units.
The structure of Zn-doped borate glass consists of randomly connected BO3 and BO4 groups. The IR spectra of
ZnO-PbO-B2O3 glasses show eight to nine absorption
peaks [14,15]. Low frequency bands in the IR spectra of
these glasses can be attributed to vibration of metal cation such as Pb2+. The broad bands are exhibited in the
oxide spectra due to the combination of high degeneracy
of vibrational states [16,17]. IR spectra of lead silicate
glasses were exhibited due to bending modes Si-O-Si and
O-Si-O as well as symmetric stretching of bridging oxygen between tetrahedra [18]. IR study of lithium borate
glasses show cleared and disappearance of boroxol rings
with the formation of BO4 groups [19]. Recently, IR
studies of B2O3-ZnO-TeO2 glass system gives absorption
bands due to vibrational Te-O bond stretching. B-O
linkages in the borate network of B-O-B bending vibrations in BO4 units and H-O-H or water groups are present
in these glasses [20]. Raman spectroscopy is a very useOJINM
C. GAUTAM ET AL.
48
ful tool to provide valuable information about impurities,
internal stress, crystal symmetry and bond nature [21-26].
IR and Raman studies on lithium-potassium-borate glasses exhibited due to vibrational stretching of borate network of the BO3 and BO4 units placed in different structural groups [27]. The various structural groups of borate
network are shown in Figure 1 [27,28].
Raman spectroscopy of epitaxial barium titanate, BT,
thin film shows both paraelectric to ferroelectric phase
transformations. The diffuse phase transition is confirmed by the gradual decrease of the intensities of the
overdamped soft mode and the tetragonal Raman shift
[29]. Raman spectra of hetero-epitaxial BST prepared on
MgO substrates were obtained in side-view backscattering geometry and causes local distortions of the
Ti-O-Ti chains [30]. Vibrational spectra of BT single
crystals have been studied and give displacive orderdisorder crossover [31-36]. Recently, IR and Raman spe-
(a)
(b)
(c)
ctroscopic studies have been done on alkaline-earth silicate glasses by Angelos G Kalampounias [37]. This study shows the vibrational spectra due to vibrational stretching of Si-O in (Si-OH) silanol groups. BST borosilicate glasses have potential applications in making high
refractive index glasses for optical devices and their glass
ceramics are used for making electronic devices, such as
barrier layer capacitor. In this research paper we are reporting our results on optical properties of BST borosilicate glasses with doping effect of La2O3.
2. Experimental Procedure
The high purity of AR grade chemicals BaCO3 (Himedia
99%), SrCO3 (Himedia 99%), TiO2 (Himedia 99%), SiO2
(Himedia 99.5%), H3BO3 (Himedia 99.8%), K2CO3 (Himedia 99.9%) and La2O3 (Himedia 99.9%) were mixed
for 1.0 hour in acetone media using mortar and pestle.
(d)
(h)
(e)
(i)
(f)
(g)
(j)
(k)
Figure 1. Structural groups found in glassy and crystalline potassium borates: (a) boroxol ring; (b) nonring BO3; (c) nonring
BO 4 ; (d) triborate; (e) diborate; (f) pentaborate; (g) di-triborate; (h) tetraborate; (i) ring-type metaborate; (j) chain-type
metaborate (k) combination of triborate and pentaborate units. Filled circles and open circles represent boron and oxygen
atoms, respectively. Dashed lines in the structures denote connections to the network, and chargesare shown for the nonbridging oxygen (NBO) in the metaborate groups [27,28].
Copyright © 2012 SciRes.
OJINM
C. GAUTAM ET AL.
The well mixed and dried powder were transfered in to a
high alumina content crucible and then crucible is replaced inside the high temperature SiC electric furnace in
the temperature range 1200˚C - 1350˚C. 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
up to 3 hours. XRD patterns of glass samples were recorded using a Rigaku Miniflex-II X-ray diffractometer
using Cu-K radiation for checking amorphous nature
glass samples. The glass samples were prepared for measurement of refractive index. The five glass samples were
designed of having equal thickness (0.7 mm) along with
equal area (25 mm2). These samples were polished with
different mesh of SiC powder to get the smooth surfaces.
Electroding has been done on the both polished surfaces
of all glass samples with silver palladium paste and then
electroded samples were dried in a preheated oven at
200˚C. Finally, well dried glass samples were carried out
for their capacitance measurement at room temperature.
The density of glass samples depends upon doping concentration of La2O3. Therefore, it is worth-while to calculate the density of the prepared glass samples. The
density of all glass samples were calculated by using
Archimedes Principle [40]. Distilled water was used as
the liquid medium. The density of these glass samples
were listed in Table 1. The following formula was used
for determination of the density of glass samples.
