development and application of vanadium oxide/polyaniline composite as a novel cathode catalyst in...

Development and application of vanadium oxide/polyaniline composite as a novel cathode catalystin microbial fuel cellKhadijeh Beigom Ghoreishi1, Mostafa Ghasemi2,3,**,†, Mostafa Rahimnejad4,*,†,Mohd Ambar Yarmo1, Wan Ramli Wan Daud2,3, Nilofar Asim5, Manal Ismail2,3

1School of Chemistry, Faculty of Science and Technology, University Kebangsaan Malaysia (UKM), 43600 Bangi, Selangor DarulEhsan, Malaysia2Fuel Cell Institute, University Kebangsaan Malaysia (UKM), 43600 Bangi, Selangor Darul Ehsan, Malaysia3Department of Chemical and Process Engineering, Faculty of Engineering and Built Environment, University Kebangsaan Malaysia (UKM),43600 Bangi, Selangor Darul Ehsan, Malaysia4Biotechnology Research Lab., Faculty of Chemical Engineering, Babol Noshirvani University of Technology, Babol, Iran5Solar Energy Research Institute (SERI), University Kebangsaan Malaysia (UKM), 43600 Bangi, Selangor Darul Ehsan, Malaysia

SUMMARY

Polyaniline (Pani), vanadium oxide (V2O5), and Pani/V2O5 nanocomposite were fabricated and applied as a cathode catalyst inMicrobial Fuel Cell (MFC) as an alternative to Pt (Platinum), which is a commonly used expensive cathode catalyst. The cathodecatalysts were characterized using Cyclic Voltammetry and Linear Sweep Voltammetry to determine their oxygen reductionactivity; furthermore, their structures were observed by X-ray Diffraction, X-ray Photoelectron Spectroscopy, Brunauer–Emmett–Teller, and Field-Emission Scanning Electron Microscopy. The results showed that Pani/V2O5 produced a powerdensity of 79.26 mW/m2, which is higher than V2O5 by 65.31 mW/m2 and Pani by 42.4 mW/m2. Furthermore, the CoulombicEfficiency of the system using Pani/V2O5 (16%) was higher than V2O5 and Pani by 9.2 and 5.5%, respectively. Pani–V2O5 alsoproduced approximately 10%more power than Pt, the best and most common cathode catalyst. It declares that Pani–V2O5 can bea suitable alternative for application in a MFC system. Copyright © 2013 John Wiley & Sons, Ltd.

KEY WORDS

cathode; catalyst; microbial fuel cell; nanocomposite; Pani/V2O5

Correspondence

*Mostafa Rahimnejad, Biotechnology Research Lab., Faculty of Chemical Engineering, Noshirvani University, Babol, Iran.†E-mail: [email protected]**Mostafa Ghasemi, Department of Chemical and Process Engineering, Faculty of Engineering and Built Environment,University Kebangsaan Malaysia (UKM), 43600 Bangi, Selangor Darul Ehsan, Malaysia.†E-mail: [email protected]

Received 10 December 2012; Revised 5 June 2013; Accepted 8 June 2013

1. INTRODUCTION

Global energy shortages and environmental pollution haveled to a crisis affecting human survival and development.There has been a recent increase in the amount of researchfocused on the use of waste materials as an inexpensiveand abundant source of renewable energy [1]. This greatconcern has caused the advancement of Microbial FuelCell (MFC). MFC is a type of fuel cell that uses bacteriaas a biocatalyst, to oxidize organic and inorganic matterto produce electricity [2,3]. MFC is able to simultaneouslyproduce electricity and treat wastewater. A typical MFCconsists of two chambers (anode and cathode) that areseparated by a Proton Exchange Membrane (PEM) [4].

