Materials Sciences and Applications, 2011, 2, 289-298
doi:10.4236/msa.2011.25038 Published Online May 2011 (
Copyright © 2011 SciRes. MSA
Thermal Properties of Se100–xZnx Glassy System
Mohd Nasir, Mohd Abdul Majeed Khan, Mushahid Husain, Mohammad Zulfequar*
Department of Physics, Jamia Millia Islamia, New Delhi, India.
Received November 14th, 2010; revised January 17th, 2011; accepted February 23rd, 2011.
The crystallization process in Se100–xZnx glassy system is investigated using differential scanning calorimeters (DSC).
The samples are prepared by conventional melt-quenching technique in the composition range 2 x 20 (at%). Non-
isothermal measurements are carried out for different heating rates .The value of the glass transition temperature Tg
the crystallization temperature Tc and the crystallization peak temperature Tp, are found to be depending upon both
heating rate as well as the composition from thermal analytical data. The investigation of crystallization kinetics indi-
cates a single stage crystallization process. The glass transition energy Eg and the crystallization activation energy Ec
are also evaluated from thermal analytical data. The analyzer has been used the most reliable non-isothermal kinetic
methods. The value of kinetics parameters Eg, E
c and n are calculated using non-isothermal kinetics methods. The
analysis shows that the incorporation of Zinc content has a strong influence on the crystallization mechanism for the
Se100–xZnx glassy system.
Keywords: Chalcogenide Glasses, Amorphous, Crystallization Kinetics, DSC, Non-Isothermal
1. Introduction
The thermal behavior of the amorphous glassy alloys
plays an important role in determining the transport me-
chanism, thermal stability and the practical applica- tions.
For chalcogenide glasses, crystallization studies are of
crucial importance due to some of technical appli- ca-
tions of these materials, namely optical recording me- dia
and memory switching devices. The differential scanning
calorimeter (DSC) technique has so far been played to
study the crystallization process in amorphous alloys and
has proved to be the very effective method for such cha-
racterizing studies [1]. Recently, in thermal analysis stu-
dies several temperature control modes are used and a
diversification is considered as an aspect of the devel-
opment in thermal analysis [2]. The most com- monly
used modes are either isothermal or heating at constant
rate. The drawback of the later is that the analy- sis of
non-isothermal. Experiments are generally more compli-
cated than isothermal one [3,4]. However, in iso- thermal
experiments, it is impossible to reach at a test tempera-
ture instantly [5]. As comparable study, we have applied
selected non-isothermal models reported to be the most
reliable for determination of kinetic parameters of the
crystallization process. Except some reported thermal
studies for the binary Se100–xZnx system [6,7], the
present contributory goal is studying the crystallization
kinetics in Se100–xZnx system using different preparation
method, compositions and non-isothermal analysis me-
thods in detail. The influence of Zink ratio on the crystal-
lization kinetics is reported. Chalcogenide glasses are a
well recognized inorganic group of glassy materials but
some chalcogenide elements like as Se, Te and S in con-
junction, they are very good electropositive elements.
Among the chalcogenide glasses, Se-based glassy alloys
are very interesting and unique class of amorphous semi-
conductors which have large technical applications in
electronics and optoelectronics. From the application point
of view amorphous Se is very most useful material due to
it’s currently in use photoreceptors in TV Videocon pick-
up [8], conventional Xerographic machines and digital
X-ray imaging [4-9]. The pure Se has practical applica-
tion shortcoming like its short lifetimes, low sensitivity
and thermal instability. The use of Se-Te, Se-Ge, Se-Sb,
Se-Ln and Se-Zn is called binary system [5-10] alloys
and is remains of their various properties like greater
hard- ness, higher sensitivity, higher conductivity and
smaller aging effect as compared to pure a-Se.
