J Mater Sci: Mater Electron (2022) 33:15107–15115

High-field conduction in fresh and aged samples of Se

and As2Se3 glasses
Shiv Kumar Pal1, Neeraj Mehta1,* , A. A. Horvat2, and V. I. Mikla2

1
Physics Department, Institute of Science, Banaras Hindu University, Varanasi 221005, India
2
Humanitarian and Natural Science Department, Uzhgorod National University, Uzhgorod 88000, Ukraine

Received: 4 May 2022 ABSTRACT

Accepted: 15 May 2022 This work provides the consequence of aging on the conduction mechanism of
Published online: fresh as well as aged Se and As2Se3 chalcogenide glasses (ChGs). In this analysis,
9 June 2022 the sample synthesized by the melt-quench route was used as identical disk-
shaped pellets for current–voltage (I–V) characteristics at different tempera-
Ó The Author(s), under tures. Our observation shows the absence of space charge limited conduction
exclusive licence to Springer (SCLC) for both fresh as well as aged samples of Se and As2Se3. The Poole–
Science+Business Media, LLC, Frenkel conduction mechanism is detected as the leading model for fresh and
part of Springer Nature 2022 aged samples of both Se and As2Se3 glasses. The activation energy is found to
rise appreciably due to the aging effect of Se while almost constant for As2Se3
samples. The reason behind this may be the slight growth of crystallite due to
aging in Se glass.

1 Introduction capacities on thermal history [2]. The study of struc-

The attention of research groups and scientists has
been attracted to understanding the phenomenon of
electrical conduction mechanism in amorphous
chalcogenide semiconducting material because the
nature of bonding, network connectivity, and rigidity
in these materials play a significant part in the con-
duction mechanism. Due to the low conductivity of
these materials, high-field effects are observed read-
ily [1]. Eastal et al. studied the heat capacity and
structural relaxation of enthalpy in As2Se3 glass and
found that the glass heat capacities are almost inde-
pendent of the rate of cooling. Thus, As2Se3 shows
different behavior from formerly considered ChGs
that demonstrate the dependence of their heat
tural properties and structural relaxation of different
As-containing materials including As2Se3 have been
investigated using several techniques by different
research groups [3–7]. Lovu et al. studied the Raman
analysis of Se–As alloys and reported that on adding
arsenic in pure Se glass, the chain of –Se-Se-Se- is
broken; however, the closed Se8 rings contribute as
the major parts of the network assembly. When
arsenic is further incorporated, the formation of new
As–Se structural units (e.g., AsSe3 pyramids, As4Se3,
and As4Se4 cages) is observed [8].
Pfister and Taylor demonstrated the important
defect states in glassy As2Se3 through their experi-
ments. As2Se3 glass is a good glass-former and pos-
sesses a saturated-bond covalent network, that’s why

