Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System presented Seminar Kebangsaan Aplikasi Sains dan Matematik 29-30 October 2013 ata UTHM Johor

1. Seminar Kebangsaan Aplikasi Sains dan Matematik (SKASM2013)
29-30 Oktober 2013 @ UTHM Johor
Synthesis
and Elastic
Studies of
Lead BoroTellurite
Glass
System
H. A. A. Sidek, Z. A. Wahab, K. A. Matori and M. K. Halimah
Glass Ceramic Composite Research Group (GCCG)
Department of Physics, Faculty of Science
Universiti Putra Malaysia
43400 UPM Serdang, Selangor, Malaysia

2. Introduction
Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
Introduction
Experimentals
Results & Discussion
Glass: Unique
properties
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Conclusions
Acknowledgement
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References
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widely used in applications
from medicine to transport to
space flight.
promising media for the
development of photonic
devices
basic elements for the
advance of optical
communication networks and
optical computing
potential applications in
various engineering and
technological fields
lower production costs with
respect to single crystals
• amorphous (noncrystalline) solid
material
• optically transparent
• typically brittle
• sufficient strength
• excellent corrosion
resistance

3. Introduction ..
Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
Introduction
Experimentals
Tellurite glasses are potentially applied in
industries of electric, optical, electronic
and etc due to their good physical
properties (Khattak and Salim, 2002).
Laser Quality Tellurium – an excellent
piezo-optical material.
TeO2 Glass
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Results & Discussion
Conclusions
Acknowledgement
References
High acousto-optical in
making:•
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acousto-optical modulators.
imaging devices
splitters
deflectors
tunable polarization filters
radio frequency spectral analysers
CD memory device
Non-linear optical devices
Electrochemical devices
Optical switching device
Laser host
Infra-Red Fiber Optics
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transparent in the visible and near IR
regions from 400 nm to 6 micron m
high refractive index n > 2, which
allows the fabrication of fibers and
waveguides with strong light
confinement
highest values of nonlinear refractive
about 10–100 times larger than
fused silica: essential for active
nonlinear photonic devices, i.e. alloptical switches or modulators
Glasses with heavy metal oxides
(TeO2, GeO2, Bi2O3, WO3, PbO,
Ag2O, etc.) are promising materials
for IR technologies, nonlinear optics,
and design of laser devices.
Low fusion temperature (800 oC)

4. Introduction …
Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
Introduction
Experimentals
Results & Discussion
Conclusions
Acknowledgement
References

5. Borate Glass ….
Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
Introduction
Boro-tellurite glasses
Experimentals
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Results & Discussion
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Conclusions
Acknowledgement
References
Binary borate glasses
(MO)x(B2O3)1-x
MO represents the oxides etc.
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Interesting physical properties
for technological applications
Non-linear optical properties
Pure boron trioxide B2O3 is
covalently bonded with
interesting physicochemical
properties
B2O3 shows unique structural
properties (boron anomaly) with
BO3 convert to BO4
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industrial importance material in
making glasses with desirable optical
properties
Both B2O3 and TeO2 are present in
boro-tellurite glass, leads to complex
specification in the glass structure
TeO2 and B2O3 are glass forming
oxides
Tellurite glass has laminar network
structure based on triangular TeO3
pyramids or square TeO4 pyramids
B2O3 in its glassy form is a laminar
network with boron atoms 3-fold
coordinated with oxygen form sixmembered boroxol rings (B3O6)

6. Tellurite Glass …..
Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
Introduction
Experimentals
Results & Discussion
Conclusions
Acknowledgement
References

7. Lead BoroTellurite
Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
Introduction
Lead Boro-Tellurite
Experimentals
•
Results & Discussion
Conclusions
Acknowledgement
References
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Pb gives excellent
infrared transmission
(high refractive index)
compared with
conventional glass
Glasses containing
heavy-metal oxides
has potential
application in radiation
shielding