The performance of an MFC is dependent on severalfactors, including the microorganism used as a biocatalyst,the cathode catalyst, the distance between the cathode andthe anode, the type of PEM used, etc. [5,6]. However, themain problem that limits the practical application of MFCis the high cost of Pt, which is used as a cathode catalyst.Therefore, finding or developing an alternative catalyst toPt is necessary to make MFC more practical [7]. Thestructure of the supporting materials can also affect theperformance of the oxygen reduction reaction (ORR) aswell as the catalyst. Vanadium is one of the most abundantmetals on Earth (widely distributed within the Earth’scrust) [8]. Both the pure and composite forms of vanadiumare used in many chemical reactions as a catalyst to obtain

INTERNATIONAL JOURNAL OF ENERGY RESEARCHInt. J. Energy Res. 2014; 38:70–77

Published online 23 July 2013 in Wiley Online Library (wileyonlinelibrary.com). DOI: 10.1002/er.3082

Copyright © 2013 John Wiley & Sons, Ltd.70

promising yields and reduce environmental problems [9].Vanadium has a wide range of applications, including steeladditives, batteries, catalysts, etc. [10,11]. Vanadium’sactive sites have an important role in its catalytic activity.However, their nature is still not fully understood[12–14]. There are different types of vanadium oxides,which are composed of single and mixed valence states,as well as different structures [15]. However, their compo-sitional stability, phase co-existence, and transformation todifferent states of vanadium multivalent vanadium are stillunclear [16–18]. Meanwhile, interest in the developmentof conducting polymers as nanocomposites has dramati-cally increased. This is due to their attractive properties,such as physical and chemical stability, high conductivity,biocompatibility, etc. [19]. Conducting polymer/metalnanocomposites show higher conductivity and stability,compared to polymers, which exhibit limited conductivityand lower stability in ultraviolet irradiation, heat, andother environmental conditions. Furthermore, metalnanoparticle-conducting polymer composites offerappropriate catalysis properties, with a high selectivityin chemical reactions, as the polymer effectively influ-ences controlling the surrounding metal [16]. Polyaniline(Pani)-supported Pd nanoparticles have been applied inthe oxidation coupling of the 2, 6-di-t-butyl phenol [17].Pt/Pani and PtO2/Pani have been used for the selectivehydrogenation of α, β-unsaturated aldehyde citral. PtO2/Paniproduced a highly dispersed supported catalyst, which wasable to hydrogenate the C=C bond of citral, whereasPani-supported Pt exhibited more selectivity to the reductionof the carbonyl groups [18]. The catalytic activity ofPani-supported cobalt has been examined in trans-stilbeneoxidation. The nanocomposite catalyst indicates a signifi-cant improvement in the reaction yield under mild condi-tions [20–23]. In a recent study, Qiao et al. synthesizedCarbon Nano Tube/Pani nanocomposite for use as anelectrode within an MFC system. They found that theperformance of the composite was superior to that of neatPani and the composite was able to produce more powerthan Pani [24]. In this research, we synthesized Pani andPani/V2O5 nanocomposite catalysts using micelle techniqueand investigated their application in the MFC, to seewhether the composite could be used as a cathode catalystin MFC. Moreover, these results were compared to theperformance of Pt, as it is the most commonly used cathodecatalyst in MFCs.

2. MATERIALS AND METHOD

2.1. Synthesis of V2O5 nanocomposite usinga micelle solution

V2O5 nanoparticles were synthesized using a Cetyltrimethyl ammonium bromide (CTAB) as a surfactantand micelle solution. For a typical preparation, 75 ml of0.05 M CTAB solution was mixed with 10 ml of 0.15 MNaOH and 1.2 mmol of vanadyl sulphate hydrate

(VOSO4. xH2O), then stirred at room temperature for2 h, followed by aging at an ambient temperature for48 h to allow precipitation. Next, the solution waswashed several times with deionized water and absoluteethanol to remove the surfactant, residual reactants, andby-products. The precipitate was then dried in a furnaceat 70 °C for 5 h and calcined at 400 °C for 2 h [25].