Address correspondence to E-mail: dr_neeraj_mehta@yahoo.co.in

https://doi.org/10.1007/s10854-022-08430-3
15108
its glass structure is not far detached from that of the
crystal and is well-thought-out to be a single-phase
compound [9, 10]. The atomistic comparison between
stoichiometric and nonstoichiometric glasses has
been done for the case of As2Se3 and As4Se4 by Jun Li
[11]. Since the theory of Phillips and Thorpe [12, 13]
says that the system which possesses an average
coordination number of * 2.4 has a floppy to rigid
transition threshold, such a feature was found for the
Arsenic tri-selenide (As2Se3) system which makes it
an interesting material for study. The photoinduced
peculiarities in As2Se3 and As4Se4 were studied and
photoinduced fluidity was investigated by Hisakuni
and Tanaka in As2Se3 glass [14]. The hologram
recording in amorphous As2Se3 thin films was
examined experimentally by Chomat et al. [15] and
they reported that in addition to the recording of a
hologram at a comparatively low exposure of some
J/cm2, the recording of another hologram can also be
achieved at exposures of 104–105 J/cm2.
The study of electrical conduction mechanism in
As2Se3 glass as a function of temperature, thickness,
and strength of applied field has been done by Wit
et al. [16] and he reported that below 70 °C, the
conduction is electronic, and breakdown in this glass
is dielectric, not thermal. The fields concerning the
diverse regions of the conductivity are independent
of the Se-to-As ratio [16]. The electrical effects
induced by implantation of highly energetic ions in
bulk amorphous As2Se3 have been studied by Singh
et al. and they observed that the leading role is
played by the creation of the defect states close to
near the Fermi level in the variable range hopping
conduction under the influence of ion irradiation.
They also reported that the bi-polaron hopping con-
duction is not much affected by ion irradiation and a
very small dose (* 1013 ions/cm2) is sufficient to
alter the electrical transport mechanism [17, 18].
Photoconductivity of amorphous As2Se3 glass and
the dynamics of the blocking-to-injecting contact
transition have been investigated by Tutihasi [19].
The investigations of different physical properties of
As2Se3 and As2Te3 glasses have been demonstrated
by Thornburg [20]. The non-linear properties and
fibers of chalcogenide glassy series As2S(3-x)Sex where
x = 0 to 3 have been studied by Sanghera et al. [21].
The investigation of microhardness measurement of
different Arsenic containing mono-component and
multi-component chalcogenide glasses has been
demonstrated by Kotkata [22]. Kastner et al.
J Mater Sci: Mater Electron (2022) 33:15107–15115
estimated the thermally created defects in the sample
of As2Se3 in the liquid phase as well as the glassy
phase [23]. The theoretical studies have been done by
Vanderbilt et al. to understand the defect states in
As2Se3 glass [24]. In their observation, this group
examined that the defect states are very dissimilar
from those in Se and a deep gap state arises in As2Se3
due to inimitable bond orbitals, while it occurs in Se
because of unique p interactions among orbitals [24].
The measurement of refractive-index variation in
As2Se3 was done by Antonyuk et al. [25] using an
optical grating method. For the excitation, they used
an argon laser source.
Thus, a lot of data are described in the literature
associated with different investigated properties of
both Se and As2Se3 samples but very few observa-
tions have been done to see the aging effects on the
electrical properties of Se and As2Se3 samples.
Keeping this fact in mind, in this paper, we have
reported the aging effects on the electrical properties
of both Se and As2Se3 samples in bulk form.
2 Theoretical basis
The investigations of Poole–Frenkel and Schottky’s
mechanism for various materials are described in the
literature by several research groups [26–35]. In 1938,
Frenkel proposed that the free carrier density
enhanced by applied field is associated with a field
reduction of a Coulombic potential barrier and he
modified Poole’s law by substituting E1/2 in place of
E [26]. There are two types of Poole–Frenkel (PF)
effects are given, the first one was ‘classical’ which
associated with Boltzmann’s approximation and
another is the ‘modern PF effect’ which was associ-
ated with the Fermi–Dirac function rather than
Boltzmann’s approximation. The charge carriers are
thermally released from Coulombic attractive traps,
which increase by the electric field in most of the
semiconducting materials, is recognized as the clas-
sical Poole–Frenkel effect. This effect is the most
common conducting mechanism in the case of
amorphous semiconducting materials and insulators
following the condition such that the electron path
between two electrons is less in comparison to the
interelectrode distance [27–30]. One can see from
Fig. 1 that when be1/2 increases toward the value of
qu, the barrier reduces to zero value i.e., all traps will
become vacant if be1/2 becomes equal to qu and this
J Mater Sci: Mater Electron (2022) 33:15107–15115 15109

