Alexandria Engineering Journal (2018) 57, 3291–3297

H O S T E D BY
Alexandria University

Alexandria Engineering Journal

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ORIGINAL ARTICLE

Characterization of atypical polyaniline

nano-structures prepared via advanced techniques
A. Abdelraheem a,b,*, A.H. El-Shazly a,c, M.F. Elkady a,d

a
Chemical and Petrochemicals Engineering Department, Egypt-Japan University of Science and Technology, New Borg
El-Arab, Alexandria, Egypt
b
Occupational Health and Air Pollution Department, High Institute of Public Health, Alexandria University, Alexandria, Egypt
c
Chemical Engineering Department, Aculty of Engineering, Alexandria University, Alexandria, Egypt
d
Fabrication Technology Department, Advanced Technology and New Materials Researches Institute, City of Scientific
Researches and Technological Applications, New Borg El-Arab City, Alexandria 21934, Egypt

Received 10 July 2017; revised 22 November 2017; accepted 9 January 2018

Available online 13 December 2018

KEYWORDS Abstract Conductive polymers had been the topic of a vast number of investigations during the
Polyaniline nano-structures; last decades, so, the synthesis of conducting polymers and study of their physical properties has
Nanoparticles; been of prime importance. One of these conductive polymers is polyaniline. The current work is
Nanorods; to prepare polyaniline (PANI) nanostructured material via four different preparation techniques
Nanofibers; which were sol-gel, rapid mixing, sonochemical and supercritical carbon dioxide (SC-CO2) assisted
Sonochemical; polymerization. The morphology of the prepared PANI samples was determined using Transmis-
Sol gel; sion electron microscopy (TEM) and Scanning Electron Microscope (SEM). The molecular struc-
Rapid mixing polymeriza- ture of prepared PANI samples was characterized by Fourier transform infrared spectroscopy
tion; (FTIR) and X-ray diffraction (XRD). The electrical conductivity of the synthesized samples was
Supercritical carbon dioxide
assessed by using the four-probe method at room temperature. The surface area of the prepared
assisted polymerization;
Polyaniline characterization
samples was determined using Brunauer Emmett Teller (BET). The characterization results of
the prepared PANI confirm that the morphology, chemical composition, crystallinity, conductivity
and surface area were altered significantly as a consequence of its synthesis via atypical techniques.
Ó 2018 Faculty of Engineering, Alexandria University. Production and hosting by Elsevier B.V. This is an
open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

