Cellulose (2012) 19:1645–1654
DOI 10.1007/s10570-012-9754-9
ORIGINAL PAPER
Electrically conducting nanocomposites: preparation
and properties of polyaniline (PAni)-coated bacterial
cellulose nanofibers (BC)
D. Müller • J. S. Mandelli • J. A. Marins •
B. G. Soares • L. M. Porto • C. R. Rambo •
G. M. O. Barra
Received: 8 February 2012 / Accepted: 23 July 2012 / Published online: 1 August 2012
Ó Springer Science+Business Media B.V. 2012
Abstract Free-standing films of bacterial cellulose
(BC) and polyaniline (PAni) (BC/PAni) composites
with high electrical conductivity values (0.9 S cm-1)
and good mechanical properties (40 MPa) were
prepared through in situ oxidative chemical polymer-
ization of aniline (Ani) on the surface of synthesized
BC nanofibers by using FeCl36H2O, as oxidant. The
influence of polymerization conditions such as oxidant
content, protonic acid, and reaction time on electrical
conductivity, morphological, tensile properties and
thermal stability of the BC/PAni composites was
investigated. Electrical conductivities of BC/PAni
composites increased with increasing reaction time
due to the formation of a continuous layer that
completely coated the nanofiber surface. FTIR spectra
of BC/PAni composites produced with and without
D. Müller  J. S. Mandelli  G. M. O. Barra (&)
Polymer and Composites Laboratory, Mechanical
Engineering Department, Federal University of Santa
Catarina (UFSC), Florianopolis, SC, Brazil
e-mail: guiga@emc.ufsc.br
J. A. Marins  B. G. Soares
Centro de Tecnologia, Federal University of Rio de
Janeiro, Rio de Janeiro, RJ, Brazil
L. M. Porto
Chemical and Food Engineering Department,
UFSC, Florianopolis, SC, Brazil
C. R. Rambo
Electrical Engineering Department, UFSC,
Florianopolis, SC, Brazil
protonic acid exhibited overlapped absorption bands
of both BC and PAni, except for quinoid and benzoid
bending modes of PAni. The in situ oxidative chem-
ical polymerization gives rise to conducting mem-
branes with the surface constituted by different PAni
content, as indicated through CHN elemental analysis.
The crystalline structure of BC was not affected by the
incorporation of PAni. Scanning electron microscopy
analysis of the composites revealed that PAni con-
sisted of nanoparticles around 70 nm in mean size to
form a continuous coating that encapsulates the BC
nanofibers. The BC/PAni composites obtained by the
method described in this work have interesting
properties that may find important technological
applications such as sensors, electronic devices,
intelligent clothes, flexible electrodes and tissue
engineering scaffolds.
Keywords Bacterial cellulose  Polyaniline 
Conducting composites
Introduction
There is a growing interest in developing nanofiber—
based conducting composites containing intrinsically
conducting polymers (ICP), such as polyaniline (PAni)
and polypyrrole (PPy) for a number of technological
applications, including electronic devices, sensors, and
intelligent clothes. These materials are generally
obtained through in situ oxidative polymerization of
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pyrrole (Py) or aniline (Ani) in the presence of
industrial textiles (Lee and Hong 2000; Cucchi et al.
2009; Johnston et al. 2005; Beneventi et al. 2006) or
electrospun nanofibrous templates (Li et al. 2006; Liu
et al. 2008; Chronakis et al. 2006; Picciani et al. 2009).
Among several nanofiber—based materials, bacte-
rial cellulose (BC) can be an attractive insulating
polymer matrix for the preparation of conducting
nanocomposites. BC is a versatile biopolymer with a
wide range of properties that can be used for several
applications, including biomedical devices and scaf-
folds for tissue and organ engineering (Rambo et al.
2008; Recouvreux et al. 2011). This polymer is
produced through cellulose biosynthesis in aqueous
solution and exhibits a nanofibrous network similar to
that those found in electrospun polymer scaffolds.
Moreover, these materials can maintain their structure
and mechanical stability even in hydrogel form. In this
context, conducting nanocomposites comprised of BC
coated with conducting polymers emerge as new
promising polymer platform that present a unique