case is known as PF saturation [31]. Thus, the 3 Experimental details

reduction of Coulombic potential barrier under the
application of an external electric field is mentioned The melt-quench technique was employed for the
as either the Poole–Frenkel effect or the Schottky preparation of Se and As2Se3 glasses in bulk form.
effect, in which, the Schottky effect is concerned with High purity (99.999%) materials were weighed in
the barrier at the surface region of metal and semi- proportion to their atomic percentages and were
conducting materials while the Poole–Frenkel effect sealed in quartz ampoules of identical geometry. The
is related to barriers in the extensive region of details of the melt-quench technique are available in
materials [28, 32]. Similar conduction mechanisms the literature [41, 42]. The aged specimens having age
were observed in oxide glasses [36, 37]. of Ten years both glasses were chosen to study the
The several types of materials display signs of PF aging effect concerning their fresh counterparts.
effect or SC effect at the high electric field that is Before studying the high-field conduction through
reflected in the current–voltage characteristics as current–voltage measurements, the bulk samples of
follows [33–40]: the as-prepared glasses were attained in the form of
! disk-shaped geometry by employing a usual
bV 1=2
I ¼ I 0 exp ð1Þ hydraulic press at a base pressure of 4 to 5 Tons. A
KB T
specifically designed sample holder was used for the
execution of the current–voltage measurements. The
Here b is an experimental constant. We can express
pellets were positioned in a specially designed
b as
metallic sample holder for current–voltage measure-
2 sffiffiffiffiffiffiffiffiffiffi 3
e3 ments using a source meter unit (Keithley Electronics,
sffiffiffiffiffiffiffiffiffiffi 6 ¼ bPF ðForf ¼ 1Þ 7
1 e3 6 per e0 7 model: 2410) under a sufficient vacuum created by a
b¼ ¼ 6 s ffiffiffiffiffiffiffiffiffiffi 7 ð2Þ rotary vacuum pump (Hindhivac, model: ED-6). The
f per e0 6 41 e3
7
5
¼ bSC ðForf ¼ 2Þ temperature of the pellets was controlled by mount-
2 per e0 ing a heater inside the sample holder and measured
by a calibrated copper-constantan thermocouple
Here, bPF and bSC are called Poole–Frenkel and
mounted very close to them.
Schottky coefficients for f = 1 and f = 2, respectively.
The PF theory was unable to identify the particu-
lars of the profile of the potential, the special range of 4 Results and discussion
potential, and the diffusion mechanism of charge
carriers at a microscopic scale [28]. The SEM images of fresh as well as the aged sample
of Se and As2Se3 glass are depicted in Fig. 2. This
surface morphological picture shows the absence of
any periodic arrangement of atoms, i.e., the amorphic
nature of materials. The amorphic nature of Se and

Fig. 1 Profile of Coulombic

potential in the presence of an
electric field (PF effect)

Reduction in height
βε1/2 with fields
15110
As2Se3 samples are checked by the XRD pattern
which is reported in our earlier papers [41, 42]. The
Raman characterization and TEM image of this
investigated sample are also reported in these papers
[41, 42].
The variation of current against voltage at 323 K for
applied voltage 500 V is depicted in Fig. 3, which
shows the absence of switching behavior in both
fresh as well as aged samples of Se and As2Se3. This
may happen because we have used bulk samples in
the present studies, while resistive switching is gen-
erally observed in thin-film samples [43]. One can
observe from Fig. 3 that there is an appreciable
increment in current are found in aged g-Se relative
to that in the fresh g-Se sample while such changes
are absent in As2Se3 samples. In the next step, we
have tried to find the mechanism behind the high-
field conduction that takes place in these samples. For
this, we have plotted the graphs between ln I versus
V1/2 and ln (I/V) versus V. Figure 4 shows such plots
for Se fresh/aged samples and cleared that these
graphs are almost linear with a good correlation
coefficient. It is reported in the literature that the
SCLC mechanism exhibited if the ln(I/V) versus
V graph is linear with a good correction coefficient
and the slope of this, decreases with increasing tem-
perature, [39, 44–46] but for present Se fresh/aged
Fig. 2 SEM images of fresh and an aged sample of Se glass in (a, b) and (c, d) at resolutions of 10 lm and 5 lm, respectively. Also, SEM
images of fresh and an aged sample of As2Se3 glass in (e, f) and (g, h) at resolutions 50 lm and 10 lm, respectively
J Mater Sci: Mater Electron (2022) 33:15107–15115
sample, graphs are approximately linear but slopes
are not decreasing smoothly with temperature which
specifies that the SCLC mechanism does not take
place in Se case.
Similarly, Fig. 5 represents the plots between ln
I versus V1/2 and ln(I/V) versus V for As2Se3 fresh/
aged samples. The non-linear nature of ln(I/V) ver-
sus V curve reveals the absence of SCLC mechanism
in As2Se3 fresh/aged samples also. The plot ln I ver-
sus V1/2, which is linear, is an indication of holding
both Poole–Frenkel and Schottky mechanisms, but
the extrapolated part should be pass through a solo
point at zero value of the applied voltage of ln I ver-
sus V1/2 curve for Schottky mechanism while it does
not happen for the Poole–Frenkel mechanism [47].
Now, one can distinguish the Poole–Frenkel and
Schottky mechanism by inserting a graph between
ln(I/T2) against (1/T) as revealed in Fig. 6 for both Se
as well as As2Se3 fresh/aged samples, which should
be linear for Schottky mechanism but not for the case
of Poole–Frenkel mechanism [46]. In Fig. 6, the lines
seem to be linear but actually, it is non-linear, i.e.,
having a poor correction coefficient for Se fresh/aged
sample while it is linear for As2Se3 fresh/aged sam-
ples with a good correlation coefficient. Thus, we
conclude that the PF mechanism is dominated over
J Mater Sci: Mater Electron (2022) 33:15107–15115 15111