1. Introduction

Conducting polymers have been significantly investigated for

their wide applications as gas sensors, batteries, light emitting
* Corresponding author at: Chemical and Petrochemicals Engineering diodes, solar cells, electrochromic devices (ECDs), field effect
Department, Egypt-Japan University of Science and Technology, New
transistors, electronic circuit boards, and fuel cells. Polyaniline
Borg El-Arab, Alexandria 21934, Egypt. (PANI) is one of the most important conducting polymers
E-mail address: amira.abdelraheem@ejust.edu.eg (A. Abdelraheem). because of its excellent processability, environmental stability,
Peer review under responsibility of Faculty of Engineering, Alexandria and its oxidation or protonation adjustable electro-optical
University. properties as well as its potential for a variety of applications.
https://doi.org/10.1016/j.aej.2018.01.012
1110-0168 Ó 2018 Faculty of Engineering, Alexandria University. Production and hosting by Elsevier B.V.
This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
3292
Polyaniline can exist as a salt or base in three isolable oxida-
tion states (1) leucoemeraldine, the fully reduced state of
polyaniline, (2) emeraldine, the half-oxidized state, and (3)
pernigraniline, the fully oxidized state. The emeraldine salt is
electrically conductive while the rest are insulators. They have
interesting properties, particularly polyaniline exists in three
different oxidized forms, such as reduced (leucoemeraldine-
yellow), neutral (emeraldine salt-green or emeraldine base-
blue) and fully oxidized (pernigraniline-black), which shows
different conductivities [1,2]. Besides various nanostructures
of PANI (1D, 2D and 3D structures) have been prepared
and studied extensively. The nanostructure, chemical and
physical properties of the prepared PANI depend mainly on
the preparation technique [3]. Polyaniline and its derivatives
were synthesized through two general routes: (a) electrochem-
ical, and (b) chemical methods. The common method for fab-
rication of polyaniline in large quantities is based on chemical
methods. In conventional chemical methods, the aniline is
polymerized in water-based solution in the presence of oxidant
and dopant [4]. Generally, there are different techniques could
influence the morphology of produced polyaniline such as
sonochemical and SC-CO2 assisted polymerization. In general,
the application of ultrasound radiation in polymerization can
improve the chemical reaction rate and can destroy the aggre-
gation and reduce the particle size due to its dispersion, crush-
ing, emulsifying and activation effect resulting in controlled
PANI morphological structure [5–8]. Another advanced poly-
merization technique that has been applied for foaming pur-
poses is supercritical CO2 assisted polymerization. The merits
of this advanced synthesis technique are reducing the waste
problem so it is considered environmentally benign technique.
Besides, the power of SC-CO2 in dissolving the solutes and
enhancing the diffusivity between reactants is significant.
Moreover, the SC-CO2 power can be altered by changing tem-
perature and pressure. Meanwhile, the elimination of unre-
acted materials and side products can be done easily
resulting in preparing PANI with high purity [9,10]. This paper
aims to study the preparation of PANI via four different tech-
niques sol-gel, rapid mixing, sonochemical and CO2 assisted
polymerization and investigating the effect of the synthesis
method on the morphology, chemical and physical character-
istics of the prepared PANI, regarding that all the operating
parameters are kept constants.
2. Materials and methods
2.1. Chemicals
Aniline (0.2 M), Hydrochloric acid (HCl 1 M), potassium per
sulphate (KPS 0.2 M), methanol (Sigma Aldrich, USA) and
distilled water.
2.2. Characterization
The scanning electron microscope (JEOL JSM-6010LV and
JEOL JSM-7500F) besides JEOL JEM-2100F transmission
electron microscope were used to examine the morphological
structure of the synthesized PANI materials. The chemical
structure of PANI was confirmed by Fourier transform infra-
red spectroscopy technique using (Vertex 70, Bruker scientific
instruments, Germany) between a range of 4000–400 cm 1.
A. Abdelraheem et al.
X-ray diffraction was used to confirm the crystalline structure
of the prepared PANI samples using (Shimadzu Xlab 6100).
The surface area and pore size of PANI samples were identified
by N2 adsorption-desorption at 77 K with the BET and BJH
methods using a Belsorp II mini (BEL Japan Inc). The conduc-
tivity of the prepared PANI samples was determined using
four probes method.
2.3. Synthesis methods
Aniline was dissolved in 50 ml HCl (1 M) at room temperature
and 50 ml of (0.2 M) KPS was promptly added to the preced-
ing aniline and HCl mixture and mixed together for three
hours. For sol-gel technique, (Fig. 1a), all the reactants were
added together and left the solution without applying any
external physical force to complete the polymerization reac-
tion. While for rapid mixing, (Fig. 1b), the reactants solutions
were mixed together using magnetic stirrer at 700 rpm. The