2.2. Synthesis of Pani using a micellesolution

For the preparation of pure Pani, 1.5 mmol of aniline wasadded to 75 ml of 0.05 M CTAB solution and mixedvigorously. Next, 3.7 � 10�5 mol of ammoniumperoxydisulfate (NH4)2S2O8, was added as an initiatorand mixed constantly for 2 min. This solution was thenfiltered and washed with deionized water and absoluteethanol to extract any oligomers or reactants. The resultingpowder was then dried in oven at 70 °C for 5 h [26].

2.3. Preparation of the Pani/V2O5

nanocomposite using a micelle solution

The nanocomposite was synthesized via a micelle solutionmethod using a hexadecyltrimethyl ammonium bromide(CTAB) cationic surfactant. First, the sample, including75 ml of the 0.05 M CTAB solution, was prepared.Then, a 10 ml solution of 0.15M NaOH was added andmixed thoroughly; 6 mmol of aniline was added to thesolution; then 1.2 mmol of vanadyl sulphate hydratewas added to the mixed solution and agitated for 90 min atroom temperature; it was then allowed to stand for 40 min.Next, 1.5 � 10�4 mol of ammonium peroxydisulfate(NH4)2S2O8, was added and mixed vigorously for 2 min.The mixed micelle solution was kept at room temperaturefor 48 h. A precipitated fine powder was then obtainedby centrifugation, which was then washed several timeswith absolute ethanol and distilled water to remove theresidual surfactant, unreacted aniline monomer, andby-products. All the products were then oven-dried for36 h at 65 °C [27].

2.4. MFC configuration

Two cylindrical and H-shaped chambers were constructedfrom Plexiglas, with an inner diameter of 6.2 cm and alength of 14 cm, separated with Nafion 117, which actedas a PEM. Oxygen was continuously fed to the cathodeusing an air pump (80 ml/min). Both the cathode’s andthe anode’s surface areas were 12 cm2 and the MFCoperated in an ambient temperature and at a neutral pH(6.5–7) within the anode and cathode’s compartments.The pH was adjusted using a phosphate buffer solution.Plain carbon paper (Gas Hub, Singapore) was used as an‘untreated’ anode. The cathode consisted of carbon papercoated with 0.5 mg/cm2 Pt [28].

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71Int. J. Energy Res. 2014; 38:70–77 © 2013 John Wiley & Sons, Ltd.DOI: 10.1002/er

2.5. Calculation and analysis

The current and the power produced by the system weremeasured using Formulas 1 and 2, respectively:

I ¼ V

R(1)

P ¼ V � I (2)

Where I represents the current (ampere), V is thevoltage (volt), R is the resistance (ohm), and P is the powerin watts.

The Coulombic Efficiency (CE) was calculated byintegrating the current over time, relative to the time atwhich the maximum theoretical current was achieved.The evaluated CE over time was calculated usingFormula 3.

CE ¼M ∫

t

0

I dt

FbVanΔCOD(3)

Where M is the molecular weight of oxygen (32), F isFaraday’s constant, b = 4 indicates the number ofelectrons exchanged per mole of oxygen, Van is thevolume of the liquid in the anode compartment, andΔ COD is the change in Chemical Oxygen Demand(COD) over time (t) [29].

A Potentiostat–Galvanostat (HAK-MILIK FRIM 04699A-2007) was used to test the oxidation and reduction oforganic compounds using microorganisms as a biocatalyst.The potential range was between �0.3 and 0.75 V. Theworking electrode, for the attachment of microorganisms,was made of Carbon Paper, and the reference electrodewas Ag/AgCl. Pt was applied as a counter electrode. Thescan rate was adjusted to 50 mV/s [30].