W2 W1
Density
(1)
W4 W1 W3 W2
where, W1 = weight of empty specific gravity bottle (in
gram);
W2 = weight of specific gravity bottle with sample (in
gram);
W3 = weight of specific gravity of bottle with sample and
distilled water (in gram);
W4 = weight of specific gravity bottle with distilled water
(in gram).
Density of distilled water = 1.0 gm/cm3
The powdered glass samples were mixed with KBr
49
powder and pressed as pellets. These pellets are carried
out for the recording of IR spectra using JASCO FT/
IR-5300 in the wave number range 450 - 4000 cm–1 at
room temperature. Micro Raman setup, Renishaw, UK,
equipped with a grating of 1800 lines/ mm and Olymapus
(model MX-50) A/T was attached with spectrometer
which focuses laser light into sample and collect the
scattered at 180˚ by scattering geometry. The 15.4 nm
Ar+ laser was used as an excitation source and GRAM-32
software for data collection. Raman spectra of powdered
glass samples were also recorded in the wave number
range 200 - 2000 cm–1.
3. Results and Discussion
3.1. X-Ray Diffraction Analysis
The XRD patterns of all glass samples are shown in Figure 2. These figures exhibit a broad diffuse scattering at
different angles instead of crystalline peaks, confirming a
long range structural disorder characteristic of amorphous network.
3.2. Density Analysis of Glass Samples
The density of BST borosilicate glass samples doped
with La2O3 is listed in Table 1. The variation of density
Vs doping concentration of La2O3 is shown in Figure 3.
With increasing doping concentration of La2O3 increases
the density of the glass samples. The density of BST
borosilicate glass without doping of La2O3 was calculated
2.67 gm/cc. This is because of high density of La is 6.17
gm/cc whereas density of Ba and Sr are 3.5 and 2.6
gm/cc.
3.3. Dielectric Constant and Refractive Index
The dielectric constant for all glass samples are measured,
by measuring their capacitance measurement at room
temperature and 50 Hz frequency, using the relation
C = εoA/d
(2)
where “εo” denotes the permittivity in air, “A” denotes the
area of samples and “d” denotes the thickness of samples.
Table 1. Glass samples code, compositional distribution of different constituents, density, dielectric constant and refractive
index of glass samples.
(Ba0.6Sr0.4)TiO3
Glass samples code
weight %
Dielectric constant
(2SiO2-B2O3)
K2O
La2O3
Density
(gm/cc )
Dielectric
constant = 2.2 × εr= ε/εo
density
Refractive index
Calculated
Experimental
BST5K0.4
65
30
5
0
2.67
5.87
5.71
2.42
2.39
BST5K1L0.4
64
30
5
1
2.69
5.92
5.76
2.43
2.40
BST5K2L0.4
63
30
5
2
2.85
6.27
6.15
2.50
2.48
BST5K5L0.4
60
30
5
5
2.98
6.56
6.50
2.56
2.55
BST5K10L0.4
55
30
5
10
3.10
6.82
7.80
2.61
2.80
Copyright © 2012 SciRes.
OJINM
C. GAUTAM ET AL.
50
Intensity (a.u.)
the relative dielectric constant.
The refractive index of these glass samples are listed
in Table 1. The measured refractive indices are of same
order, which are calculated by two methods. The refractive of glass sample BST5K1L0.4 is found to be 2.43
whereas for glass sample BST5K2L0.4 is 2.50. It is observed from Table 1 the refractive index of glass samples
are increases with increasing the concentration of La2O3.
It is because of the refractive index of La2O3 is very high.
The refractive indices of all glass samples were found to
be more than 2. Therefore, these glass samples are useful
for making lenses application in small optical devices
such as smart phones with a digital camera, endoscopes,
and next-generation optical disk systems [39]. These results indicate that the La2O3 doped BST borosilicate glass
system would be useful for optical applications in the
visible to infrared region.
20
40 50 60
(degree)
30
70
80
Figure 2. XRD pattern of BST borosilicate glass samples.
3.2
Density (gm/ cc)
3.1
3.0
2.9
2.8
2.7
2.6
0
2
4
6
8
10
Weight % of La2O3
Figure 3. Density of glass samples vs doping concentration
of La2O3.
The numerical value of dielectric constant can be estimated for most industrial glasses by using the empirical
formula [38]:
Dielectric constant = 2.2 × density
(3)
The dielectric constants calculated by both methods
are comparable which are listed in Table 1. The refractive index of BST borosilicate glass samples were calculated by using the relation between refractive index and
dielectric constant.
n = (εr)1/2
(4)
where n is the refractive index of the material and εr is
Copyright © 2012 SciRes.