combination of the tensile strength, toughness, bio-
compatibility, high surface areas with the non cytotoxy
(Li et al. 2006; Kamalesh et al. 2000), electronic,
optical, magnetic and chemical properties of conduct-
ing polymers (Müller et al. 2011) .
Although several papers deal with the preparation of
cellulose—based conducting materials (Sasso et al.
2010a, b) only very recently was BC employed for this
purpose (Müller et al. 2011; Marins et al. 2011; Hu
et al. 2011; Lee et al. 2012). Some studies dealing with
carbon nanotubes (Yoon et al. 2006; Yan et al. 2008;
Chen et al. 2010) or silver nanoparticles (Barud et al.
2008; Maneerung et al. 2008; Santa Maria et al. 2009)
filled BC composites were reported in the literature.
However, the first BC/ICP conductive nanocomposite
with electrical conductivity value as high as 1 S cm-1
was recently reported by Müller et al. (2011). In this
work, dried BC nanofibers were coated with polypyr-
role through in situ oxidative polymerization of pyrrole
aqueous solution by using iron III chloride
(FeCl36H2O), as oxidizing agent. BC/PAni compos-
ites, on the other hand, have been developed by
different groups. Marins et al. performed the in situ
polymerization of aniline in the presence of BC
hydrogel sheets (Marins et al. 2011). The polymeriza-
tion occurred in the presence of dodecylbenzene
sulfonic acid (DBSA) and ammonium persulfate
(APS). According to the authors, the morphology,
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Cellulose (2012) 19:1645–1654
crystallinity degree and electrical conductivity were
affected by DBSA concentration. Hu et al. used wet BC
membranes and studied the influence of reaction time
and different types of protonic acids on the electrical
conductivity of BC/PAni composites (Hu et al. 2011).
As expected, the amount of PAni deposited on the BC
nanofibers and electrical conductivity values of BC/
PAni blends enhanced with increasing the reaction
time reaching a maximum of 5 9 10-2 S cm-1 after
90 min. Lee et al. (2012) obtained BC/PAni compos-
ites through direct in situ polymerization of aniline on
BC fibers by using HCl and p-toluene sulfonic acid
(PTSA) solutions as protonic acid and APS, as the
oxidant. Electrical conductivity values of BC/PAni
doped with and without PTSA were 1.3 and
0.8 S cm-1, respectively. All BC/PAni reported in
the literature employed APS as the oxidant. The FeCl3
should be a good approach for preparing these
conducting nanocomposites because in aqueous solu-
tions, iron III forms aquo-hydroxyl complexes (Hosny
et al. 1997; Sasso et al. 2010a, b) and some of them
(mainly Fe3? and Fe(OH)2?) are adsorbed on a-
cellulose surface (Beneventi et al. 2006). When an
appropriated amount of iron III is adsorbed on the
cellulose fibers, the polymerization takes place pref-
erentially on the fiber surface to form a continuous
conducting coating that fully encapsulates the fibers
without altering significantly their morphology and
physical–chemical properties (Beneventi et al. 2006;
Johnston et al. 2005; Kelly et al. 2007). Considering the
reported advantages of FeCl3 as the oxidant, the aim of
this work is the preparation and characterization of
conducting nanomaterial through in situ chemical
polymerization of aniline in the presence of hydrated
BC by using iron (III) chloride hexahydrate.
Experimental
Materials
Aniline (analytical grade, Merck) was distilled under
vacuum and stored in a refrigerator. Iron (III) chloride
hexahydrate (FeCl36H2O) was purchased from Vetec
and used without any further purification. Glu-
conacetobacter hansenii, strain ATCC 23769,
acquired from the ‘‘Collection of Tropical Culture
(CCT)’’ (André Tosello Foundation, Brazil) was used
for the cellulose production.
Cellulose (2012) 19:1645–1654
Synthesis of bacterial cellulose
The bacterial cellulose (BC) membrane synthesis was
carried out by cultivating the bacterium for 3 days,
under static conditions, according to the procedure
described elsewhere (Rambo et al. 2008). Briefly, G.
hansenii pre-cultivation was carried out overnight in
conical flasks, containing sterile aqueous medium
with mannitol, yeast extract, and bactopeptone,
adjusted to an initial pH of 6.6 with NaOH aqueous