sonochemical technique involved the application of ultrasonic
irradiation to the reactants solution for the pre-set polymeriza-
tion time (Fig. 1c). Regarding the CO2 assisted polymerization;
the reactants were mixed together inside a high-pressure vessel
which is connected to CO2 pump. CO2 was pressurized into the
reactor at 10 MPa pressure and 40 °C temperature for three
hours (Fig. 1d). After termination of the polymerization pro-
cess, the produced precipitate was washed several times using
hydrochloric acid, methanol, and distilled water and filtered
by centrifugation and then vacuum dried at 60 °C for 24 h.
3. Results and discussion
3.1. Morphology
The morphology of the synthesized PANIs samples was exam-
ined using SEM and TEM techniques and presented at Figs. 2
and 3. First, the preparation of PANI via sol-gel technique
resulted in producing PANI with nanoparticle morphology
(PANI-NP) because of slow diffusion and polymerization rate
of aniline contributing in the production of spherical nanopar-
ticles. From previous studies, the usage of strong inorganic
acid always yielded PANI granules, spherical and non-
spherical particles depending on various reaction conditions
like molar ratios between monomer and oxidizing agent, reac-
tion time and acidity. Granules of PANI were successfully pre-
pared by the same techniques despite using sulfuric acid
(strong acid) which promote the formation of granular nanos-
tructured PANI rather than other structures that can be pro-
duced using week acid that suppress the nanoparticles
fabrication and promote nanotube formation [11]. From
SEM and TEM images the average diameter of the prepared
nanoparticles was about 60 nm. The same range of average
diameter was prepared by more complicated synthesis method,
ultrasonic assisted inverse micro-emulsion polymerization,
adding a benefit to sol gel polymerization method as it the sim-
plest method of PANI synthesis [6]. While the application of
mechanical stirring as a mixing routine resulted in fabricating
PANI with nanofiber morphology (PANI-NFR) [11–15]. It is
noticed that the average diameter of fibers was about 90 nm
while the length was about 200 nm. Sonochemical polymeriza-
tion of polyaniline improved the nanofibers (PANI-NFS)
aspect ratio resulting in preparing thinner and longer
Characterization of atypical polyaniline nano-structures
A Sonicator
B APS
sol.
APS
sol.
Aniline
sol.
Aniline sol. Magnetic stirrer
Heater
Pressure
gauge
High pressure
vessel
Fig. 1 Schematic diagram of the four synthesis techniques (A) sol gel, (B) rapid mixing, (C) sonochemical polymerization, (D) SC-CO2
assisted polymerization.
nanofibers than those prepared via rapid mixing method. The
synthesized (PANI-NFS) nanostructure average diameter and
length were about 60 and 400 nm respectively. The formation
mechanism of nanofibers still unclear but applying rapid mix-
ing causes the rapid consumption and diffusion of aniline and
KPS preventing the formation of nanoparticles and producing
primary nanofibers. Xinli Jing et al prepared nanofibers with
diameter of 50 nm by the same techniques, rapid mixing and
ultrasonic polymerization with different molar ratios of aniline
and oxidizing agent. Shorter and thicker fibers were obtained
by rapid mixing than Sonochemical polymerization and this
is with good agreement with our study. [17]. Beside that short
polymerization time was applied to prevent the secondary
growth of nanofibers leading to less agglomeration. B.A.
Bhanvase and S.H. Sonawaneb stated the advantages of apply-
ing ultrasound irradiation during polymerization. First ultra-
sonication improves the rate of the polymerization reaction.
Secondly narrow molecular weight and particles size distribu-
tion were obtained and more radicles were generated, all of
these factors are leading to yield thinner more long nanofibers
[18]. More uniform and harmonized nanorod PANI structure
(PANI-NR) was prepared by using supercritical CO2 assisted
3293
C
APS
sol.
Aniline
sol.
Water bath
CO2 gas
cylinder
CO2 pump
polymerization technique. The use of SC-CO2 facilitate dis-
solving of reaction solutes together owing to its high solvation
power besides producing high purity product. The high solva-
tion power of SC-CO2 enhance rapid polymerization reaction
and prevent agglomeration of the produced nanostructure [9].
The mechanism of PANI nanorod formation, using different
synthesis method, was clearly discussed by Haibing Xia et al
[19]. They claimed that, at the initial stage, nanoparticles of
PANI were created then these particles attached together by
hydrogen bond forming rodlike structure. In our case the pres-
ence of SC-CO2 improved the linear growth of the nanostruc-
ture resulting in fabricating uniform PANI-NR with average
diameter of approximately 80 nm.
3.2. Crystallinity
Fig. 4 shows the XRD patterns of the different synthesized
PANI structures via the pre-mentioned four techniques (sol-
gel, rapid mixing, sonochemical and SC-CO2 polymerization).
As previously stated that the prepared PANI ascertain mainly
two definite peaks at 2h = 20° and 25° which were assigned
3294 A. Abdelraheem et al.

