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Duy Et Al., 2021 - Fuel Cell
Duy Et Al., 2021 - Fuel Cell
Duy Et Al., 2021 - Fuel Cell
Fuel
journal homepage: www.elsevier.com/locate/fuel
A R T I C L E I N F O A B S T R A C T
Keywords: The electrical conducting bacterial cellulose/polyaniline (BC/PANI) based composites were synthesized over in
Bacterial cellulose/polyaniline/titanium- situ polymerization of aniline onto BC with ammonium-persulphate (APS) and chloride hexahydrate of iron (III)
dioxide as oxidant (FeCl3⋅6H2O). The conductivity of synthesized BC was improved in the presence of a titanium-dioxide
Shewanella xiamenensis
(TiO2) coating. The conductivity of BC/PANI/TiO2/APS was 3.7 S/m compare 2.9 S/m and 2.67 S/m with BC/
Microbial fuel cells
Hydrogel bioanode
PANI/TiO2/FeCl3⋅6H2O and BC/PANI/APS, respectively. Moreover, when using the BC/PANI/TiO2/APS as
Immobilization anode with the immobilization of Shewanella xiamenensis, an improved efficiency of microbial fuel cell was
observed. The power-density maximized 38.89 W/m3 with BC/PANI/TiO2/APS anode compared with 2.57 W/
m3 in the case of bare BC anode. These results will serve as a good base for the development of compact microbial
fuel cell with high power density.
1. Introduction integral parts because of their key electron transfer role and research
leading to enhanced efficiency of MFC [14] is worthwhile. Electrode
In recent years, alternative renewable energy systems have elicited materials should have good electrical conductivity, biocompatibility,
great interest. Microbial fuel cell (MFC) can convert organic (biological) chemical stability, large surface area and mechanical strength [15–17].
matter directly into energy [1–4], thus they are classified as renewable Carbon materials with their high electric conductivity and stability are
energy systems [5–6]. In MFC, microorganisms biocatalyze the oxida usually used in anode fabrication. Besides carbon materials, other ma
tion of organic matter and release electrons into the anodic electrode. terials have been studied and used as anode materials in MFC [18].
Then, these electrons are transported to the cathodic electrode via the Cellulose is a well-known non-toxic and low-cost polymer. It is also a
external circuit, resulting in a current generated. The organic com naturally biocompatible polymer and has been used in many fields
pounds play a primary role as an electron source in microbial processes [19–20]. Bacterial cellulose (BC) produced by fermentation of Aceto
[7–10]. Many factors affect MFC performance such as microorganisms, bacter under static or agitated conditions and it is also classed as an
substrate, mediator, electrode material etc. [11–13]. Electrodes are exopolysaccharide. It has some outstanding characteristics compared to
* Corresponding authors.
E-mail addresses: vijaifzd@gmail.com (V.K. Gupta), Nguyen.Duc.Quang@szie.hu (Q.D. Nguyen).
https://doi.org/10.1016/j.fuel.2020.119259
Received 31 May 2020; Received in revised form 13 August 2020; Accepted 13 September 2020
Available online 5 October 2020
0016-2361/© 2020 Elsevier Ltd. All rights reserved.
D.H. Truong et al. Fuel 285 (2021) 119259
Fig. 1. Schematic construction of dual-chamber MFC using BC, BC/PANI, BC/PANI/TiO2 composites as anode.
plant cellulose such as ultrafine network structure, higher purity, water 2. Materials and methods
retention capability, porosity, biological interaction and mechanical
strength [21–23]. Chemically, BC is linear polysaccharide chains having 2.1. Microbial culture conditions
glucose units linked together by β(1,4) glycosidic bonds, and intermo
lecularly by hydrogen bonds. Acetobacter bacteria is considered as a Shewanella xiamenensis DSMZ 2215 strain was obtained and main
strictly aerobic model bacteria species with high BC production capacity tained accordingly to Szöllősi et al. [6]. The bacterial cells from 24 h
[24] and hydrogel cellulose will be formatted on the top surface of the cultures in Luria-Bertani (LB) medium at 180 rpm were separated by
liquid culture [25]. centrifuge 10,000 rpm and used for immobilization.
