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Electrochemical and spectroscopic characterization of a new polymerbased on eriochrome black T doped by carbon nanotubes
OUAHIBA BOURICHE1,2,* , NAIMA MAOUCHE3, HICHAM KOUADRI1,2
and DJAHIDA LERARI21Laboratory: Preparation and Modification of Multiphase Polymeric Materials, Department of Process Engineering,
University of Ferhat Abbas Setif, 19000 Setif, Algeria2Center of Scientific and Technical Research in Physicochemical Analyzes (CRAPC), 42004 Tipaza, Algeria3Laboratoire d’Electrochimie et Materiaux, University of Ferhat Abbas Setif, 19000 Setif, Algeria
*Author for correspondence (anesk2011@yahoo.fr)
MS received 2 May 2020; accepted 22 October 2020
Abstract. An electropolymerized film of new eriochrome black T (EBT) doped with carbon nanotubes (CNTs) has been
prepared on the surface of indium tin oxide (ITO) in a solution of acetonitrile containing lithium perchlorate (LiClO4) as
supporting electrolyte by cyclic voltammetry (CV). The distribution of CNTs in the poly eriochrome black T (PEBT)
matrix was studied through scanning electron microscope (SEM) and energy-dispersive X-ray spectroscopy. Their
chemistry and electrical properties were determined by CV and electrochemical impedance spectroscopy (EIS). The
optical characterization of the composites was made by UV–Vis absorption. The results showed that CNTs nanoparticles
were dispersed and co-deposited into the PEBT matrix; the voltammogram of EBT before and after doping with the
semiconductor of CNTs present a large difference in the form of recorded cyclic voltammograms. It is noticed that the
shape (intensity, potential and number of redox couple) of the cyclic voltamperogram varies with the addition of CNTs;
the appearance of new peaks of oxidation and reduction suggests the formation of a new composite material. This
confirmed that there is a reaction which develops between the EBT, CNTs and LiClO4. The best distinction of the peaks
was obtained during the addition of 0.2 mg of CNTs, leading to increase the conductivity of the PEBT film that forms on
the ITO electrode. The images of SEM confirm the presence of CNTs in the composite, which consequently modifies
significantly the morphology of the film. The CV study showed redox couples characteristic of poly EBT at 0.6 and 0.5 V.
The EIS measurements show that the resistance of the PEBT films decreases with increasing of CNTs amounts. This
demonstrates that the inclusion of the CNTs enhance the electrical properties of the polymer. Thus, these composite films
can be used in various fields. The optical bandgap decreased generally with increase in content of CNTs compared with
PEBT only. This is explained by the introduction of the donor levels in the bandgap of PEBT by the CNTs, this decrease
in gap energy is explained by the Burstein–Moss effect.
Keywords. Electropolymerization; EBT; CNTs; CV; ITO electrode.
1. Introduction
The modification of the electrodes by polymeric films
take a great interest in the researchers in the last years,
because they have excellent physical and chemical
properties such as good stability, insolubility, homo-
geneity in the electrochemical deposit and a strong
adhesion to the surface of the electrodes, more active
sites [1–3].
Polymer-modified electrodes are widely applied in the
field of molecular electronic as organic light-emitting
diodes [4], sensors and supercapacitors [5].
In addition, poly eriochrome black T (PEBT) is a con-
ductive polymer that has very interesting analytical prop-
erties, it is characterized by the presence of high
concentration of negative charges of sulphate group –SO–3
on its surface [6–10].
Consequently, PEBT [10] has an affinity for the incor-
poration of counter-ions or other form of functions to have
electronic properties similar to metals in addition to con-
ventional properties of organic polymers. It can distinguish
interference via hydrophobic and hydrophilic affinities,
hydrostatic interaction or ion exchange capacity. It could
also avoid deterioration of the electrodes by forming a
surface protection by its deposit. Recently, PEBT-modified
glassy carbon electrodes (GCEs) have been used for
voltammetric analysis of pharmaceuticals, metals and bio-
logically active compounds, such as dopamine, uric acid
and ascorbic acid [7], adenine and guanine [8], nora-
drenaline [9] and mercury [10].