525 540
500 V, 323 K 500 V, 323 K
480
425 420
(a) 360 (b)
325
V (Volts)

300

V (Volts)
240
225
180

120
125 As2Se3 Fresh
Se Fresh 60
Se Aged As2Se3 Aged
25 0
0 9 18 27 36 45 54 0.0 0.1 0.2 0.3 0.4 0.5 0.6
I ( A) I ( A)

Fig. 3 I–V characteristics of (a) fresh/aged Se and (b) fresh/aged As2Se3 samples

-12.5 -18.9
Se Fresh, 500V Se Fresh, 500V

-13.0
-19.1

-13.5
ln(I/V) (mho)
lnI (A)

-19.3
-14.0
303 K
308 K 303 K
-19.5 308 K
-14.5 313 K
318 K 313 K
323 K 318 K
323 K
-15.0 -19.7
12 13 14 15 16 17 18 19 20 21 22 150 225 300 375 450 525
1/2
V (Volts) V (Volts)
-9.9 -16.1
Se Aged, 500V Se Aged, 500V
-10.2
-16.3
-10.5
-16.5
-10.8
ln(I/V)(mho)
lnI (A)

-11.1 -16.7

-11.4
303 K -16.9
303 K
-11.7 308 K
313 K
308 K
318 K -17.1 313 K
-12.0
323 K 318 K
323 K
-12.3 -17.3
12 13 14 15 16 17 18 19 20 21 22 90 150 210 270 330 390 450 510
1/2
V (Volts) V (Volts)

Fig. 4 Variation of ln I versus V1/2 and ln (I/V) versus V for both Se fresh/aged samples

the SC mechanism for Se fresh/aged while the The activation energy can be calculated by the
reverse is true for As2Se3 fresh/aged samples. thermally activated current relation [48], given as:
Another parameter, that is also mentioned in the  
DE
literature to differentiate between these two mecha- I ¼ I 0 exp  ð3Þ
kT
nisms, is the activation energy. The activation energy
should be equal to or greater than 0.98 eV i.e., (E Here DE is the activation energy, k is the Boltzmann
C 0.98 eV) for the Schottky mechanism but less than constant and T is the absolute temperature. One can
0.98 eV i.e., (E B 0.98 eV) for the Poole–Frankel estimate the values of activation energy from the
mechanism. slope of the graph between ln I versus 1/T (from
15112 J Mater Sci: Mater Electron (2022) 33:15107–15115

-13.8 -19.7
As2Se3 Fresh, 500V As2Se3 Fresh, 500V 323 K
328 K
-14.1 333 K
-19.9
338 K
-14.4 343 K

-20.1

ln(I/V) (mho)
-14.7
lnI (A)

-15.0
-20.3

-15.3 323 K
328 K
333 K -20.5
-15.6 338 K
343 K
-15.9 -20.7
10 12 14 16 18 20 22 24 50 120 190 260 330 400 470 540
1/2
V (Volts) V (Volts)

-13.6 -19.8
As2Se3 Aged, 500V As2Se3 Aged, 500V 323 K
328 K
-14.0 333 K
-20.0
338 K
-14.4 343 K

-20.2

ln(I/V) (mho)
-14.8
lnI (A)

-15.2
-20.4

-15.6 323 K
328 K
333 K -20.6
-16.0
338 K
343 K
-16.4 -20.8
8 10 12 14 16 18 20 22 24 30 90 150 210 270 330 390 450 510
1/2
V (Volts) V (Volts)