Fig. 2 SEM of (A) PANI-NP (B) PANI-NFR (C) PANI-NFS and (D) PANI-NR.

Fig. 3 TEM of (A) PANI-NP (B) PANI-NFR (C) PANI-NFS and (D) PANI-NR.

to the periodicity parallel to the polyaniline chains and perpen- prepared PANIs depend significantly on the synthesis tech-
dicular to the polyaniline chain respectively [16,17]. The loca- nique and all the XRD patterns confirmed that the prepared
tion and strength of the peaks in the XRD spectra of all PANIs are typical emeraldine salt of partial crystallinity
Characterization of atypical polyaniline nano-structures 3295

800

600
Intensity Sol gel

Sonochemical
400
SC-CO2

Rapid mixing
200

0
0 10 20 30 40 50 60 70 80 90
2θ

Fig. 4 XRD spectra for the PANI synthesized via sol gel, rapid mixing, sonochemical and SC-CO2 assisted polymerization.

1.4

Sol gel
Transmiance %

1.2 Rapid mixing

Sonochemical

1 SC-CO2

0.8

0.6
0 500 1000 1500 2000 2500 3000 3500 4000 4500
Wave number cm-1

Fig. 5 FTIR spectra for the PANI synthesized via sol gel, rapid mixing, sonochemical and SC-CO2 assisted polymerization.

nanostructures. The XRD spectra of the PANI-NP and PANI-
NFR produced via sol-gel and rapid mixing techniques respec-
tively show the two characteristic peaks of PANI at
2h = 19.34°, 24.3° and 19.48°, 25.82° with approximately the
same intensity. While PANI prepared via Sonochemical
(PANI-NFS) and SC-CO2 assisted polymerization (PANI-
NR) have their peaks around 2h = 21.12°, 25.62° and
20.04°, 25.64°. Closer examination of the peaks intensities, it
is noticed that the two characteristic peaks of PANI-NP and
PANI-NFR have approximately the same intensity and this
indicates that the prepared PANI is poorly doped. While the
intensity of the peak at 2h = 25.62° and 25.64° in case of the
prepared PANI-NFS and PANI-NR synthesized via Sono-
chemical and SC-CO2 polymerization respectively is more
intense than the peak at 2h = 21.12°, and 20.04° indicating
that the prepared samples are highly doped PANI [18].
Another peak strongly appeared at 2h = 6.84° and 6.5° in
the case of PANI-NP and PANI-NFR and disappeared in case
of PANI-NFS and PANI-NR. This peak related to the period-
icity along the polymer chain and denoted that these PANIs
samples are highly crystalline nanostructure [19]. The XRD
patterns are in good agreement with the information given in
the morphology section and FTIR data.
3.3. Chemical composition
The FTIR spectra of the synthesized four PANI morphologies
in the range from 400 to 4000 cm 1 are shown in Fig. 5. It was
observed that there is a similarity between FTIR spectra of the
prepared PANIs that synthesized via the four techniques men-
tioned before. Table 1 displays the absorption characteristic
bands of the synthesized PANIs four samples [3,4,20,21].
The values of characteristic peaks of PANI-NP prepared by
sol gel were in good agreement with the values of PANI gran-
ules prepared by I. Sedenkova [11]. Comparing the FTIR
results of the synthesized nanofibers by rapid mixing and ultra-
sonic polymerization, there is noticeable shifting in the
1589.2 cm 1 band down to 1571 cm 1 assigned to high doping
level and conductivity and this matches the results obtained
from SEM images where more thinner and uniform nanofibers
were prepared using ultra-sonication. Approximately compa-
rable values of characteristic peaks of nanofibers were men-
tioned in Xinli Jing study and the slight variances between
these values for the same nanostructure (nanofibers) and the
PANI-NFR and PANI-NFS may be due to the alteration of
synthesis method [17]. For PANI-NR, comparing the values
of characteristic peaks of PANINR, in the table, with
3296 A. Abdelraheem et al.

Table 1 Absorption bands of synthesized PANIs samples.