Bull. Mater. Sci. (2021) 44:76 � Indian Academy of Scienceshttps://doi.org/10.1007/s12034-021-02360-2Sadhana(0123456789().,-volV)FT3](0123456789().,-volV)
In the study by Wei et al [7], the PEBT film was ready by
simple electropolymerization in alkaline solution containing
EBT.
Hong et al [2] also described an electropolymerized film
of PEBT-modified GCE by cyclic voltammetry (CV). The
PEBT film at the electrode conspicuously enhanced the
redox peak current of dopamine and could separately
determine it at its low concentration (0.1 M) in the presence
of 4000 and 700 times higher concentrations of ascorbic
acid and uric acid, respectively.
In another study, Hong et al [11] fabricated PEBT
membrane on the surface of the GCE in a 0.01 M NaOH
solution with CV. The polymer has been shown to be
electrically active for the oxidation of epinphrine.
The electrochemical behaviour of PEBT was investigated
at a carbon paste electrode by Chandra et al [12]. It showedirreversible two-step one electron reduction mechanism in
cyclic voltammograms and the electrochemical process was
diffusion controlled.
A reversible CV of an aqueous solution of EBT was
provided by Bedoui et al [13] on carbon-doped diamond
electrode. However, these works do not suggest any
methodology for the sensitive determination of PEBT in
aqueous solutions. In many cases, PEBT was used on dif-
ferent working electrode surfaces to enhance the sensitivi-
ties of these electrodes to some specific analysis [14–21].
Cittan et al [22] have studied electrochemical detection
for the analysis of traces of EBT using a GCE modified with
multi-wall carbon nanotubes (CNTs) by voltammetric
adsorption with linear scanning. There are few reports of
research on the measurement of EBT in environmental
systems. In research published by Zahran et al [23], a novelelectrochemical displacement method is reported to assess
EBT in natural water, which is based on the modified GCE
silver nanoparticles produced by Ficussycomorus Latex.
For the first time, a new type of material produced by in-situ electropolymerization of EBT has been proposed by
Tavares and Sales [24] to produce molecularly imprinted
polymers (MIP) suitable for protein recognition.
CNT is a material of choice for the development of new
materials for applications in many fields such as electronics,
chemistry, biochemistry and electrochemistry. CNTs have
caused a revolution in the field of nanotechnology, and the
advent of the nano world. Thus, these nano-objects have
provoked a real craze in many research laboratories since
they bring an undeniable wealth of many fields.
The doping of polymeric matrices by the incorporation of
CNTs has also been reported in the literature in various
applications. As a result, composite materials resulting from
the insertion of nano-objects into conductive polymers often
have improved with novel properties (which are not
observed in the constituents when considered individually).
Little literature (if we can say there are no studies) are
available on the development of a new PEBT composite
material doped with CNTs by electrochemical polymer-
ization. In this study, we present for the first time a
successful and a facile electrochemical, one-step method to
modify the surface of ITO with PEBT ? CNTs nanocom-
posite in acetonitrile medium to obtain a new composite
(PEBT ? CNTs)/ITO. The occupancy of CNTs leads to an
increase in the active surface area of new polymer formed.
The effect of CNT on the electrochemical, structural,
optical properties was investigated; the impedance spec-
troscopy measurements were used to get information on the
electrochemical properties and spectroscopic characteriza-
tion of composite materials obtained. The optical charac-
terization of the composites has been carried out by UV–Vis
transmittance, while the morphological properties have
been investigated by scanning electron microscopy (SEM)
and energy-dispersive X-ray (EDX) spectroscopy.
2. Experimental
2.1 Materials
Eriochrome black T (EBT, scheme 1) ACS reagent (indi-
cator grade) was purchased from Sigma Aldrich (France).
CNTs (purity[98%, diameter 110–170 nm, length 5–9 lm)
as a doping semiconductor was also obtained from Aldrich
(France). Supporting electrolyte used in electropolymer-
ization is lithium perchlorate (LiClO4, 0.1 M) (Fluka pro-
duct, Switzerland) dissolved in acetonitrile (CH3CN).