Fig. 5 Variation of ln I versus V1/2 and ln (I/V) versus V for both As2Se3 fresh/aged samples

Se Fresh Se Aged
-24.1 -21.3
ln[I/T 2] ( AK-2)
ln[I/T 2] ( AK-2)

300 V 300 V
-24.4 -21.6
350 V 350 V
-24.7 400 V -21.9 400 V
450 V 450 V
-25 -22.2
500 V 500 V
-25.3 -22.5
3.07 3.12 3.17 3.22 3.27 3.32 3.07 3.12 3.17 3.22 3.27 3.32
1000/T(K) 1000/T(K)

As2Se3 Fresh As2Se3 Aged

-25.4 -25.4
ln[I/T 2] ( AK-2)

ln[I/T 2] ( AK-2)

300 V 300 V
-25.7 -25.7
350 V 350 V
-26 400 V -26 400 V
450 V 450 V
-26.3 -26.3
500 V 500 V
-26.6 -26.6
2.9 2.95 3 3.05 3.1 2.9 2.95 3 3.05 3.1
1000/T(K) 1000/T(K)

Fig. 6 Variation of ln [I/T2] versus reciprocal of temperature for both Se as well as As2Se3 fresh and aged samples
J Mater Sci: Mater Electron (2022) 33:15107–15115 15113

Eq. 3) as shown in Fig. 7. The calculated values of Table 1 The activation energy of fresh/aged Se as well as As2Se3
activation energy are found to be less than 980 meV samples
(given in Table 1) thereby indicating that the Poole– Voltage (V) Se As2Se3
Frenkel mechanism occurs in the dominant mode for
these investigated samples. Fresh Aged Fresh Aged
DE (meV) DE (meV) DE (meV) DE (meV)
From Table 1, we see that activation energy is
increased appreciably after aging in both g-Se and 300 121 186 206 223
g-As2Se3. Luckabauer et al. [49] observed a reduction 350 121 174 208 217
in the activation energy of fast relaxation processes in 400 113 168 203 225
a metallic glass during aging. Elabbar [50] also found 450 103 154 208 221
that the activation energy for glass transition 500 93 154 208 217
decreases with aging in glassy Se and Se90Te10 glass.
On other hand, Vyazovkin and Chen [51, 52] reported
an increase in effective activation energy of a-relax- that the leading mechanism of high-field conduction
ation during the physical aging of a glassy maltitol. in both aged and fresh samples of g-Se and g-As2Se3
Thus, it is clear that the results of aging effects on the is governed by the Poole–Frenkel effect. However,
activation energy of different physical phenomena the activation energy related to the PF conduction is
are highly diversified in nature and so more work is increased in the case of the aged sample of g-Se,
required in this direction. while it remains almost the same for the aged sample
of g-As2Se3. This signifies the noticeable signs of
aging in g-Se over g-As2Se3. This is also reflected in
5 Conclusions the current–voltage characteristics of fresh/aged
samples of g-Se and g-As2Se3.
The effect of aging on high-field conduction is stud-
ied in g-Se and g-As2Se3 by comparing their current–
voltage characteristics. The detailed analysis confirms

Se Fresh Se Aged
-12.6 -9.6
300 V -9.9 300 V
-12.9
350 V 350 V
-10.2
lnI

lnI

-13.2 400 V 400 V

-10.5
450 V 450 V
-13.5 -10.8
500 V 500 V
-13.8 -11.1
3.07 3.12 3.17 3.22 3.27 3.32 3.07 3.12 3.17 3.22 3.27 3.32
1000/T(K) 1000/T(K)

As2Se3 Fresh As2Se3 Aged

-13.8 -13.9
300 V 300 V
-14.1 -14.2
350 V 350 V
lnI

lnI

-14.4 400 V -14.5 400 V

450 V 450 V
-14.7 -14.8
500 V 500 V
-15 -15.1
2.9 2.95 3 3.05 3.1 2.9 2.95 3 3.05 3.1
1000/T(K) 1000/T(K)

Fig. 7 Exponential variation of current against temperature for both Se as well as As2Se3 fresh and aged samples
15114 J Mater Sci: Mater Electron (2022) 33:15107–15115

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