3.4. Infrared Spectroscopy
The IR absorption spectra gives significant information
about molecular vibrations as well as rotation associated
with a covalent bond. The IR spectra occur due to change
in the dipole moment of the molecule. It involves the
twisting, bending, rotating and vibrational motions in a
molecule. IR spectra of various BST borosilicate glasses
doped with La2O3 are shown in Figure 4. IR spectra of
all glass samples consist of broad and sharp bands in
different regions lies between wavenumbers 450 - 4000
cm–1. These bands are strongly influenced by doping of
La2O3. Wavenumbers of different absorption peaks for
all the glass samples are listed in Table 2. All the absorption peaks have been marked as numbered 1, 2, 3,…,
8 starting from high wave number side to low wave number side. The broad bands are exhibited in the oxide
spectra, most probably due to the combination of high
degeneracy of vibrational states, thermal broadening of
the lattice dispersion bands and mechanical scattering
from powder samples [40]. The first absorption peak lies
in the wavenumber range 3467 - 3479 cm–1. This absorption peak is sharp in glass sample BT5K10L0.4 in comparison to other glass samples. The sharpness of this
peak increases by increasing the doping concentration of
La2O3. This band occurs due to molecular water inside
the glassy network [41]. The absorption peaks 2 and 3
were found in all glass samples and lies within wavenumber 2852 - 2925 cm–1. The absorption band of this
wavenumber range occurs due to hydrogen bonding in
the glassy matrix [42]. IR spectra of various glass samples show sharp and diffuse absorption peaks in wavenumbers range 2346 - 2380 cm–1 (peak no. 4 a, b). This
peak shows a splitting into two closed doublet peaks with
different peak position in their IR spectra. The sharpness
of the peaks decreases by increasing the doping concentration of La2O3. This absorption band attributed to O-H
OJINM
C. GAUTAM ET AL.
51
Table 2. Peak positions in IR spectra of glass samples in the system (65 − x)[(Ba0.6Sr0.4)TiO3]-30[2SiO2.B2O3]-5[K2O]-x[La2O3].
Wave length of different absorption peaks (cm−1)
Glass samples code
1
2
4
3
a
b
5
6
7
8
-
988
707
BST5K0.4
3479
2924
2853
2365
2346
1328
BST5K1L0.4
3467
2923
2852
2366
2346
1351
-
991
704
BST5K2L0.4
3467
2925
2854
2380
-
1355
1204
983
715
BST5K5L0.4
3467
2925
2854
2380
2346
1348
1208
960
715
BST5K10L0.4
3468
2925
2854
-
2346
1352
1196
971
712
(a)
Transmitance (A.U.)
(b)
(c)
3.5. Raman Spectroscopy
(d)
(e)
4000 3500
(peak no. 6) is attributed to stretching vibrations of BO-Si linkage [45]. An absorption peak no.8 is observed
with wavenumber range 704-715 cm–1 in the IR spectra
of all glass samples. This peak was present due to the
diborate linkage of B-O-B, in the borate glassy network.
In this linkage both boron atoms are tetrahedrally coordinated with triborate superstructural units [46]. Assignment of Infrared bands in the spectra of different
glass samples is listed in Table 3. The addition of La2O3
increases the sharpness of the absorption peaks and decreases the broadness of absorption peaks.
3000 2500 2000 1500
Wavenumber (cm-1)
1000
500
Figure 4. IR spectra of BST borosilicate glass samples (a)
BST5K0.4; (b) BST5K1L0.4; (c) BST5K2L0.4; (d) BST5K5L0.4 and (e) BST5K10L0.4.
bond groups. These O-H bond groups are formed at nonbridging oxygen sites. A broad peak no. 5 is observed
with wavenumbers range 1196 - 1296 cm–1 in the IR
spectra of glass samples containing amount of La2O3 (x =
2, 5 and 10) while this peak is absent for glass samples
BST5K0.4 and BST5K1L0.4. Generally absorption bands
occur due to the vibrational mode of the borate network
in such type glass system. The vibrational modes of the
borate network are mainly due to the asymmetric stretching relaxation of the B-O bonds of trigonal BO3 units.
Such type of vibrational modes occurs within the wavenumbers range 1200 - 1750 cm–1 [43,44]. The broad absorption band around wavenumbers, 960 - 991 cm–1
Copyright © 2012 SciRes.