2.2 Instrumental analysis
The device used for electrochemical characterization is the
potentiostat/galvanostat type Voltalab 40 (PGP 301) radio-
meter driven by voltamaster software to choose the method
of analysis and data processing.
A conventional three-electrode system was used
throughout. The working electrode was a glass substrate of
indium tin oxide (ITO), the auxiliary electrode was plat-
inum (Pt); thread and a saturated calomel electrode (SCE)
was employed as a reference electrode. All electrode
potentials were reported referring to SCE electrode in this
article.
Electrochemical impedance spectroscopy (EIS) mea-
surements were performed using an alternative current
Scheme 1. Chemical structure of eriochrome black T [21].
76 Page 2 of 9 Bull. Mater. Sci. (2021) 44:76
voltage of 10 mV, at open circuit potential (Eocp), in the
frequency range 100 kHz and 10 mHz. The surface mor-
phology of PEBT, PEBT ? CNTs films was characterized
by SEM and EDX using JEOL Sam-700 1F.
A Shimadzu UV–Visible spectrometer (Japan) was used
to investigate the optical properties and optical gap (Eg) of
the composites; all measurements were performed at room
temperature.
2.3 Preparation of composite films
A new composite material poly (EBT ? CNTs) was elec-
trochemically synthesized in a glass cell obtained by CV,
containing the solution ? EBT (5 9 10-3 M) and semi-
conductor (CNTs) particles at v = 10 mV s–1, between -0.2
and 1.4 V/SCE, in which three electrodes are immerged.
The supporting electrolyte used is lithium perchlorate
(LiClO4), in acetonitrile (CH3CN). This electrolyte was
chosen because of its solubility in organic and aqueous
solution, and of its electrochemical stability on a large range
of potential.
3. Results and discussion
3.1 Electropolymerization of EBT in CH3CN medium
Figure 1 displays the cyclic voltamperograms of EBT
electropolymerization over the range of –0.2, 1.4 V at
10 mV s–1 for 20 cycles. During the polymerization process,
the oxidation and reduction peak potential appear at 0.6 and
0.5 V, respectively, as shown in figure 1a and b.
During successive scanning (20 cycles; figure 1a), an
increase in the intensity of oxidation and reduction currents
with cycling is observed. This is a proof of the deposition
of PEBT film on the surface of the electrode (ITO) and,
the increase in current intensity indicates that the
electrodeposited polymer is less conductive. The PEBT is
formed according to the proposed polymerization
(scheme 2) [21].
3.2 Electrochemical behaviour study of PEBT
After the formation of PEBT film, it was carefully washed
with distilled water and dried at ambient temperature to
study its electroactivity by CV in a potential range of –0.2 V
and 1.4 V/SCE.
As shown in figure 2, during the positive potential sweep
an anodic peak towards Epa = 0.76 V/SCE, corresponding
to the oxidation of the electrodeposited polymer on the ITO,
and to the backwards scan, the absence of the reduction
peaks was observed. It is found that the successive
recording (3 cycles) shows a decrease in the intensity of the
first cycle current, but after the second cycle, the voltam-
perogram becomes stable with the cycling suggesting the
electrochemical stability of the polymer.
3.3 Effect of nanotube content on PEBT
We studied the effect of the addition of CNTs, which has
been added by varying contents (0.1, 0.2, 0.4 mg) in the
solution of electropolymerization of EBT, for different
cycles. The corresponding cyclic voltamperograms are
grouped in figure 3.
When comparing the voltammogram of PEBT before and
after doping with the semiconductor, a large difference is
observed in the form of recorded cyclic voltammograms.