2. Experiment
The melt-quenching technique is adopted to prepare bulk
Se100–xZnx glasses in the composition range of 2 x 20
Thermal Properties of Se100–xZnx Glassy System
Copyright © 2011 SciRes. MSA
(x = 2, 5, 10, 20). Appropriate amounts of highly pure
elements were sealed in evacuated quartz ampoules un-
der a vacuum of 104 Torr, heated at 850˚C for 10 hours
and then quenched in ice-cold water. Amorphous nature
of these glasses was confirmed using XRD; the result
shows the samples to be amorphous. The glassy alloy
Se100–xZnx is prepared to make fine powder for different-
tial scanning calorimeter (DSC) studies. The DSC tech-
nique is very important due to the fact that it is easy to
carry out, it requires a little sample preparation, it is also
very sensitive and it is relatively free of the sample ge-
ometry. The thermal properties of glassy alloy Se100–xZnx
are studied using a Model-DSC (Rheumatic Scientific
Company, UK) with the temperature correctness of this
equipment being 0.1 K with average error of about 1
K in the measured values of glass transition and crystal-
lization temperature. Non-isothermal runs are carried out
of chosen heating rates, β = 5, 10, 15 and 20 K/min. The
temperature and enthalpy calibrations of the instrument
are performed using the well known melting temperature
and melting enthalpy of high purity indium supplied with
the instrument. The quenched glasses material well grind
powder of Se100–xZnx and is keep into the aluminum pan
~10 mg, before loading the (DSC) calorimeter.
3. Results and Discussion
To evaluate the thermal studies of the glassy Se100–xZnx
system, DSC characteristic measurements have been car-
ried out at different heating rates (
) 5, 10, 15, and 20
K/min. The traces of all composition of glassy Se100–xZnx
system are carried out at different heating rates along
with the results of all samples are as shown in the Figure
1. It is clear that all of the compositions samples show
single endothermic and exothermic peaks are observed
(a) (b)
(c) (d)
Figure 1. DSC Thermo grams for glassy Se100–xZnx (x = 2, 5, 10, 20) alloys at different heating rates 5, 10, 15 and 20 K/min.
Thermal Properties of Se100–xZnx Glassy System
Copyright © 2011 SciRes. MSA
glass transition temperature (Tg), crystallization tempe-
rature (Tc) and their values difference are given in the
Table 1(a).It is noticeable that those glasses have single
endothermic and exothermic peaks, this types of glasses
are most stable than which has two or more multiples’
endothermic and exothermic peaks in their characteristics.
The obtained value of (Tc) at 4% is show maximum cry-
stallized temperature with Zn content, in Figure 2(a). The
value of crystallized peak temperatures (Tp) is given in
the Table 1(b).The exothermic peak temperature (Tp), is
used to identify maximum crystallization rate at 5.8%
with different heating rates as well as in composition is
given in the Figure 2(b). The value of peak crystalliza-
tion temperature Tp, the glass transition temperature (Tg)
is increase linearly with increasing in the heating rates,
and (Tg) is also increases linearly with increase the Zn
content for each sample except for 5% Zn in the glassy
alloy. The onset crystallization temperatures (Tc) are in-
creases linearly at 5% - 20% for each sample in Figure
2(a), respectively and is decrease at 2% Zn content in the
glassy. The exchange in (Tc) may be due to change from
one two dimensional structure (bundles to layers) in the
glassy systems Se-Zn as given in the Figure 2(c). This
type of behavior is typical for glass-crystalline transfor-
mation [11]. It is also shows characteristic temperatures
are shifted to higher temperatures with increase in the
heating rates of the heat flow measurement.
For the determination of crystallization activation en-
ergy (ΔEc) from the data of DSC non-isothermal experi-
ments are use several types of kinetic analysis methods.