Raman spectroscopy is one of the powerful techniques to
investigate the structure of a material. Raman spectra of
various BST borosilicate glass samples doped with La2O3
are shown in Figures 5(a)-(e). Raman spectra of these
glasses indicate two peaks at different position. Figure
5(a) shows Raman spectra of glass sample BST5K0.4 (x
= 0) without doping of La2O3. In this spectral pattern,
two separate peaks were observed at wavenumbers 675
and 820 cm–1. The peak at 675 cm–1 was attributed to
metaborate groups while peak at wavenumber 820 cm–1
occurs due to symmetric breathing vibrations of sixmember rings with one or two BO3 triangles replaced by
BO4 tetrahedra [47]. The Raman spectra of glass sample
BST5K1L0.4 doped with 1 wt% of La2O3 is shown in
Figure 5(b). Raman spectra of glass sample BST5K2L0.4
doped with 2 wt % La2O3 depict three peaks at wavenumbers 283, 708 and 830 cm–1 respectively (Figure
5(c)). The peak at 708 cm–1 is the characteristic of Symmetric breathing vibrations BO3 triangles replaced by
BO4 tetrahedra. An extra peak at low wavenumber, 283
cm–1 was also observed. This peak occurs due to La-O
and K-O (metalic cations) bonding vibrations. Figure
5(d) shows Raman spectra of glass sample BST5K5L0.4
doped with 5 wt% of La2O3. This spectra represents three
peaks at wavenumbers 288, 697 and 841 cm–1 respectively. A shifting in the peak was also observed due to
increase in doping concentration of La2O3. Raman spectra of glass sample BST5K10L0.4 doped with 10 wt % of
La2O3 are shown in Figure 5(e). Three peaks were also
OJINM
C. GAUTAM ET AL.
52
Table 3. Assignment of Infrared and Raman bands in the spectra of different glass samples.
Wave number (cm−1)
IR assignments
Raman assignments
283 - 292
Vibrations of metal cations such as Ba2+, Sr2+
Metal cations bond vibrations
704 - 715
675
Bonding of B-O-B linkages (diborate linkage)
metaborate groups
960 - 991
700 - 725
Stretching vibration of B-O-Si linkage
Symmetric breathing vibrations BO3 triangles
replaced by BO4 tetrahedral units
1196 - 1355
820 - 850
Asymmetric stretching relaxation of the B-O bond of
trigonal BO3 units
symmetric breathing vibrations of six-member
rings with one or two BO3 triangles replaced by
BO4 tetrahedra
2346 - 2380
-
IR
Raman
471 - 523
-OH bonding
2852 - 2925
-
Hydrogen bonding
-
3467 - 3469
-
Molecular water
-
(a)
Raman shift variation
840
Intensity (A.U.)
(b)
830
820
810
(c)
800
0
(e)
600
400
200
Figure 5. Raman spectra of BST borosilicate glass samples
(a) BST5K0.4; (b) BST5K1L0.4; (c) BST5K2L0.4; (d) BST5K5L0.4 and (e) BST5K10L0.4.
observed at different wavenumbers, 292, 720 and 796
cm–1 in the Raman spectra of this glass sample. The second peak is closed to the first peak (796 cm–1). In other
words, we can say that this peak is shifted towards higher
wavenumber side because of high doping concentration
Copyright © 2012 SciRes.
8
10
Figure 6. Variation of raman shift with respect to doping
concentration of La2O3.
(d)
2000 1800 1600 1400 1200 1000 800
Raman Shift (cm-1)
2
4
6
Weight % of La2O3
of La2O3. The Raman shifting was observed with increasing the doping concentration of La2O3 which is
shown by the two parallel lines in Figure 5. The variation of the peak position in Raman spectra was observed
with varying concentration of La2O3. Variation of Raman
shift with respect to doping concentration of La2O3 is
shown in Figure 6. Assignment of Raman bands in the
spectra of different glass samples is also listed in Table 3.
Raman spectra show a shifting in the peaks towards high
wavenumber side from 0 to 5 wt% of La2O3 while this
shifting is going towards low wavenumber side for 10
wt% of La2O3.
4. Conclusion
Bulk transparent glasses were prepared successfully in
the BST borosilicate glass system with and without doping of La2O3. The absorption peaks occur in IR spectra is
due to different vibrational modes of the borate network
and asymmetric stretching relaxation of the B-O bond of
OJINM
C. GAUTAM ET AL.
BO3 units. The addition of La2O3 decreases the sharpness
of peaks and increases the broadness of absorption peaks
in their IR spectra because La2O3 acts as network modifier for this glass system. Raman spectra of all BST glass
samples are observed in several spectral bands. These
bands are attributed to symmetric breathing vibrations of
six-member rings with one or two BO3 triangles replaced
by BO4 tetrahedra, La-O and K-O bonding vibrations. As
increasing the doping concentration of La2O3 the intensity of the peaks are also increases. These results indicate
that the La doped BST borosilicate glass system may be
useful for optical applications in the visible to IR region.
5. Acknowledgements
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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