In recent years, conducting polymer-cellulose composites received
significant interest due to high potentials in industrial applications,
2.2. Preparation of BC hydrogel
including as batteries, sensors and electrical devices. Polyaniline (PANI)
has played a great role in energy storage, due to its controllable elec
Acetobacter xylinum ATCC 23768 strain was used for bacterial cel
trical conductivity, facile synthesis and availability as a low-cost mate
lulose production. Bacteria were cultivated on Schramm-Hestrin (SH)
rial [26]. Besides other types of scaffolds based on cellulose (e.g. plant
medium [32]. A single Acetobacter xylinum colony on SH agar medium
cellulose, cellulose derivatives and microcrystalline cellulose), bacterial
was transferred into liquid SH medium. The cellulose sheets were sha
cellulose membrane is an attractive cellulose scaffold for the preparation
ped on the top-surface of the culture broth after 7 days at 28 ◦ C. The
of conducting polymer-cellulose [23]. BC coated with conducting
cellulose sheets with 0.5 cm thickness were removed and washed with
polymers is now well known as a new promising polymer [27]. BC/PANI
deionized water, sodium dodecyl sulphate 2% and purified in NaOH 0.1
is a typical example for BC combination and conducting polymer with
N [33]. They were cut into 2 × 3 cm pieces and sterilized before they
the integration of several properties such as tensile strength, biocom
were used for the fabrication of electrically conducting composites and
patibility, high surface areas and electrical conductivity [27–28]. In
cell immobilization.
addition, Wang et al. [23] have fabricated BC/PANI material with high
electrical conductivity. In many types of research, the PANI coated
anode was successfully used in the MFC to enhance power density 2.3. Development of electrically conducting BC/PANI, BC/PANI/TiO2
[16,29–30]. Furthermore, the modification of PANI polymers with the and bare BC composites
supplement of titanium dioxide have significantly enhanced the current
densities of MFC [31]. BC/PANI composites were made in situ by oxidative polymerization
The main focus of the present study is in situ fabrication of electri of aniline using ammonium persulphate (APS) called BC/PANI/APS or
cally conducting bacterial cellulose/polyaniline/titanium-dioxide com iron (III) chloride hexahydrate (FeCl3⋅6H2O) called BC/PANI/
posites with the immobilization of Shewanella xiamenensis and its FeCl3⋅6H2O as oxidant. For the preparation of BC/PANI composites, BC
electrical performance in the microbial fuel cell. hydrogel membranes with 2 × 3 × 0.5 cm were cut and immersed in
distilled water (1:10 w/v) and then aniline (Merck, Hungary) were
2
D.H. Truong et al. Fuel 285 (2021) 119259
Fig. 2. Effect of reaction conditions (aniline concentration and ammonium persulfate, FeCl3⋅6H2O) on the conductivity of BC/PANI composites: (a) BC/PANI/APS;
(b) BC/PANI/FeCl3⋅6H2O.
added. In the first ultra-sonification process, the Clifton MU-8 sonicator Pd = P/d, where d is the volume of bare BC or synthesized BC.
at 40 kHz and 30 W performance was used for 2 h; hydrogen bonding
was formed allowing the monomer to assemble onto the BC surface. In 2.6. Bare BC, BC/PANI and BC/PANI/TiO2 characterization
the next step, the oxidant (ammonium-persulphate, Reanal, Hungary) or
iron (III) chloride hexahydrate) was mixed. The BC was synthesized in 2.6.1. Conductivity measurements
the 2nd ultra-sonication (40 kHz, 30 W) condition for 2 h in the ice. After BC/PANI, BC/PANI/TiO2 conductivity was analyzed with four-point
polymerization was started the colour of the solution changed to dark probe technique. According to the four-point method, electrical resis
green from ivory in an overnight reaction. In the case of fabrication of tance and electrical current were measured by a digital multimeter VC-
electrically conducting BC/PANI/TiO2 composites, TiO2 (Sigma 830 (Voltcraft, Germany).
Aldrich) was mixed simultaneously with oxidants. For comparison, bare
BC without aniline oxidative polymerization was used. 2.6.2. FT-IR
The infrared spectra of newly fabricated bare BC, BC/PANI and BC/
2.4. Immobilization of Shewanella xiamenensis into bare BC, BC/PANI PANI/TiO2 composites were obtained on a JASCO-4700 infrared spec
and BC/PANI/TiO2 using adsorption method trometer using KBr pellets with a wavelength range of 4000 to 400 cm− 1.
The Shewanella xiamenensis cells in LB broth medium after 24 h at 2.6.3. Scanning electron microscope
30 ◦ C in incubator shaker 180 rpm were separated using the centrifugal Scanning electron microscope (SEM, JSM-6480LV-JED 2300, Jeol,
method and suspended in isotonic saline phosphate-buffer (PBS, Sigma- Japan) was used to analyze the structure of the surface of bare BC, BC/
Aldrich) to get cell number of 109 CFU/ml. Bare BC, BC/PANI and BC/ PANI and BC/PANI/TiO2.