However, the two types which are broadly applied iso-
conversion methods and the peak methods. In an inves-
tigation study of the accuracy of known iso-conversion
methods, Starink [1] reported that the most accurate me-
thods are Kissinger-Akahira-Sunose (KAS) [9-12] me-
thod and the method developed by Author [1-13]. All of
the iso-conversion methods require the determination of
the onset temperature Tc at which a fixed fraction value α
(where α = A'/A, It means that A'-Partial Area and A is the
total Area in the exothermic peak) of the total amount is
transformed. In the KAS method, the relation between
the temperatures and the heating rate β is given by
ln constant
 (1)
where R is gas constant and ΔEc is the crystallization
effective activation energy. Plotting of in
1/Tc enables calculation of ΔEc from the linear fits to
experimental data. The results for α = 0.4, 0.5, 0.9 and
1.0 are shown in Figure 3. The most reliable iso-conver-
sion methods are as reported by Ozawa [13], Flynn-Wall-
Ozawa (FWO) [14,15], KAS and the Friedman-Ozawa
[15,16]. The FWO model has been developed for non-
Figure 2. (a) Composition dependence of crystallization
temperature Tc for glassy Se100–xZnx alloys. (b) Composition
dependence of crystallized peak temperatures Tp for glassy
Se100–xZnx alloys. (c) Plots of 103/T vs. ln (103/2
T), 103/T vs.
ln (103/Tc) and 103/T vs. ln (
)for glassy Se100–xZnx alloys.
Thermal Properties of Se100–xZnx Glassy System
Copyright © 2011 SciRes. MSA
Table 1. (a) The value of glass transition, onset temperature and their differences for glassy Se100–xZnx alloys; (b) The value of
peak crystallization temperature Tp at different heating rates for glassy Se100–xZnx alloys.
Rate (β) K/min
Se98Zn2 Se95Zn5 Se90Zn10 Se80Zn20
Tg (K) T
c (K) Tc Tg (K) T
g (K)Tc (K)Tc Tg (K)Tg (K)Tc (K)Tc Tg (K) Tg (K) Tc (K)Tc Tg (K)
5 357.09 497.78 140.69 368.15 496.01127.86 345.02495.35150.33 353.95 494.16 140.21
10 360.09 499.13 139.04 347.96497.56149.60 349.59500.47 150.88 356.33 501.21 144.88
15 361.71 495.73 134.02 354.64 494.68140.04 350.08496.82 146.74 359.28 497.8 138.52
20 366.55 495.72129.17 353.89494.9141.01 353.06496.28143.22 359.21 496.85 137.64
Heating Rate (β) K/min
Se98Zn2 Se95Zn5 Se90Zn10 Se80Zn20
Tp (K) Tp (K) Tp (K) Tp (K)
5 502.69 501.10 499.12 498.82
10 504.28 503.28 504.62 502.64
15 500.56 499.73 501.41 500.07
20 500.10 501.48 502.28 501.87
isothermal analysis of crystallization in which the final
relation is as follows
ln 1.0518const
 (2)
By plotting (lnβ) vs. 1/Tc, for chosen value of fraction
transformed α, the effective activation energy ΔEc have
been determined, from the Figures 4, 5 and 6 with the
fixed value of (α = 0.4, 0.5, 0.9, 1.0) is given in the Ta-
ble 2.
3.1. Composition Dependence of Crystallization
and Peak Temperature in Exothermic Peak
Figure 2(a) indicates the composition dependence of peak
crystallization temperature Tc of glassy alloy Se100–xZnx
for four different heating rates. The crystallization kine-
tics of Se100–xZnx alloy is characterized by solving the
exothermic peak, where Tc is onset temperature and Tp is
the peak temperature of the exothermic peak. At lower
concentration of Zn the system Gaines the unit dissolved
in a matrix composed of Se chains with increase of Zn
content. The Se-Se bond energy (205.8 kJ/mol) will be
replaced by Se-Zn bond energy which has higher bond
energy (450.5 kJ/mol) [9], since cohesive energy of the
system doesn’t decrease with increases in the Zn content.
This type of composition is to be considered as a series
composition of the system behaving as a chemically or-
dered alloy by taking the high energy Se100–xZnx on he-
tropolar bonds of the system. A comparable turn- around
has been found by Tonchev and Kasap [17] in glassy
alloy Se100–xZnx. Under these circumstances the Tc would
get converted from one to two dimensional structures
(bundles to layers) in the Se-Zn system 5 at% Zn [15].
Further more addition of Zn favors’ the formation of
(Zn-Zn) bonds, means reducing the bond concentration.