Note that the shape of the cyclic voltammogram presented
in figure 3(a–d) varied with the addition of CNTs by the
increase or decrease of current intensity and the shift of the
position of the peaks. The appearance of new oxidation and
reduction peaks was the sign of the formation of a new
composite material. These changes in the electrochemical
(a) (b)
Figure 1. Cyclic voltammograms corresponding to a solution of (EBT) 5 9 10-3 M dissolved in (LiClO4
0.1 M/CH3CN) obtained with v = 10 mV s–1, between -0.2 and 1.4 V/SCE. (a) 20 cycles and (b) first cycle.
Bull. Mater. Sci. (2021) 44:76 Page 3 of 9 76
behaviour of PEBT resulted from a reaction that developed
between the EBT, CNTs and LiClO4. The best distinction
of two redox couples was obtained during the addition of
0.2 mg of CNTs. This value appeared as the ideal content
corresponding to current intensity and therefore to increase
the conductivity of the PEBT film that formed on the ITO
electrode. After polymerization of PEBT in the presence of
CNTs, the ITO surface was covered with a uniform straw-
shaped film indicating that the PEBT composite film had
been electrodeposited successively on the surface of the
electrode.
3.4 Effect of cycling on PEBT
We undertook a study of the influence of cycle number on
the shape of the electropolymerization voltammogram of
EBT. Cyclic voltammograms relating to a solution of (EBT)
5 9 10-3 M dissolved in LiClO4 0.1 M/CH3CN, obtained
for different contents of CNTs, recorded at v = 10 mV s–1,
between -0.2 and 1.4 V/SCE, on an ITO electrode,
for different cycles (1, 5, 10, 20 cycles) are shown in
figure 4a–d.
According to figure 4, and in general, we note there is no
effect of the cycle number on the electrochemical behaviour
of virgin PEBT and PEBT doped with CNTs. Concerning
the effect of the addition of CNT on the behaviour of PEBT,
from the same figure, we observed that the addition of
0.1 mg of CNT in the solution increases the current of
intensity peaks of the PEBT formed and modified the
behaviour of this polymer; which implies an increase in the
active surface, and consequently increases the conductivity
of the film formed.
3.5 EIS of PEBT/ITO, PEBT/CNTs/ITO
The impedance diagrams for the PEBT and PEBT ? CNTs
films are plotted under the same experimental conditions
(figure 5). In general, all the added CNTs values decreased
the PEBT semi-circle. Thus, we often see that increasing the
concentration decreases the radius and therefore will
increase the physical phenomenon (the conductivity) of the
film that formed on the electrode surface. The correspond-
ing values are given in table 1, which were calculated once
by extrapolating the Nyquist plots.
Scheme 2. The proposed polymerization of EBT on PGE [21].
Figure 2. Cyclic voltammograms corresponding to the film of
PEBT in (LiClO4 0.1 M/CH3CN), recorded at v = 10 mV s–1,
between –0.2 and 1.4 V/SCE (3 cycles).
76 Page 4 of 9 Bull. Mater. Sci. (2021) 44:76
3.6 EDX elemental analysis of the PEBT and PEBT/CNTsfilms
The electrochemical polymerization on the ITO substract is
presented in figure 6a and b, respectively. The comparison
of the spectra corresponding to the films of the PEBT with
that of the composite material (PEBT ? CNTs) by the EDX
technique, gives us information on the elements present in
the material. Indeed, the EDX spectrum of the PEBT film
modified or not modified by the CNT, exhibits a carbon
(C) signal at 0.25 keV and sulphur (S) at 2.4 keV charac-
teristic of PEBT.
The peaks of chlorine (Cl) at 2.62 keV and oxygen (O) at
0.53 keV presented in figure 6a and b indicate that the
PEBT film is doped with perchlorate ions (ClO4–), which
has been used as a support electrolyte.
The incorporation of CNTs in the polymer film is con-
firmed by the EDX analysis, which shows the presence of the
carbon lines at 0.25 keV (figure 6b). The other elements (Si,
K, …) are characteristic of the presence of traces of impuri-
ties. Thus, the presence of CNTs in the composite film is
confirmed by SEM analysis. Therefore, we can conclude that
the CNT particles are incorporated into the polymer during
the electropolymerization of EBT, which led to the pigmen-
tation of the polymer film, and the formation of the composite
material on the electrode. Thus, interesting electrochemical
properties can be obtained, allowing the use of this composite
as electrode material in electrochemical, electronic and
electrocatalytic applications.