solution (1 mol L-1). To produce the BC mem-
branes, sterile medium with the same composition as
the sterilized pre-inoculum was inoculated with 10 %
of the pre-inoculum that was previously, vigorously
stirred to release cells from the cellulosic mass, and
added to a 24-well culture plate (TPP Techno Plastic
Products AG, Switzerland) and left for 3 days at
room temperature. At the end of the batch culture the
bacteria and their residues were removed with a
solution of 0.1 mol L-1 NaOH at 90 °C for 20 min
and thoroughly washed in distilled water until neutral
pH.
BC/PAni composite preparation
Bacterial cellulose/PAni nanocomposites were pre-
pared through the in situ aniline oxidative polymer-
ization by using iron (III) chloride hexahydrate
(FeCl36H2O) as oxidant. The reactions were per-
formed in the presence of HCl aqueous solution
(namely BC/PAni.HCl) or in the absence of mineral
acid (series BC/PAni.W). In the first series, BC
hydrogel membranes with diameter of 10 mm were
immersed in an HCl aqueous solution (0.5 mol L-1)
containing 0.1 mol L-1 of aniline. After 10 min under
magnetic stirring, an appropriate amount of FeCl3
aqueous solution was added and the polymerization
was carried out at 5 °C during different time intervals,
under magnetic stirring. Similar procedure was
employed for the reactions performed without the
addition of HCl. After polymerization the BC/PAni
membranes were thoroughly washed with HCl aque-
ous solution (0.1 mol L-1) in order to extract the
byproducts and residues of the reaction and vacuum
dried at room temperature. The thickness of the dried
conducting polymer composites was in the range of
0.01–0.02 mm.
For comparison, pure PAni samples were also
synthesized using a similar procedure. PAni samples
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obtained in the presence of HCl (PAni.HCl) and in
absence of HCl (PAni.W) as conducting powder were
filtered, washed with HCl aqueous solution
(0.1 mol L-1) and distilled water, respectively, and
dried at room temperature.
Physico–chemical and electrical characterization
The electrical conductivity of the membranes was
measured using the four-probe method by a Keithley
electrometer 6517A and a Keithley power source 6220.
The impregnation of the BC nanofibers with PAni
was evaluated through Fourier transform infrared
spectroscopy (FTIR) in a Shimadzu, model IR PRES-
TIGE-2, instrument with an ATR (attenuated total
reflectance) accessory and ZnSe crystal (ATR Smart
Performance module). The spectra of dried BC and
BC/PAni composites were recorded in the range of
4,000–700 cm-1 by accumulating 64 scans at a
resolution of 4 cm-1.
Thermogravimetric analysis (TGA) was performed
on a Q50 thermobalance from TA Instruments Inc.
The samples were heated from 30 to 700 °C, at a
heating rate of 20 °C/min, under nitrogen flow.
The PAni content in the composites was determined
using CHN Elemental Analyzer from PerkinElmer
2400 Series II with accuracy of ±0.3 %. The method
was based on the combustion of the BC, PAni and
composites in an oxygen atmosphere at 925 °C.
Tensile tests of BC membranes and BC/PAni
composites with thicknesses in the range 10–30 lm
were performed using a Dynamic mechanical analyzer
(Q-800, TA Scientific) equipped with clamp for films.
The tests were performed at room temperature and
speed of 3 mm min-1. The BC and composites were
kept under vacuum conditions before analysis. The
modulus of elasticity, tensile strength and elongation
at break were calculated from the stress–strain curves
considering at least six analyses of each sample.
X-ray diffraction (XRD) measurements were
obtained at room temperature using a Philips diffrac-
tometer model X0 Pert with CuKa radiation (k =
1.54 nm). Dried BC and composite membrane were
placed on an aluminum plate and measured over a 2h
interval of 5°–50° with steps of 1° min-1. The degree
of crystallinity (vc) of the cellulose membrane was
estimated from the diffractogram through the ratio
between the areas under the ð110Þ and (200) crystalline
peaks and the total area, according to the method
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1648 Cellulose (2012) 19:1645–1654