PANI/TiO2 composite membranes were incubated in Shewanella xiame
nensis suspension at 30 ◦ C with shaking at 200 rpm from 12 to 96 h. After 2.6.4. Electrochemical measurements
that, composite membranes were washed 3 times with PBS to remove Electrochemical characterization of bare BC and BC/PANI was per
free cells. formed by cyclic voltammetry (CV) techniques. Cyclic voltammetry
(CV) was conducted using the open-source potentiostat (IO Rodeo, USA)
2.5. Construction batch and semi-continuous batch of MFC with saturated calomel electrode (SCE) and platinum wire.
Dual-chamber MFC was prepared with a similar volume of anode and 2.6.5. Cell number determination of immobilized Shewanella xiamenensis
cathode chamber (24 mL) and a Nafion 117 proton-exchange membrane The cell number of immobilized Shewanella xiamenensis in bare BC,
was applied for separation of two chambers. The cathode chamber was BC/PANI and BC/PANI/TiO2 were determined by plate count method on
filled with solution of 0.5 M of Sorensen phosphate buffer (pH = 7) Marine agar (Scharlau, Spain). After immobilization of Shewanella xia
contained 0.1 M of potassium-hexaferrocyanate. Bare BC, BC/PANI and menensis cell, bare BC and synthesized BC were washed 3 times with PBS
BC/PANI/TiO2 with immobilized bacteria cells act as an anode electrode and digested with the cellulase enzyme (Sigma, Aldrich). The grown
and anode chamber was filled with modified LB medium that contains 1 colonies were counted after incubation for 24 h, and the number of
g/L glucose without agar. Graphite sheets with surface area 6 cm2 as colonies was determined.
cathode were placed in the respective chambers. Generally, the external
resistance with capacity of 500 Ω in parallel with a digital multimeter 3. Results and discussions
was used to connect the electrodes (Fig. 1). Both batch and semi-
continuous operation modes used for investigation of electric perfor 3.1. Fabrication of electrically conducting composites from bacterial
mance of MFC. cellulose
The voltage was continuously measured in the external resistance
(500 Ω). The Ohm’s law (I = V/R) was used to calculate the current (I) in The BC/PANI electrical conductivity composites were strongly
MFC based on the electric voltage (V) and the external resistance (R). dependent upon reaction conditions. The effect of preparation condi
While the current density (P) of MFC was calculated according to tions (aniline, FeCl3⋅6H2O and ammonium persulfate concentration) on
equation P = I.V, whereas the power density (Pd) was obtained based on the BC/PANI nanocomposites conductivity was investigated using the
3
D.H. Truong et al. Fuel 285 (2021) 119259
Fig. 3. Effect of titanium dioxide concentration in fabrication of BC/PANI/TiO2 composites process on its conductivity: (a) BC/PANI/APS; (b) BC/PANI/FeCl3⋅6H2O.
Fig. 4. FT-IR spectra of bare BC, BC/PANI and BC/PANI/TiO2 using ammonium persulfate as oxidant.
Central Composite Design (CCD) of response surface method (Fig. 2). composite, the stretching vibration of quinoid and benzenoid rings
The BC/PANI electrical conductivity increased when the aniline, structure was at peaks 1556 and 1470 cm− 1, respectively. C-O-C
FeCl3⋅6H2O and ammonium persulfate concentration increased. The stretching vibrations of the pyranose skeletal ring were at the range of
maximum BC/PANI composites conductivity could be attained when 1060–1030 cm− 1 [23]. The FT-IR spectra of BC/PANI/TiO2 composite
prepared as follows: concentration of aniline 0.2 mol/L; molar ratio of showed an absorption band at 637 cm− 1. This feature supports our
ammonium-persulfate:aniline 1.2:1; molar ratio of FeCl3⋅6H2O:aniline claims that an interaction between TiO2 and the hydroxyl group of
1.5:1; reaction temperature 0–5 ◦ C; polymerization reaction time 14 h cellulose occurred [37] and that the BC was sufficiently coated by PANI
for the completion of polymerization. The conductivity of BC/PANI/APS and TiO2.
composites obtained was 2.67 S/m and with BC/PANI/FeCl3⋅6H2O The surface characteristics of bare BC, BC/PANI and BC/PANI/TiO2
composites 2.29 S/m. were evaluated by SEM images at x1000 magnification (Fig. 5). The
Fig. 3 illustrates the effect of TiO2 concentration on the conductivity morphologies are particularly different between bare BC and BC/PANI.