8. Abstract
Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
Introduction
Experimentals
Results & Discussion
Conclusions
Acknowledgement
References
This paper reports the physical and
elastic properties of the
(PbO)x(B2O3)y(TeO2)z (where x = 10–
30, y = 21–36 and z = 42 – 63 mol%)
ternary lead boro tellurite (PBT) glass
system.
The PBT glass series were synthesized
by the conventional rapid melt
quenching technique.
The composition dependence of the
physical, mainly density and molar
volume, and elastic properties are
conferred in term of the PbO
modifiers addition that are likely to
produce quite significant changes in
their properties.
The lack of any crystalline peaks in the
X-ray diffraction (XRD) patterns of the
present glass samples designates the
amorphous nature.
The addition of PbO increased the values of the
densities in ternary PBT glass systems.
The longitudinal and transverse ultrasonic waves
propagated in each glass sample were measured
using a MBS8020 ultrasonic data acquisition
system at 15 MHz resonating frequency and at
room temperature.
The longitudinal modulus (L), shear modulus (G),
Young’s modulus (E), bulk modulus (K) and
Poisson’s ratio ( ) are obtained from both
velocities data and their respective density.
Experimental data shows the density and elastic
moduli of each PbO–B2O3-TeO2 series are found
strongly depend upon the glass composition.
The addition of PbO modifiers into the
borotellurite causes substantial changes in their
density, molar volume as well as their elastic
properties.

9. Experimental Methods
Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
Introduction
•
Experimentals
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Results & Discussion
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Conclusions
Acknowledgement
References
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Ternary (TeO2)y
[(PbO)x (B2O3)1-x]1-y
glass system
prepared using a
conventional meltquenching method
All samples are
homogenous,
transparent and
bubble free
TeO2 (Alfa Aesar
99.99%), lead
oxide, litharge PbO (99%) and
boron oxide - B2O3
(Alfa Aesar, 97.5%).

10. Results and Discussion
Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
Introduction
Experimentals
Results & Discussion
Conclusions
Acknowledgement
DTA measurement
using SETARAM
X-ray diffraction using
an X-ray diffractometer (Philips
X’pert Pro Panalytical)
IR and Raman spectroscopy
using a Raman spectrometer
(RSI 2001 B, Raman system, INC)
References
Elastic Properties
Using MBS 8000 Ultrasonic Data
Acquisition System

11. Composition and Density
Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
Introduction
Experimentals
Results & Discussion
Conclusions
Acknowledgement
References
Density
Measurement
(Archimedes
Method)
Molar
volumes
a

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s   wawwac  ac
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V 
M
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Volume occupied by one mole of
material
Density is defined as the
mass per unit volume.
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Intrinsic property of
matter, meaning it
remains the same
regardless of sample
size.
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Important property
capable of evaluating the
compactness and casting
the light on the short
range structure of the
glass.
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It is considered a
characteristic property of
a substance and can be
used for material’s
classification

12. Composition – Density …
Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
TeO2 – B2O3 glass
The density and the molar
volume of this glass system
increases with increase in mole
percentage of TeO2 /PbO is due
to the atomic weight and size of
the constituent oxides.
Introduction
Experimentals
Results & Discussion
Conclusions
TeO2- PbO – B2O3 glass
PbO – B2O3 glass
References
Density (g/cc)
Acknowledgement
PbO (mol%)

13. Thermal Properties
Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
Introduction
Experimentals
Results & Discussion
Conclusions
Acknowledgement
References
Studies of the thermal
stability and crystallization
behaviour in TeO2 based
glasses