This is in turn the results with the decrease of bond
energy of (Zn-Zn) – (Se-Zn) = 245.5 kJ/mol. Hence, the
cohesive energy decreases with increase of Tc which is
shown in Figure 2(c).
3.2. Evaluation of Activation Energy of
Crystallization (ΔEc)
The activation energy of crystallization for the glassy
alloy Se100–xZnx are evaluated by using the method Sta-
rink [1] Kissinger-Akahira-Sunose (KAS) [9-12] Flynn-
Wall-Ozawa (FWO) [14,15], KAS and the Flynn-Wall-
Ozawa [15,16], Kissinger’s relation, Augis-Bennett’s Ap-
proximation, and Approximation method of Mahadevan
et al. The different kinds of non-isothermal plots for
glassy Se100–xZnx alloy in (Figures 3, 4 and 5) are calcu-
lated for the present sample by utilizing the five methods
as given in the Table 2, with the help of Equation (3).
ln ln
 (3)
The value of activation energy ΔEc according to Kissin-
ger-Akahira-Sunose (KAS) and Flynn-Wall-Ozawa (FWO)
varies linearly with systematically and the value very
close to each other remaining three i.e. Kissinger’s rela-
tion, Augis-Bennett’s and Approximation method of Ma-
Thermal Properties of Se100–xZnx Glassy System
Copyright © 2011 SciRes. MSA
Figure 3. Plots of (103/2
T) vs. ln (β/2
T) 103/Tc vs. ln (β/Tc)
and 103/Tc vs. (β) for glassy Se100–xZnx alloys.
hadevan et al. show much variation in their activation
energy for different composition in the glassy Se100–xZnx
alloy. Kissinger’s relation, Augis-Bennett’s and Appro-
ximation method of Mahadevan et al. method can be
applied in the present analysis as recommended by the
Kasap and Juhasz [18]. Comparative values of activation
energy ΔEc is given in the Table 2, these values are in
well agreement with one another, in the first three cases
with each other in the giving two.
3.3. Evaluation of Avrami Index ‘n’
To calculate the order parameter ‘n’ and the activation
energy ΔEc has great helped to evaluate Avrami index ‘n’
by using the methods Matusita-Ozawa and Vazquez.
lnln 1lnln
 
 (4)
Figure 6 shows the volume fraction increases with
increases the temperature and variation of ln(
) with ln
[ln (1 α)1] varied in system for glassy Se100–xZnx al-
loy at different temperatures with different heating rates
[19,20]. The value of Avrami index ‘n’ have been evalu-
ated from the slopes of these curves at four fixed differ-
ent temperatures given in the Table 3. According to them,
Avrami index ‘n’ basically depends on volume fraction
in the exothermic peaks. It is linearly increases with con-
centration of Zn and temperature for individual composi-
tion of the sample as shown in the Table 3. This is an
indicate property of the order parameter and for the fluid
in the glass transition region, the relaxation times for the
molecular movements change into experimental scale. At
these circumstances the diffusive movements convert
comparable to the experimental timescale. However dif-
fusive motion of the liquid has been trapped and the sys-
tem is not in the thermal equilibrium [18-21]. At this
time, the size of the nuclei does not achieve the critical
size required to initiate the nucleation process as the
glass is supposed to have no nuclei (of critical size).
When the glass is heated in the furnace, the rate of crys-
tal nucleation in the glass reaches the highest value at a
temperature than the glass transition temperature and
then decrease suddenly with increasing the temperature,
during this period the rate of crystal growth is much at a
temperature higher than the temperature upon which the
nucleation rate is highest. If the glass is heated at a con-
stant rate, the crystal nuclei is formed only at very few
temperatures and crystals rise-up in size at higher tem-
peratures without any increase in number. From the Ta-
ble 3, it is show that ‘n’ decreases with an increase in the
temperature. It is very familiar that the crystallization of
chalcogenide glasses is connected with nucleation and
the growth process and the amount of crystallization α
increases with increase in temperature, it approaches to
with its standard value 1. Hence, increasing the tempera-
Thermal Properties of Se100–xZnx Glassy System
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Figure 4. Plots of (103/T) vs. ln (β/T) at fix value of crystallized fraction α for glassy Se100–xZnx alloys.