3.7 Surface morphology of PEBT/ITO, PEBT ? CNTs/ITO
The SEM images corresponding to the ITO plates, modified
by PEBT films and the composite material (EBT ? CNTs
(0.2 mg)) are represented, respectively, on figure 7a and b.
Comparing the micrographs of the composite material
PEBT ? CNTs/ITO and non-doped PEBT show that the
PEBT film has a well-defined homogeneous surface indi-
cating that the PEBT film has been successively integrated
on the surface of the electrode. However, after the poly-
merization of the EBT in the presence of CNTs, the surface
was also covered with a film of PEBT, which was mor-
phologically modified by the CNTs and the surface was
more amorphous and spongiest.
3.8 UV–Vis absorption spectroscopy study of PEBT
The optical measurements of the deposition of PEBT films
and (PEBT ? CNTs) for different content of CNTs 0, 0.1,
-0.3 0.0 0.3 0.6 0.9 1.2 1.5
0.0
0.2
0.4
0.6
0.8
1.0
1.2
E (V/SCE)
I (m
A/c
m2 )
(a)
0.63V
0.47V
-0.3 0.0 0.3 0.6 0.9 1.2 1.5
-0.4
-0.2
0.0
0.2
0.4
0.6
0.8
1.0
E (V/SCE)
I (m
A/c
m2 )
(b)
0.00V
0.91V
-0.3 0.0 0.3 0.6 0.9 1.2 1.5-0.3
0.0
0.3
0.6
0.9
1.2 (c)
E (V/SCE)
I (m
A/c
m2 )
0.88V
1.21V
1.03V0.80V
-0.3 0.0 0.3 0.6 0.9 1.2 1.5-0.01
0.00
0.01
0.02
0.03
0.04
0.05
I (m
A/c
m2 )
E (V/SCE)
(d)
0.69V
1.29V
0.45V
Figure 3. Cyclic voltammograms relating to a solution of (EBT) 5 9 10-3 M dissolved in LiClO4 0.1 M/CH3CN,
obtained for (a) 0 mg CNTs, (b) 0.1 mg CNTs, (c) 0.2 mg CNTs and (d) 0.4 mg CNTs, recorded at v = 10 mV s–1,
between -0.2 and 1.4 V/SCE, on an ITO electrode.
Bull. Mater. Sci. (2021) 44:76 Page 5 of 9 76
0.2 and 0.4 mg were carried out at room temperature. The
spectra of the optical transmission of the samples are shown
in figure 8a.
We note that the PEBT samples have a transmission of
59% and the optical transmittance intensity decreases with
the addition of CNTs in the visible domain. This result
confirmed that the addition of CNTs in the polymerization
solution involves the modification of the surface of the
PEBT films.
To estimate the optical gap Eg of the PEBT and (PEBT ?
CNTs) films that are presented in table 2, the characteristic
curves of (ahm)2 as a function of (hm) [25–27] were plotted,in figure 8b, where a is the absorption coefficient and hmthe photon energy. The value of the optical gap Eg is
(a) (b)
(c) (d)
Figure 4. Cyclic voltammograms relating to a solution of (EBT) 5 9 10-3 M dissolved in LiClO4 0.1 M/CH3CN,
obtained for different contents of CNTs, recorded at v = 10 mV s–1, between -0.2 and 1.4 V/SCE, on an ITO electrode
for different cycles (1, 5, 10, 20 cycles).
0 20 40 60 80 100 120-20
0
20
40
60
80
100
120
140
EBT EBT+0.1mg CNTs EBT+0.2mg CNTs EBT+0.4mg CNTs
Re(Z)(Kohm.cm2)
-Im(Z
)(Koh
m.c
m2 )
Figure 5. Nyquist diagrams relative to films of PEBT/ITO,
PEBT/CNTs/ITO for different content of semiconductor.
Table 1. Electrical parameters corresponding to the PEBT/ITO
and PEBT/CNTs films obtained for different content of CNT.