placed over an aluminum support and sputtered with

gold.

Results and discussion

The in situ polymerization of aniline in the presence of

BC hydrogel membranes was performed in water
solution (BC/PAni.W) or in HCl aqueous solution
(BC/PAni.HCl). During polymerization the BC mem-
branes turned from white to lightly green within 2 h of
reaction and after 6 h the membranes became com-
pletely green, indicating the coating of the BC
nanofibers by PAni. The effect of the oxidant/aniline
Fig. 1 Electrical conductivity of BC/PAni composites versus
FeCl3/Ani molar ratio

described by Watanabe and Tabuchi (1998). The

crystalline domain size (t) or the extent of order of the
polymers prepared in water and HCl was estimated
using the Scherrer’s equation:
0:9k
t¼ ð1Þ
W cos h
where k is the x-ray wavelength, W is the line
broadening at half the maximum intensity (FWHM)
in radians, and h is the Bragg angle. The ð1 10Þ
diffraction plane was used for the calculus of W.
The microstructure of the samples was evaluated by
Field-Emission Gun Scanning electron microscopy
(FEG-SEM, JEOL JSM-670F) operating at 15 kV and
80 A. For the observations, BC and composites
membranes with diameters of 5 mm were dried and

Fig. 3 FTIR spectra of BC; PAni and BC/PAni composites

Fig. 2 Electrical conductivity as function of reaction time prepared with 6 and 18 h reaction time

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Fig. 4 TG curves of BC;
PAni and BC/PAni
composites prepared with 6
and 18 h reaction time
(FeCl3/Ani) molar ratio on the electrical conductivity
of BC/PAni composites after 6 h of reaction is shown
in Fig. 1. In both systems, the electrical conductivity
increased as the FeCl3/Ani molar ratio increased,
reaching a plateau at a FeCl3/Ani ratio of 2, with
electrical conductivity values of around 3.5 9 10-2
and 5 9 10-1 S cm-1 for BC/PAni.W and BC/
PAni.HCl, respectively. For all FeCl3/Ani molar ratios
employed, the addition of HCl resulted in higher
values of conductivity, suggesting higher protonation
degree of PAni. Nevertheless, relatively high conduc-
tivities were obtained in systems obtained without the
presence of HCl. According Kelly et al. the reduction
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process of FeCl3 may provide enough HCl to promote
the formation of emeraldine (Kelly et al. 2007).
Moreover, for FeCl3/Ani molar ratio higher than 4,
BC/PAni samples could be handled but very brittle
when compared to the BC/PAni membranes obtained
by using FeCl3/Ani ratio of 2 or 1.3 for aniline
polymerization on BC nanofibers. According Bene-
venti et al. (2006), under aggressive polymerization
conditions cellulose can be subjected to acid hydro-
lysis and fiber degradation.
In order to obtain BC/PAni composites with higher
electrical conductivity at low FeCl3/Ani ratio, and
prevent cellulose degradation, the influence of the
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Table 1 TGA parameters

Code BC Reaction Onset Residue PAni contenta Electrical
of BC, PAni and their
(mm3) time (h) degradation (%) (%) conductivity
corresponding BC/PAni
temperature (S cm-1)
composites
(oC)

BC 1 – 276 2 – 1.7 9 10-13

PAni.HCl – 18 220 57 – 9.1 9 10-1
Pani.W – 18 218 61 – 7.4 9 10-2
BC/PAni.HCl 1 6 224 29 17.8 8,2 9 10-4
BC/PAni.HCl 1 18 240 28 38.8 8,9 9 10-1
BC/PAni.W 1 6 215 28 24.0 2.2 9 10-4
a
Calculated by CHN BC/PAni.W 1 18 214 40 42.5 5.5 9 10-2
analysis