Table 2. The values of activation energy of crystallization (Ec) and the activation energy structural relation Eg of glassy
Se100- x Znx alloy evaluated by using non-isothermal methods.
Non-isothermal method
Activation Energy of crystallization Ec (kJ/mol)
Se98Zn2 Se95Zn5 Se90Zn10 Se80Zn20
Kissinger’s relation 205.61 409.46 540.91 1052.39
Augis-Bennett’s app. 286.83 307.53 321.17 1044.82
Approximation method of
Mahadevan et al. 369.47 263.55 386.19 744.10
FWO 451.48 150.02 315.88 795.76
KAS 483.22 149.43 340.60 828.66
Non- isothermal method The activation Energy of structural relation Eg (kJ/mol)
Kissinger’s relation 152.39 281.59 155.39 333.47
Approximation method of
Mahadevan et al. 156.55 206.10 160.38 238.19
FWO 95.34 101.70 92.22 101.26
KAS 94.09 100.78 90.76 100.22
Thermal Properties of Se100–xZnx Glassy System
Copyright © 2011 SciRes. MSA
Figure 5. Plots of (103/Tc) vs. ln (β/2
T) for glassy Se100–xZnx alloys.
Table 3. Temperature dependence of Avrami index (n).
Se98Zn2 Se95Zn5 Se90Zn10 Se80Zn20
Temp (K) ‘n’ Temp(K) ‘n’ Temp (K) ‘n’ Temp (K) ‘n’
476.0 1.04 478.0 1.43 480.0 1.00 494.0 1.23
476.5 1.08 478.5 1.44 480.5 1.14 494.5 1.30
477.0 1.14 479.0 1.48 481.0 1.24 495.0 1.65
477.5 1.16 479.5 1.58 481.5 1.33 495.5 1.75
ture with increase in the order of the glassy Se100–xZnx
alloys suggests that the character of characterization
converts from a nucleation-driven system at the begin-
ning to a growth-driven system by the crystallization
process [13-21].
3.4. Rate of Crystallization Glassy Se100–xZnx
After knowing the calculated parameters as ΔEc is used
to Equations (1), (3), and K0 with the help of Equation
(3), and the value of rate constant K are evaluated from
the Equation (4). Finally, the frequency factor K0 is ob-
tained by using this relation and with the help of JMA
model of authors [7].
0exp c
KERT (5)
Therefore, the values of lnK at different temperatures in
the crystallization region are given in the Table 4, for
Thermal Properties of Se100–xZnx Glassy System
Copyright © 2011 SciRes. MSA
Figure 6. Plots of ln (β) vs. ln [ln (1 αT] for four constant
temperature for glassy Se100–xZnx alloys.
Table 4. Temperature dependence of rate constant K in the
crystallization region.
475 4.71 4.79 4.86 5.12
480 3.96 4.09 4.17 4.41
485 3.59 3.71 3.75 4.01
490 3.31 3.41 3.47 3.72
glassy Se100–xZnx alloys, It shows that K increases with
increase in temperature in the Figure 7(a). It is clear that
the crystallization rate is highest for glassy Se80Zn20 alloy.
To know more information about morphology of growth,
the given Equation (5) from the Gao-Wang model [22]
leads to the Equation (5) is
where KP being the value of the rate constant K at peak
crystallization temperature Tc for the constant heating
rate. Therefore, the heating rate dependence of KP is
given in the following Table 4. The value of KP is in-
creases with increasing in the x at% and with increasing
the heating rates in Table 5. It is clear that the crystalli-
zation rate constant is highest for glassy Se80Zn20 alloy as
given in the Figure 7(b). The value of K0 increases with
increases the x at% and with increase in the heating rates.