2.6. Catalyst characterization

The infrared (IR) spectra were recorded at room tempera-ture in KBr pellets, using a Perkin Elmer Paragon 2000FTIR spectrometer, under atmospheric conditions. Thephase structures of the catalysts were determined fromX-ray Diffraction (XRD) patterns, using a Bruker AXSD8 Advance X-ray Powder Diffractometer, with Cu Kα(λ = 0.15406 nm) at the angles 2θ= 10–60. The surfacearea of the catalyst was measured using the Brunauer–Emmett–Teller (BET) method (N2 adsorption) with aGemini apparatus (Micromeritics 2010 Instrument Corpo-ration). The morphology and microstructure data for thesamples were obtained from Field-Emission ScanningElectron Microscopy (FESEM) using a LEO 1450VP,equipped with an Energy Dispersive X-ray detector. Allsamples were analysed in a high vacuum at 20 kV. X-rayPhotoelectron Spectroscopy (XPS) were acquired using aKratos (XSAM HS) spectrometer, equipped with a hemi-spherical electron analyser and Mg Kα (hv 12536 eV,1eV= 1.6302 � 10�19 J) 120 W X-ray source. Thesamples were analysed at 3 � 10�9 mbar, using C1s line

at 284.5 eV using adventitious carbon as a reference forthe binding energies.

3. RESULT AND DISCUSSION

3.1. FTIR analysis

Figure 1 depicts the FTIR spectra of V2O5 nanoparticles,pure Pani, and Pani/V2O5 nanocomposite. The strongbands in the region of 750–1800 cm�1 are characteristicof Pani. Their position and intensity show that the conduc-tive form of the polymer has been produced. Thesenanocomposite bands exhibit a slight shift compared toPani, suggesting an interaction of the polymer with V2O5

in the nanocomposite. Pure Pani and nanocomposite showthe same peaks, at approximately 1460–1490 cm�1 and1590–1640 cm�1, which are assigned to benzenoid andquinoide ring in the polymer, respectively. The peak, at1200–1300 cm�1, corresponds to the C–N stretching ofthe secondary aromatic amine present in Pani [21,22]. Inthe case of the V2O5 nanoparticle, the strong band ob-served below 1000 cm�1 is related to the V=O stretching,which is overlapped by the plane bending vibration modeof C–H in the composite. The peaks at approximately500 and 800 cm�1 revealed the V–O–V symmetric andasymmetric stretching modes, respectively, which showthat both modes shift to higher wave numbers upon inter-action with Pani. The data suggest a highly interactingPani/V2O5 composite system, in which the coordinationenvironment at the metal centre is affected by interactionwith the organic conducting component [31].

3.2. XRD analysis

The XRD results are shown in Figure 2. These patterns re-veal that the synthesized vanadium pentoxide crystallizedinto an orthorhombic lattice form. The effect of addingV2O5 to the Pani and its composite were analysed usingthe same XRD technique. This pattern also shows partialcrystallinity in the synthesized nanocomposite. As reportedin most literature, most forms of Pani are essentially amor-phous and show the presence of a broad high-angle asym-metric scattering peak, stretching from 2θ values between 15

40060080010001200140016001800

Wavenumber (cm-1)

a

b

c

Figure 1. FTIR spectrum for a) V2O5 nanoparticle, b) Pani, and c)Pani/V2O5.

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72 Int. J. Energy Res. 2014; 38:70–77 © 2013 John Wiley & Sons, Ltd.DOI: 10.1002/er

and 25°. XRD results show that the diffraction peaks of V2O5

become wider and weaker after the intercalation of aniline.This indicates that the intercalation of aniline caused theV2O5 lattice structure to collapse and that the product beingrelatively crystalline is ascribed to the limited short-range or-der, in accordance with Li’s result [25]. The slight shift tohigher 2θ in the nanocomposite, compared to V2O5, confirmsthe effect of the interaction between Pani and V2O5 at thesurface of the nanocomposite.

3.3. XPS analysis

An XPS measurement was performed to determine thesurface composition and chemical state of the preparednanocomposite, the results of which are shown in Figure 3.