PEBT ? CNTs
CNTs (mg) 0 0.1 0.2 0.4
RX (kX) 121.0 27.19 — 30.41
Cdl (lF cm–2) 10.41 8.611 — 9.362
76 Page 6 of 9 Bull. Mater. Sci. (2021) 44:76
determined by extrapolating the linear part of the curve
from (ahm)2 to the axis (x) up to (ahm)2 = 0, as indicated in
figure 8b. The estimation of the optical gap Eg energies of
the films of PEBT and PEBT ? CNTs is summarized in
table 2.
Figure 9 shows the variation of the optical interval energy
Eg as a function of the mass of the CNTs to be added. This
figure shows a notable decrease in the energy of the optical
interval that goes from 2.38 to 1.22 eV when the mass of the
CNTs goes from 0 to 0.4 mg. This decrease in the energy of
the gap is explained by the Burstein–Moss effect [26].
Consequently, the optical bandgap of the film (PEBT) is
wider than that of the polymer doped with 0.4 mg of CNT.
This phenomenon can contribute to several parameters,
such as the thickness of the film, the concentration of charge
carriers and the presence of defects [26].
Figure 6. EDX patterns of (a) PEBT/ITO and (b) (PEBT ? CNTs)/
ITO.
Figure 7. Micrographs of (a) PEBT/ITO and (b) PEBT ? CNTs/ITO (0.2 mg).
Bull. Mater. Sci. (2021) 44:76 Page 7 of 9 76
4. Conclusion
The objective of our study is to develop and characterize
new composite materials based on PEBT electrodeposited
on transparent ITO electrodes using CV. These electrodes
have been modified by CNTs for the purpose of improving
its conductivity and modifying its electrochemical
properties.
In this study, we first studied the electrochemical
behaviour of PEBT separately in the absence of nan-
otubes, in a CH3CN/LiClO4 solution containing the
appropriate monomer (EBT). The doping by the nan-
otubes of the films obtained was done in situ (the addition
of the CNTs in the same solution of the polymerization)
to show the effect of the CNTs on the physicochemical
characteristics of the PEBT films. In this case, we fol-
lowed the evolution of their electrochemical behaviour
by the effect of the content of CNTs added (0.1, 0.2 and
0.4 mg).
The obtained electrochemical results showed that the
electrochemical polymerization of the films was carried
out successfully and quickly by formation of good
adhesive films covering the entire surface of the elec-
trodes. The addition of CNTs has significantly modified
the electrochemical properties; the SEM photographs
confirmed the modification of the morphology of the
composite films.
The comparison of the spectra corresponding to the films
of the PEBT with that of the composite material (PEBT ?
CNTs) by the EDX technique, gives us information on the
elements present in the material. The transmission mea-
surements performed by UV–Vis spectroscopy have also
shown that PEBT samples have a transmission of 59%, and
the optical transmittance intensity decreases with the addi-
tion of CNTs in the visible domain.
The optical bandgap decreased generally with increasing
of content of CNTs compared with PEBT only. This is
explained by the introduction of the donor levels in the
bandgap of PEBT by the CNTs, this decrease in gap energy
is explained by the Burstein–Moss effect.
(a) (b)
Figure 8. Variation of (ahm)2 vs. hm of (a) PEBT and (b) PEBT thin films electrodeposited at a different content of
CNTs.
0.0 0.1 0.2 0.3 0.40.0
0.5
1.0
1.5
2.0
2.5
cont
ent (
mg)
Eg (eV)
Figure 9. Variation of the optical gap energy of PEBT as a
function of the added content CNTs (0, 0.1, 0.2 and 0.4 mg).
Table 2. Estimation of the optical gap Eg energies of the films of
PEBT and PEBT ? CNTs.
Sample Bandgap (eV)
PEBT 2.38
PEBT ? 0.1 mg CNTs 2.38
PEBT ? 0.2 mg CNTs 2.21
PEBT ? 0.4 mg CNTs 1.22
76 Page 8 of 9 Bull. Mater. Sci. (2021) 44:76
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