14. XRD Pattern
Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
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Introduction
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Experimentals
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Results & Discussion
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Conclusions
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Acknowledgement
References
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Intensity (a.u)
3400
3200
3000
2800
2600
2400
2200
2000
1800
1600
1400
1200
1000
800
600
400
200
0
10
20
30
2 theta
40
50
TeO2 powder
The XRD pattern show the partially
crystalline precipitation.
the partially crystalline glass fit the
amorphous state as the amount of
PbO increases.
The presence of broad peak for 2θ
around 20° - 35°.
XRD reflections were assigned to
the two polymorphic phases;
hexagonal of tellurium and
monoclinic of lead tellurite.
The intensity of the XRD reflections
indicate that more monoclinic
crystals are reduced in quenched
samples as the intermediate content
increases.
The structures of lead tellurite
contain Pb3TeO6 probably
consisting of TeO3 trigonal pyramid
connected by 3(PbO) tetragonal
forming a three-dimensional
network.

15. Raman Spectra
Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
•
Introduction
Experimentals
Results & Discussion
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Conclusions
Acknowledgement
References
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Raman spectra show increasing peak at <100cm-1 which
indicates the strong presence of Pb in the chemical bonding
through vibrational mode due to addition of PbO.
Decreasing on (symmetry stretching) Te-O-Te and B-O-B
bending shoulder at approximately 490 cm-1 and 450 cm-1
ascribe that the splitting of Te-O-Te and B-O-B bonds and hence,
the bridging oxygen’s (BOs) are converted into NBOs.
The spectral features from
710 cm-1 to 730 cm-1 and
790 cm-1 correspond to the
TeO4 bi-pyramidal
arrangement and the
TeO3+1 (or distorted TeO4)
and TeO3 trigonal pyramids
structures respectively.
It can be clearly observed
that the evolution of TeO3+1
and TeO3 units occurs as
the TeO2 concentration
decreases.
The increasing peak on the
TeO3 trigonal pyramids
shows that modification of
lattice and interstitial
occurs in the system.

16. Elastic Properties
Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
Elastic Properties
Introduction
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Experimentals
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Results & Discussion
Conclusions
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Acknowledgement
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References
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Provide information about
the structure of solids
internal arrangement of the
constituent oxides
directly related to the
interatomic potentials
Estimate the mechanical
strength of the solids
Elastic moduli (longitudinal,
shear, bulk and Young’s),
Debye temperature ,
Poisson’s ratio and etc.

17. Elastic Properties
Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
Elastic Behaviour of TeO2-B2O3 glass
Wave Velocity (m/s)
Experimentals
Results & Discussion
Acknowledgement
References
The results of the elastic moduli
and those of Poisson’s ratio, micro
hardness, softening temperature
and Debye temperature shows a
tightening in the bonding of the
glass structure and increase in
rigidity of the glass structure.
VL
VS
Elastic Constant (GPa)
Introduction
Conclusions
PbO – B2O3 glass
L
E
K
G
PbO (mol%)

18. Conclusions
Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
Introduction
•
Experimentals
Results & Discussion
Conclusions
•
Acknowledgement
References
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Lead Borate, Boro-Tellurite
and Lead-boro tellurite
glasses were successfully
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prepared by melt
quenching techniques.
The structural rigidity and
compactness of the glass
were determined from the
measurement of density
and differential thermal
•
analysis (DTA).
Their respective glass
structure were estimated
using Raman scattering.
For Lead borate and Lead
borotellurie, the addition of PbO
results leads to the increasing of
density and molar volume.
However, the accumulation of
PbO results in splitting of O-Te-O
and B-O-B bonds and hence, the
bridging oxygen’s (BOs) are
converted into NBOs besides
which leads to decrease the
rigidity in the glass network.
Experimental data shows the
density and elastic moduli of
each PbO–B2O3-TeO2 system are
found strongly depend upon the
glass composition.

19. Acknowledgement
Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
Introduction
Experimentals
Results & Discussion
Conclusions
Acknowledgement
References
•
The author gratefully acknowledged Ministry
of Science and Innovation (MOSTI), Ministry
of Education (MoE) and University Putra
Malaysia for financial assistance.

20. References
Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
Introduction
Experimentals
Results & Discussion
Conclusions
Acknowledgement
References