The major feature of the core-level spectrum of C1s is apeak at approximately 284.5 eV, which is characteristicof the neutral carbon species. The V2p band showing theV2p3/2 and V2p1/2 is attributed to the oxide form of V+5.The peak of vanadium 2p3/2 in vanadium oxide occurs at517.3 eV. This spectrum shifts to a lower binding energy(approximately 516.5 eV in the Pani/V2O5 composite),which means the vanadium converts to a lower oxidationstate in the presence of Pani. In other words, the vanadiumcore is influenced by the Pani electrons.

The XPS spectrum of the nitrogen (1s level) in the Panireveals a peak centred at 399.6 eV, which shifts to a higherbinding energy at about 1 eV in the Pani/V2O5 composite.The shifting of N1s to the higher binding energy in thecomposite is presumably related to the interaction ofnitrogen in the Pani with the V2O5 oxygen atom.These results are in agreement with the FTIR andXRD results [32,33].

3.4. BET surface area analysis

The nitrogen adsorption/desorption isotherms of Pani andPani/V2O5 nanocomposite are shown in Figure 4. Clearly,the isotherm depicts type IV isotherms with H3 typehysteresis loops. Both Pani and Pani/V2O5 nanocompositesrepresent a mesoporous structure.

The nanocomposite exhibits a highly mesoporousstructure, which is of great interest for its application aselectrodes, because it represents an optimization of theelectrode–electrolyte interface [34]. The average pore sizeswere determined at 22.9 nm for Pani and 16.2 nm for Pani/V2O5 nanocomposite. The BET surface area for both

510515520525530535

Inte

nsit

y (a

.u.) V2O5

b) V2p

2p3/2

2p1/2

390 395 400 405 410

Inte

nsit

y (a

.u.)

Binding Energy (ev)

Binding Energy (ev)

a) N 1s

Pani/V2O5 nanocomposite

Pani/V2O5 nanocomposite

Pani

Figure 3. XPS spectra of a) N1s in Pani and Pani/V2O5, b) V2plevel in: V2O5 and Pani/V2O5.

10 20 30 40 50 602θ (°)

200 00

1

101

110

400

011

302

411

102

002

310

a

b

c

Figure 2. XRD pattern for a) Pani/V2O5, b) V2O5 nanoparticle,and c) Pani.

0

60

120

180

0 0.2 0.4 0.6 0.8 1

Relative Pressure P/p0

Relative Pressure P/p0

b) Pani/V2O5 nanocomposite

0

50

100

150

200

0 0.2 0.4 0.6 0.8 1

Qu

anti

ty A

dso

rbed

(cm

3 /g

) Q

uan

tity

Ad

sorb

ed(c

m3 /

g)

a) Pani

Figure 4. N2 adsorption/desorption isotherms of a) Pani and b)Pani/V2O5.



compounds was also identified at 35.2 and 9.2 m2/g forPani and nanocomposite, respectively.

3.5. FESEM analysis

The morphologies of the prepared Pani/V2O5

nanocomposite and pure Pani are shown in Figure 5. Bothpure Pani and its nanocomposite present a specific struc-ture with a fairly uniform size distribution. The V2O5

nanoparticles are very fine and are scattered in all placesof the Pani support. The nanocomposite exhibits a highlymesoporous structure, which leads to interest in its applica-tion as a catalyst [35].

The FESEM results are totally compatible with theresults obtained from the N2 adsorption/desorptionisotherms. In terms of the nanocomposite, no barenanoparticles were observed, which confirms that themicelle technique produced a well-dispersed nanoparticle.

3.6. Electrochemical properties

To determine whether Pani, V2O5, and Pani/V2O5 contrib-ute to the catalytic reaction, their oxygen reduction proper-ties in a half cell were analysed using Cyclic Voltammetry(CV) and Linear Sweep Voltammetry (LSV).

