Study of Activation Energy of Crystallization and Growth
Morphology of Ge
25x
Se
75
Sb
x
(x ¼ 12, 15, 18)
Chalcogenide Glasses
Naveen Tanwar and Vibhav K. Saraswat*
In the present paper crystallization kinetics of Ge
25-x
Se
75
Sb
x
(x ¼ 12, 15, 18)
chalcogenide glasses has been investigated using thermal analysis (TA)
technique. Ge
25-x
Se
75
Sb
x
(x ¼ 12, 15, 18) chalcogenide glasses have been
prepared by rapid quenching of melt technique. For structure characterization
XRD technique has been used. Out of various TA techniques Differential
Scanning Calorimetery (DSC) has been used for present study. DSC scans
have been carried at different heating rates i.e. 5, 10, 15 and 20 K/min. For
evaluation of activation energy of crystallization various theoretical models
Kissinger, Ozawa, Augis-Bennet and Matusita-Sakka have been used. Activa-
tion energy of crystallization increases with increase of Sb content in Ge
25-
x
Se
75
Sb
x
(x ¼ 12, 15, 18) glassy series. The value of Avrami index indicates
bulk crystallization with one or two dimensional growth.
1. Introduction
Chalcogenide glasses in recent years have been under
investigation of researchers because of wide range of application
in field of electronics and optics.
[1–4]
Amorphous Se because of
its high glass forming ability acts as good host matrix for
preparation of chalcogenide glasses. Doping of Ge further
increases the glass forming region and also increase the strength
and rigidity of structure. Antimony acts as good doping agent to
modify the properties of Ge-Se chalcogenide glasses for specific
technological application. Doping of Sb in Ge-Se glassy matrix
reduces optical losses considerably making these materials
suitable for fabrication of IR-optical fibers.
[5–8]
For production of
high quality glass for Infrared optical application crystallization
should be avoided. The study of crystallization kinetics gives
information about activation energy of crystallization and
growth morphology that helps to provide information about
resistance to crystallization. Understanding of crystallization
kinetics is essential to find the utility of a material for a specific
application. For the study of crystallization kinetics Differential
Scanning Calorimetery has been widely
used.
[9–12]
Activation energy of crystalliza-
tion has been evaluated using Kissinger,
Ozawa, Augis-Bennet and Matusita
Sakka models. Matusita-Sakka model pro-
vides information about Avrami Index and
dimensionality of growth.
2. Material Preparation and
Experiment Procedure
Preparation of Ge
25-x
Se
75
Sb
x
(x ¼ 12, 15, 18)
glassy samples have been carried out using
rapid quenching of melt technique. High
purity (99.999 %) constituent materials Ge, Se
and Sb has been taken in elemental powder
form in proper atomic weight percentage and
sealed in quartz ampoules under vacuum of
10
5
torr. The sealed ampoules have been kept inside a programmable
furnace whose temperature was raised initially at rate of 3-4
C/min
and was kept at this value for 2 hrs then maintained at 950
C for
17 hrs. Quenching has been done in ice- cooled water to get glassy
state. Amorphous nature of so produced glassy samples has been
confirmed by X-ray diffraction.
Differential scanning calorimetery (DSC) Netschz 204 F1
Phoenix has been used for thermal studies under non-
isothermal condition. DSC scans have been carried at four
different heating rates 5, 10, 15, 20 K/min on accurately weighted
samples sealed in aluminum pans. These scans were recorded
from room temperature to 550
C.
3. Result and Discussion
Figure 1(a–c) represents DSC thermograms of Ge
25x
Se
75
Sb
x
(x ¼ 12, 15, 18) glasses.
When glassy samples are subjected to DSC under constant
heating rate they undergo phase transition, an endothermic peak
is obtained corresponding to glass transition and exothermic
peak corresponding to crystallization.
4. Kinetics of Crystallization
The kinetic of crystallization has been studied under non-
isothermal condition. Samples under test have been heated from
room temperature to an elevated temperature at constant
heating rate and the heat evolved is recorded as a function of
N. Tanwar
Department of Physics, Ahir College
Rewari-123401, India
V. K. Saraswat
Department of Physics, Army Cadet College Wing, IMA
Dehradun-248007, India
E-mail: vibhav.spsl@gmail.com
DOI: 10.1002/masy.201600185
Macromolecular Symposia
Chalcogenide Glass www.ms-journal.de
ARTICLE
Macromol. Symp. 2017, 376, 1600185 © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim 1600185 (1 of 8)