Kinetics of glassy

system using differential scanning

calorimeter

Presented by Debasis Saran
x x
Cd S
25 75
Se
Objective
To study the kinetics of selenium based chalcogenide glassy
system by non iso -thermal DSC measurements.
To find out how Tg and Tc depends on different heating rates
and on concentration of different alloying elements.
To find out the stable glassy system among the different
variables that are being studied.
To find out the crystallization enthalpy for different glassy
system.
To find out the activation energy of the glassy system by using
different theories like Ozawa and Kissinger and comparing the
two results.


INTRODUCTION
Chalcogenide glass is a glass containing one or
more chalcogenide elements(not counting oxygen).
These are three elements in Group 16 in the periodic
table: sulfur, selenium and tellurium.
They have wide commercial applications in switching , optical
memory devices , xerography etc.
Why S and Cd added?
Se has short lifetime and low sensitivity .To overcome these
difficulties certain additives are used for getting various
properties like greater hardness, higher sensitivity, higher
crystallization temperature, higher conductivity and smaller
ageing effects as compared to pure amorphous Se . Here we
have chosen S and Cd as an additive to overcome these
problems..
Sample Preparation
Bulk glasses of Se75S25xCdx (x = 0, 2, 4, 6 and 8) system
were prepared by the conventional melt-quenching
technique.
High purity materials (99.999% pure) Se, S and Cd in
appropriate atomic percentage proportions were weighted
and sealed in an evacuated (103 Pa) quartz ampoules.
The sealed quartz ampoules were kept inside a furnace,
where the temperature was raised to 1123K and it was
maintained for 14 h with frequent rocking to ensure the
homogenization of the melt.
The ampoules were subsequently quenched in ice water. The
ingots of the sample were taken out by breaking the quartz
ampoules. These ingots were then ground into a fine powder.
Equipments used
A Philips Model PW 1710 X-ray diffractometer was
employed for studying the structure of the material.
The crystallization studies were done by using
differential scanning calorimeter (Model-DSC plus,
Rheometric Scientific Company, U.K.).
The temperature precision of this equipment is 0.1K
with an average standard error of about 1K in the
measured values (glass transition and crystallization
temperatures)
Results
DSC plot at a heating rate of 10K/min
Variation of Tg with Cd content
Variation of Tc with Cd content
Calculation of Activation energy by
Ozawas method
Calculation of Crystallization enthalpy
Conclusion
The temperature difference (Tc Tg) is lowest for the
composition of 4% of Cd. Hence the glass with 4% of
Cd is least stable and the enthalpy released is found
to be maximum for 4% of Cd which further indicates
the minimum stability of the glass.
The activation energy of crystallization increases with
increasing Cd content in the present system in both
the methods, indicating that the rate of
crystallization is faster as the Cd content increases