Absorption bands (cm 1) Synthesized PANIs samples
PANI-NP PANI-NFR PANI-NFS PANI-NR
Quinoid ring stretching vibrations 1587.3 1589.2 1571 1576.6
Benzenoid ring stretching vibrations 1502.5 1508.2 1475.5 1479.3
C–N stretching vibrations 1303.8 1307.6 1299.8 1305.7
C–H in-plane bending vibrations 1143.7 1151.4 1134.1 1136.4
N–H stretching vibrations 3456.2 3460.1 3460 3462.1
C–H out of plane bending vibration 831 836.1 806.6 808.3

prepared samples due to the usage of low acid molarity [6].

Table 2 Surface area, total pore volume and average pore Besides the time of polymerization was approximately one
diameter of PANIs samples. hour that did not produce a polymer with high molecular
Synthesis Surface area Total pore Average pore
weight consequently this leads to lower conductivity of the
method (m2/g) volume (cm3/g) size (nm) synthesized PANI samples [23].
PANI-NP 20.782 0.0294 14.566
PANI- 33.37 0.084 10.107
4. Conclusion
NFR
PANI-NFS 35.085 0.099 11.292 Various PANI nanostructures with different characteristics
PANI-NR 24.61 0.0336 5.466 were synthesized by mixing the aniline and KPS solutions in
the presence of mechanical mixing, ultrasonic irradiation and
SC-CO2 that were compared with PANI prepared by mixing
nanorods prepared by Haibing Xia et al, there were close with the reactants only without applying any external influence.
little difference due to the change in preparation technique and All the reaction parameters were kept unchanged to investigate
the presence of hydrophilic Allura Red as a structure-directing the real effect of synthesis techniques on the characteristics of
agent [19]. the synthesized PANIs. The polymerization time was main-
tained fixed at three hour to prevent the further growth of
3.4. Porosity the targeted PANIs nanostructure into thicker and agglomer-
ated structures. The morphology of the prepared PANIs varied
Table 2 shows the BET surface area, total pore volume and from nanoparticles, nanofibers (with low and high aspect
average pore size of prepared PAN-NP, PANI-NFR, ratio) and nanorods by changing the synthesis method from
PANI-NFS and PANI-NR. The surface area and the total sol-gel, rapid mixing, sonochemical and SC-CO2 polymeriza-
pore volume of PANI-NF (either it prepared via rapid mixing tion respectively. The crystallinity of the synthesized PANIs
or sonochemical polymerization) were larger than those of the prepared via sol-gel and rapid mixing was higher than that
PANI-NP and PANI-NR morphologies [22]. Comparing the exposed to ultrasonic irradiation or SC-CO2. While there
BET surface area values in the current study with polyaniline was a nonsignificant variation in the chemical composition
prepared by the same protonic acid (HCl) in Jing Wang et al of the synthesized PANIs. Another PANI property of BET
study, it was found that the polyaniline prepared using surface area was influenced significantly by altering the synthe-
sono-assisted synthesis has lower value (22.38 m2/g) than sis method and it ranged approximately from 20 to 35 m2/g.
PANI-NFR (33.37 m2/g), PANI-NFS (35.085 m2/g) and Moreover, the conductivity of the synthesized PANIs also
PANI-NR (24.61 m2/g) [27]. changed and ranged from 1.6  10 8 to 2.7  10 5 S/cm.

3.5. Conductivity Acknowledgment

There are many parameters that control the conductivity of
prepared PANI, the doping level, the oxidation state, mor-
phology, molecular weight and crystallinity. From the pre-
mentioned data, these parameters can be affected by the syn-
thesis technique. The conductivity of the synthesized PANI-
NP was about 1.6  10 8 S/cm. This value is considered too
low compared with nanoparticles prepared by Byoung-Jin
Kim et al and the main reason was the different synthesis
method [28]. While the conductivity of nanofibers obtained
by rapid mixing and sonochemical polymerization were
1.5  10 7 and 1.3  10 6 S/cm respectively. The highest con-
ductivity was assigned to the nanorods prepared by SC-CO2
assisted polymerization method (2.7  10 5 S/cm). The
obtained conductivity values were not high enough and that
may be due to several reasons. The low doping level of the
This work is supported by Egyptian Ministry of Higher Edu-
cation, Egypt (for fully funded Ph.D grant), Egypt-Japan
University of science and technology (E-JUST) and kyoto uni-
versity for the facilities required to accomplish this work.
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