of BC/PANI/TiO2 composites. The maximum conductivity of BC/PANI/ In the case of bare BC, a smooth surface with featureless morphology
APS was 3.7 S/m when prepared at 0.3 mol/L TiO2 concentration and was observed (Fig. 5a). In comparison, the surface of BC/PANI was
for BC/PANI/FeCl3⋅6H2O was 2.9 S/m with 0.2 mol/L TiO2. rough and covered with materials (Fig. 5b–d). The surface structure of
Infrared spectra of bare BC and synthesized BC composites were BC/PANI/TiO2 showed the particles entangled with cellulose and PANI
measured by FT-IR to evaluate chemical structure (Fig. 4) The FT-IR particles, present a much denser structure (Fig. 5c, d). This result
spectrum of pure BC presented broad absorption band of 3200–3550 showed that the BC coating adhered to the cellulose and formed a
cm− 1, assigned H-bond for –OH [23,34–36]. The peak at 2895 cm− 1 continuous conducting network for the high electrical conductivity
showed the aliphatic C–H stretching vibration. In the case of BC/PANI [23,38–39].
4
D.H. Truong et al. Fuel 285 (2021) 119259
Fig. 5. SEM images of (a) Bare BC, (b) BC/PANI/APS, (c) BC/PANI/TiO2/APS, (d) BC/PANI/TiO2/FeCl3⋅6H2O.
5
D.H. Truong et al. Fuel 285 (2021) 119259
Fig. 8. The power density of MFC with BC/PANI/TiO2/APS anode composite in semi-continuous batch (“↓” indicate the new feeding cycle).
Table 1
The power density of different polyaniline modified anode materials in the MFC.
Anode material MFC contruction Bacteria Substrate Pmax (W/m3) References
illustrated in Fig. 7.
The power density rapidly increased in MFC with BC/PANI/TiO2
anode (MFC4 and MFC5) compared with the control system bare BC
(MFC1). The power density of MFC5 reached the maximum value
(38.89 W/m3) after 8 h of operation and maintained this power density
for 28 h. The power density of MFC5 was 15-fold higher than MFC1 with
bare BC anode (2.57 W/m3). MFC1 reached a maximum value (7.09 W/
m3) after 16 h of operation. In the case of BC/PANI/TiO2 (MFC4) using
FeCl3⋅6H2O as an oxidant – the power density value peaked around
23.95–29.30 W/m3, lower than MFC5. MFC2 and MFC3 also showed
lower power density values in comparison with MFC4 and MFC5. The
combination of BC/PANI and TiO2 contributed to the increase in power
density. Taşkan et al. [40] used a Ti-TiO2 electrode to enhance the
electricity generation in MFC and their research showed that the current
density achieved 15-fold higher than the carbon-based electrode. Also,
in 2013, Wu et al. [41] successfully fabricated the carbon nanotube-
gold-titanium-dioxide (CNT/Au/TiO2) that has nanostructure, and it Fig. 9. Polarization curve of MFC with BC/PANI/TiO2/APS anode composite.
was applied as modified anode in the MFC. They reported that the power
density was 3-fold higher than the bare carbon paper electrode. Indeed, densities by 300% and 180% for abiotic cathodes and biocathodes,
due to the number of technological and economical advantages such as respectively, compared to unmodified carbon felts electrodes.
large surface area, low cost and high conductivity, the conducting To consider the effectiveness of BC/PANI/TiO2/APS with immobi
polymers can serve very good materials for formation of anodic elec lization of Shewanella xiamenensis, semi-continuous batch was set-up
trode in MFC. For example, Szöllősi et al. [6] successfully fabricated an after voltage output of MFC5 decreased. The anode chamber of MFC5
alginate/PANI/TiO2/graphite composite for MFC application and they was fed with fresh substrate and the performance is shown in Fig. 8.
reported that the MFC with this anode had significantly high electrical Maximum power density of each cycle peaked around 35.81 W/m3 after
conductivity and power density as well as exhibited good stability. Li 30 hours. In this result, MFC still retains the ability to produce electricity
et al. [42] also used modified carbon felt electrodes with four classes of if the nutritional medium is met. The cycle time of MFC takes about
conducting polymers, namely polyaniline, poly(aniline-co- 70–72 h from the fresh feeding medium to exhaustion of glucose. Several
aminophenol), poly(aniline-co-2,4-diaminophenol) and poly(aniline- authors also reported the increase in power density of MFC using
1,8 diaminonaphthalene) . Their method enhanced the power modified anode with supplement of polyaniline (Table 1). Additionally,
6
D.H. Truong et al. Fuel 285 (2021) 119259
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