Figure 6 shows the CV graph of the catalysts.Apparently all three catalysts exhibited an ORR peak.The position and size of the peaks indicate whether thematerial is good enough to be applied as a catalyst and

whether the reaction is spontaneous or not. In this case,all three peaks were in negative potential range, whichconfirms that the reaction was spontaneous. Furthermore,the Pani/V2O5 peak was larger than that of both V2O5

and Pani, which shows that Pani/V2O5 has a higherpotential for ORR than Pani or V2O5.

The results from the LSV test for different catalysts areshown in Figure 7. The figure shows that among all cata-lysts, Pani/V2O5 nanocomposite has the highest electrocat-alytic activity for ORR. This may be due to the smaller sizeof the nanocomposite (as mentioned in the BET results)and also the significant electronic interaction of V2O5 andPani in the nanocomposite, which makes Pani/V2O5 abetter redox catalyst. Furthermore, the homogeneousmesoporous structure of the nanocomposite producespromising catalytic activity and, consequently, an effectiveinteraction between Pani/V2O5 and O2 during thereduction reaction [36].

3.7. Power density

Figure 8 shows the power density graph of differentcathode catalysts in MFC. The Pani/V2O5 nanocompositecathode catalyst produced 79.26 mW/m2 power density at194.29 mA/m2 current density. This was higher than the

Figure 5. FESEM micrographs of the: a) Pani/V2O5 and b) Pani.

E/ V vs. Ag/AgCl

-1.0 -0.5 0.0 0.5 1.0

I (A

)

-0.1

0.0

0.1

0.2

0.3Pani

Pani/V2O5

V2O5

Figure 6. CV of the fabricated electrodes.

mA.m-2

-1.0 -0.5 0.0 0.5 1.0

W.m

-2

-0.14

-0.12

-0.10

-0.08

-0.06

-0.04

-0.02

0.00

0.02

0.04

PaniV2O5Pani/V2O5

Figure 7. LSV of the fabricated electrodes.



power produced by Pt., which was 72.1 mW/m2 at 173.3mA/m2. This shows that the Pani/V2O5 nanocomposite cat-alyst can produce even more power than Pt as a traditionalcathode catalyst. This could be due to the unusual proper-ties of composites compared to neat materials. A V2O5

production of 65.31 at 208.66 demonstrates a good poten-tial for being a cathode catalyst, followed by Pani with42.4 mW/m2 at 132.9 mA/m2.

3.8. COD removal and CE

To observe the performance of MFCs in wastewatertreatment and the electricity production, the COD removaland the CE of different MFCs were calculated (Figure 9).As the figure shows, the MFC using the Pani/V2O5

nanocomposite had a higher CE (16%) than the MFC usingwith V2O5 (9.2%) or Pani (5.5%). This result is inagreement with the power density and ORR data andmeans that a higher percentage of consumed substratescan be converted into electricity in the MFC using with aPani/V2O5 cathode catalyst. This is due to a better andfaster ORR in the system, which maintained the MFC pHbalance, and the microorganisms tended to produceelectrons and protons faster [37]. Furthermore, the CODremoval data shown in Figure 9 confirms that MFC is a

suitable tool for wastewater treatment and the productionof electricity [38,39].

4. CONCLUSIONS

The main objective of this study was to find an alternativefor Pt, which is a common but expensive cathode catalystused in MFCs. Therefore, three cathode catalysts wereprepared and tested for their power production ability inan MFC system. The results showed that Pani/V2O5

produced as much power as Pt. Moreover, V2O5 couldproduce approximately 80% of the power of Pt. Thisimplies that Pani/V2O5 could be a good alternative to Ptin MFC. Moreover, by improving the properties of V2O5

(i.e. the attachment of some groups to make a composite,etc.), it could serve as a cathode catalyst in MFCs.

ACKNOWLEDGEMENT

The authors appreciate the financial support rendered bythe National University of Malaysia by young researcher’sgrant (GGPM-2013-027) for this project.

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