It is clear that the frequency factor K0 is highest for glas-
sy Se80Zn20 alloy as given in the Figure 7(c). Figure 8(a)
shows the rigidity of glass sample [22]. Figure 8(b)
Figure 7. Plots of Temperature T(K) vs. Rate constant (lnK),
) K/min vs. rate constant Kp min1 and Temperature (T)
K vs. K0 for glassy Se100–xZnx alloys as shown in the above
Thermal Properties of Se100–xZnx Glassy System
Copyright © 2011 SciRes. MSA
Table 5. Heating rate dependence of rate constant KP.
Heating rate(β)K/min Kp (min1) Se98Zn2 Kp (min1) Se95Zn5 Kp (min1) Se90Zn10 Kp (min1) Se80Zn20
5 4.95 × 104 10.05 × 104 13.28 × 104 25.83 × 104
10 9.93 × 104 20.02 × 104 26.02 × 104 51.87 × 104
15 15.08 × 104 29.43 × 104 39.66 × 104 77.81 × 104
20 20.18 × 104 39.88 × 104 52.47 × 104 102.90 × 104
(a) (b)
Figure. 8. Plots of Zn content vs. glass transition temperature, (Tg) crystallization Temperature Tc and Tc Tg (K) vs. ln K, for
glassy Se100–x Znx glasses at different heating rates 5, 10, 15, and 20 as Mention in the above Figure (a) and (b).
the glass alteration temperatures Tg represents the power
or strictness of the glass structure in chalcogenide glasses.
Since thermal stability depends on the Tg value in the
glassy state [20-23]. From the Figure 8(b) Tg individual
doesn’t give the information about the thermal stability
[24] but the difference value Tc Tg, is give in the thermal
stability for all composition with different heating rates
[25]. The maximum value of Tc Tg is giving the informa-
tion of highest thermal stability for the sample Se90Zn10
at 10 K/min as shown in the Table 1. It is very important
to know the composition Se90Zn10 is more stable than
other composition of the alloy Se100xZnx. It is obvious
from the Figure 8(a) and Table 1 in first the crystalliza-
tion temperature increases with increase in the Zn con-
tent up-to 10% and then decreases up-to 20 at% of Zn
content in the Se100–xZnx system. Therefore, it is said that
the rate of crystallization is highest at 10% of Zn content
in the glassy system [26].
4. Conclusions
The kinetics parameter of crystallization has been inves-
tigated under the non-isothermal methods in glassy
Se100–xZnx (2 x 20). The DSC thermograms are used
to evaluate the data of kinetic parameters. There are three
best fit methods Kissinger’s relation, Augis-Bennett’s
app and Approximation method of Mahadevan et al., the
activation energy (ΔEc) is increases as increased the Zn
concentration in the glassy. According to Flynn-Wall-
Ozawa (FWO), Kissinger-Akahira-Sunose (KAS), the
activation energy ΔEc also increases linearly on (5 - 20)
at% Zn concentration systematically in the glassy. The
activation energy of structural relation ΔEg is increase
non-linearly with increases in the composition of the
alloy. Avrami index ‘n’ is increases linearly with in-
creasing the temperature and non-linearly with Zn con-
centration in the glassy Se100–xZnx. The rate constant K
increases with the temperature increases in the composi-
tion of the glassy. The rate of crystallization is highest in
the glassy Se98Zn2 alloy. The thermal stability on the ba-
sis of experimental data is highest for the glassy Se90Zn10.
The rate of crystallization constant is high because of the
highest difference of Tc Tg in Se90Zn10; furthermore it
indicates that thermally is most stable this glass in the
range of composition. It has been seen that the crystalli-
zation is to deliberate for the chalcogenide glasses by
taking the maximum thermal stability. Finally the fre-
quency factor K0 is also increases with increase the tem-
perature in the glassy Se100–x Znx.
5. Acknowledgements
Thanks are due to Department of Physics (Materials
Sciences Lab-2) of JMI, New Delhi (India) for providing
financial assistance in the form of major research pro-
Thermal Properties of Se100–xZnx Glassy System
Copyright © 2011 SciRes. MSA
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