Fig. 5 Tensile stress–strain curve of (a) air dried BC, (b) BC/
PAni.W (66/34) and (c) BC/PAni.HCl (49/51) (wt./wt.)
reaction time on the electrical conductivity was
investigated for samples prepared at FeCl3/Ani =
1.3/1 (Fig. 2). The electrical conductivity profiles are
characterized by a sharp initial increase after 5 h of
reaction, and tend to a plateau after 18 h. This
behavior is probably attributed to the high PAni yield
achieved at this time which allows the formation of
continuous conducting layers on the BC nanofiber
surface. These results reveal that the adequate reaction
time to prepare BC/PAni composites with higher
electrical conductivities at 0.1 mol L-1 aniline con-
centration and molar ratio (FeCl3/Ani) of 1.3/1 is
above 18 h.
Figure 3 shows the ATR-FTIR spectra of
PAni.HCl, PAni.W, BC and BC/PAni composites
prepared with aniline concentrations (0.1 mol L-1),
oxidant/aniline molar ratio (1.3/1) and reaction times
of 6 and 18 h. The characteristic broad band of
Fig. 6 X-ray diffraction patterns of pure cellulose membrane,
pure PAni polymerized in water and HCl and PAni/BC blends
synthesized in H2O and HCl for 18 h
cellulose O–H groups appears at 3,342 cm-1. The
bands 2,915 and 1,642 cm-1 are attributed to the
asymmetrically stretching vibration of C–H and the
O–H bending of the absorbed water, respectively. The
broad absorption band in the range of 1,060–
1,030 cm-1 is assigned to the vibration of the C–O
and C–O–C functional groups of the pyranose ring
skeletal (Grande et al. 2009). PAni exhibits an
absorption band at 1,556 cm-1 and 1,470 cm-1,
assigned to the stretching vibration of quinoid and
benzoid structure, respectively. The spectra of the BC/
PAni.HCl and BC/PAni.W composites produced with
6 and 18 h reaction time exhibited overlapped absorp-
tion bands of both components, except for the quinoid
and benzoid structure. Small peaks in transmittance at
around 1,556 and 1,470 cm-1 and the bending modes

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Cellulose (2012) 19:1645–1654 1651

Fig. 7 FEG-SEM micrographs of BC (a), BC/PAni.W and BC/PAni.HCl composite obtained with 0.1 mol L-1 aniline concentration
after: 6 h (b and c) and 18 h (d and e) reaction time, respectively

for OH groups of BC were observed for BC/PAni
composites obtained for 6 h reaction time, which
indicates that the BC was coated with PAni.HCl or
PAni-W. Otherwise, with increasing the reaction time
(18 h), the stretching vibration of quinoid and benzoid
structure of PAni is increased while the OH group
band is decreased. As expected, these results indicate
that the content of PAni in the coating layer was
enhanced with reaction time.
Thermogravimetric analysis was employed to
determine the thermal stability of BC/PAni samples
prepared by different procedures. Figure 4 compares
the TG profiles of the BC/PAni samples prepared with
different conditions. The main degradation parameters
are summarized in Table 1. The TG curves of the BC/
PAni composites display two main degradation stages.
The first one is related to the presence of moisture in
the samples. The second stage is attributed to the
decomposition of the amorphous BC region (Hu et al.
2011). The onset temperature of the thermo-degrada-
tion of BC/PAni is similar for all samples, as shown in
Table 1. However, the composites exhibited lower
onset degradation temperature than that of pure BC.
According to Hu et al. and Marins et al., this behavior

