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
Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
Seminar Kebangsaan Aplikasi Sains dan Matematik (SKASM2013) 29-30 Oktober 2013 @ UTHM Johor
Introduction
Experimentals
Results & Discussion
Conclusions
Acknowledgement
References
Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
Introduction
Glass: Unique properties • 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 (non-
crystalline) solid material
• optically transparent
• typically brittle • sufficient strength • excellent corrosion
resistance
Introduction
Experimentals
Results & Discussion
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Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
Introduction ..
TeO2 Glass • 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. all-optical 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)
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.
High acousto-optical in making:-
• 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
Introduction
Experimentals
Results & Discussion
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Acknowledgement
References
Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
Introduction …
Introduction
Experimentals
Results & Discussion
Conclusions
Acknowledgement
References
Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
Borate Glass ….
Boro-tellurite glasses • 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 six-membered boroxol rings (B3O6)
Binary borate glasses
(MO)x(B2O3)1-x
MO represents the oxides etc.
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
Introduction
Experimentals
Results & Discussion
Conclusions
Acknowledgement
References
Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
Tellurite Glass …..
Introduction
Experimentals
Results & Discussion
Conclusions
Acknowledgement
References
Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
Lead BoroTellurite
Lead Boro-Tellurite • Pb gives excellent
infrared transmission
(high refractive index)
compared with
conventional glass
• Glasses containing
heavy-metal oxides
has potential
application in radiation
shielding
Introduction
Experimentals
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Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
Abstract
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.
Introduction
Experimentals
Results & Discussion
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Acknowledgement
References
Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
Experimental Methods
• Ternary (TeO2)y
[(PbO)x (B2O3)1-x]1-y glass system
• prepared using a conventional melt-quenching 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%).
Introduction
Experimentals
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Acknowledgement
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Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
Results and Discussion
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) Elastic Properties Using MBS 8000 Ultrasonic Data Acquisition System
Introduction
Experimentals
Results & Discussion
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Acknowledgement
References
Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
Composition and Density
Density is defined as the
mass per unit volume.
• Intrinsic property of
matter, meaning it
remains the same
regardless of sample
size.
• Important property
capable of evaluating the
compactness and casting
the light on the short
range structure of the
glass.
• It is considered a
characteristic property of
a substance and can be
used for material’s
classification
Density
Measurement
(Archimedes
Method)
acaca
as ww
w
Molar
volumes
MV
Volume occupied by one mole of
material
Introduction
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Acknowledgement
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Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
Composition – Density …
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.
PbO (mol%)
Den
sity
(g/
cc)
PbO – B2O3 glass
TeO2- PbO – B2O3 glass
TeO2 – B2O3 glass
Introduction
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Acknowledgement
References
Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
Thermal Properties
Studies of the thermal stability and crystallization behaviour in TeO2 based glasses
Introduction
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Conclusions
Acknowledgement
References
Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
0200400600800
1000120014001600180020002200240026002800300032003400
10 20 30 40 502 theta
Inte
nsi
ty (
a.u
)
XRD Pattern
• 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.
TeO2 powder
Introduction
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Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
Raman Spectra
• 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.
Introduction
Experimentals
Results & Discussion
Conclusions
Acknowledgement
References
Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
Elastic Properties
Elastic Properties • 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.
Introduction
Experimentals
Results & Discussion
Conclusions
Acknowledgement
References
Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
Elastic Properties
Elastic Behaviour of TeO2-B2O3 glass
The increase in ultrasonic velocity reveals that adding of TeO2 in the glass system causes an easy movement for the ultrasonic waves inside the network of the glass structure and hence the ultrasonic velocity increases as TeO2 content increases.
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.
PbO (mol%)
Wav
e V
elo
city
(m/s
)
VL
VS
PbO – B2O3 glass
Elas
tic
Co
nst
ant
(GP
a)
L E K G
Introduction
Experimentals
Results & Discussion
Conclusions
Acknowledgement
References
Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
Conclusions
• Lead Borate, Boro-Tellurite
and Lead-boro tellurite
glasses were successfully
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.
Introduction
Experimentals
Results & Discussion
Conclusions
Acknowledgement
References
Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
Acknowledgement
• The author gratefully acknowledged Ministry
of Science and Innovation (MOSTI), Ministry
of Education (MoE) and University Putra
Malaysia for financial assistance.
Introduction
Experimentals
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Conclusions
Acknowledgement
References
Synthesis and Elastic Studies of Lead Boro-Tellurite Glass System
References