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Fig. 8 FEG-SEM micrographs of BC (a), BC/PAni.W (b) and BC/PAni.HCl (c) obtained with 0.1 mol L-1 aniline concentrations
after 18 h fracture surface
can be associated with the weakened intermolecular
hydrogen bonding of cellulose chains by the presence
of PAni (Hu et al. 2011; Marins et al. 2011).
The amount of PAni in the composites was
determined by CHN analysis and the results are also
presented in Table 1. The composite prepared without
the addition of HCl (BC/PAni.W) presented higher
incorporation of PAni on BC surfaces than those
found for BC/PAni.HCl composites. However, the
electrical conductivity values of BC/PAni.W com-
posites were not higher, which indicates that the lower
protonation degree of PAni.W should be the cause for
the lower conductivity.
Figure 5 shows the stress–strain curves for BC and
BC/PAni composites. BC sheets and their composites
show typical brittle behavior material, i.e., all samples
exhibit elongation at break lower than 1.9 %. The
tensile strength and Young0 s Modulus of pure BC are
about 64 MPa and 4.8 GPa, respectively. For BC/
PAni.W or BC/PAni.HCl, the tensile strength values
were 48 and 41 MPa, respectively, which are 25 and
36 % lower than the values for the pure BC. Moreover,
the Young0 s modulus of composites were approxi-
mately 2.5 GPa, which are 48 % lower than BC. These
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Cellulose (2012) 19:1645–1654
results suggest that PAni is formed on BC nanofibers,
reducing inter and intramolecular hydrogen bonding
of BC nanofibers.
Figure 6 shows the X-ray diffraction spectra of
PAni, BC and composites produced in water and in
HCl. Diffraction patterns of PAni produced in H2O
and HCl exhibit two broad peaks around 20° and 26°,
which are peaks assigned to PAni (Yun and Kim 2006;
Raghavendra et al. 2003). XRD-spectrum of cellulose
reveals its nanocrystalline nature, characterized by
two main diffraction planes ð110Þ and (200) typical of
cellulose I (Watanabe and Tabuchi 1998; Czaja et al.
2006). The estimated crystallite size of the pure
cellulose membrane is 7.4 nm, in accordance with
Watanabe and Tabuchi (1998). The estimated degree
of crystallinity of the cellulose membranes is
55 ± 5 %. The produced blends exhibit a semi-
crystalline nature. Two main peaks can be identified
in the spectra of BC/PAni blends prepared in water and
HCl, which are assigned to the ð110Þ and (200)
diffraction planes of cellulose, with a superposing halo
from PAni. The crystallite size of the blend was
6.1 nm and the blend prepared in H2O exhibits
crystallite size of 7.7 nm, which suggests that
Cellulose (2012) 19:1645–1654
polymerization of PAni in HCl caused a decrease on
the extent of order of cellulose, probably due to a weak
acidic degradation rather than a direct effect of PAni.
The FEG-SEM micrographs of a dried BC and BC/
PAni composite surfaces are shown in Fig. 7. The BC
membrane was formed by a network structure of long
cellulose nanofibers with high aspect ratio (Fig. 7a) as
described in Müller et al. (2011). In both BC/PAni
composites the presence of PAni particles entangled
with cellulose nanofibers can be observed (Fig. 7c–f).
A more detailed morphological analysis of BC/PAni
composites produced with 0.1 mol L-1 after 18 h
reaction time is shown in high magnification FEG-
SEM micrographs of Fig. 8. The micrographs
revealed that PAni was constituted of particles with
mean size of 10 nm merged together to form a uniform
layer that completely coated the nanofiber surface.
The polymer coating adhered to the nanofiber and a
continuous conducting network was formed which
was responsible for the high electrical conductivity
values. For BC/PAni composites the mean diameter
was 100 nm, which is approximately 2-fold higher
than the values for the uncoated cellulose nanofibers.
Conclusion
Flexible and conducting nanofibrous membranes com-
posed of BC and PAni were obtained through in situ
oxidative chemical polymerization of aniline in the
presence of BC membranes by using FeCl36H2O as
the oxidant. The electrical conductivity of the com-
posite was dependent on the oxidant concentration and
reaction time. BC/PAni.HCl composites prepared with
HCl solution exhibited higher electrical conductivity
but lower tensile strength than BC/PAni.W. Neverthe-
less, relatively high conductivity was achieved in
systems obtained in absence of HCl. The BC/PAni
micrographs revealed that the conducting nanofiber
material was constituted of a continuous conducting
material distributed uniformly on the BC nanofiber
surface. The method described in this article reveals
that FeCl3 is a promising candidate as oxidant for
preparing BC/PAni composites with good mechanical
properties and electrical conductivity values higher or
similar than those found for BC/PAni composites
obtained by using APS and protonic acids. These
materials may exploit BC properties, which include
good tensile strength, toughness, biocompatibility, and
1653
high surface area with electrical, optical and magnetic
properties of PAni.
Acknowledgments The authors gratefully acknowledge the
financial support by Conselho Nacional de Desenvolvimento
Cientı́fico e Tecnológico—CNPq, Coordenação de
Aperfeiçoamento de Pessoal de Ensino Superior—CAPES,
and Fundação de Amparo à Pesquisa e Inovação do Estado de
Santa Catarina—FAPESC. We are sincerely thankful to Central
Electronic Microscopy Laboratory, Santa Catarina Federal
University (LCME-UFSC).
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