Journal of Power Sources 276 (2015) 32e38

Contents lists available at ScienceDirect

Journal of Power Sources
journal homepage: www.elsevier.com/locate/jpowsour

Water soluble graphene as electrolyte additive in magnesium-air
battery system
M. Mayilvel Dinesh a, K. Saminathan a, *, M. Selvam a, S.R. Srither a, V. Rajendran a,
Karan V.I.S. Kaler b
a
Center for Nanoscience and Technology, K.S. Rangasamy College of Technology, Tiruchengode, 637215 Tamil Nadu, India
b
Department of Electrical and Computer Engineering, Schulich School of Engineering, University of Calgary, Calgary, Alberta, Canada

h i g h l i g h t s 

WSG was successfully synthesized and utilized as a catalyst to improve Mg-Air system. 
High specific capacity of 1030.71 mAh g 1 and current density of 19.33 mA cm 2 achieved. 
Mg anode breakdown during self-discharge cycle was circumvented. 
Reduction in Hydrogen gas evolution at Mg anode in WSG based NaCl electrolyte.

a r t i c l e i n f o a b s t r a c t

Article history: Magnesium-air (Mg-air) batteries are an important energy source used to power electronic equipment
Received 26 August 2014 and automobiles. Metal-air batteries give more energy density due to surplus air involved in reduction
Received in revised form reaction at air cathode. In this study, the scope of improvements in the efficiency of Metal-air batteries is
10 November 2014
investigated through addition of water soluble graphene (WSG) as inhibitor in NaCl electrolyte. The
Accepted 15 November 2014
Available online 20 November 2014
discharge performance, corrosion behaviour and electrochemical impedance are studied for (i) the
conventional Mg-air battery using 3.5% NaCl and (ii) Mg-air battery with WSG-based 3.5% NaCl elec-
trolyte. X-ray diffraction analysis for WSG is carried out and it shows the crystalline nature of WSG by an
Keywords:
Magnesium-air battery
intense sharp peak at 26.3 . Scanning electron microscope study is also performed and shows the flake-
Electrochemical property like structure of WSG denoted by thin layers of carbon. The immersion of WSG in 3.5% NaCl electrolyte
Graphene increased the current density from 13.24 to 19.33 mA cm 2. Meanwhile, the WSG-based Mg-air battery
Corrosion resistance was found to hold specific discharge capacity of 1030.71 mAh g 1, which was higher than that obtained
in 3.5% NaCl electrolyte (i.e., 822.85 mAh g 1). The WSG-based Mg-air battery shows good self-discharge
capacity and higher electrochemical activity during discharge.
© 2014 Elsevier B.V. All rights reserved.

1. Introduction predicted to generate high energy densities due to surplus oxygen
taken from ambient atmosphere at cathode as a result of the open
Electrochemical method of energy production in batteries used cell structure [6]. Moreover, the anode in a metal-air battery can be
for powering electronic devices and for greener transportation of mechanically recharged, thus minimizing the battery charging
electric vehicles has received considerable attention in research time. The unique feature of the metal-air battery is that only one
community [1]. Vehicles powered by batteries or fuel cells can in- active component of the negative electrode (anode) is sufficient to
crease their efficiency and reduce emission of pollutants and store energy.
greenhouse gases [2e4]. Metal-air batteries generate electrical Magnesium-air (Mg-air) primary batteries are a preferred
power as a result of redox reaction between a metal electrode and source of power because of their longer discharge times, high
oxygen present in air [5]. Metal-air batteries are theoretically theoretical output voltage (3.09 V), high energy density
(3910 Wh kg 1), lower cost [5,7e9], and environment-friendly
nature. The open-circuit voltage obtained from an Mg-air battery
* Corresponding author. using a magnesium anode with a sea-urchin like nanostructure is
E-mail address: ksaminath@gmail.com (K. Saminathan).

http://dx.doi.org/10.1016/j.jpowsour.2014.11.079
0378-7753/© 2014 Elsevier B.V. All rights reserved.
M. Mayilvel Dinesh et al. / Journal of Power Sources 276 (2015) 32e38 33

1.42 V, compared to 1.32 V from a battery with magnesium anode water was slowly added and the solution was maintained at 30  C
having nano sphere structure [10]. It is well-known that sodium in a stirrer for 15 min. After this, 3 ml hydrogen peroxide (30%
chloride (3.5% NaCl) is the most suitable electrolyte for magnesium H2O2) was slowly added by a dropper. The colour of the solution at
electrode to provide a maximum discharge current. Despite many this point changed from dark brown to light brownish yellow,
advantages of Mg-air batteries, it is highly susceptible to corrosion indicating the reduction of graphite with mixture under continuous
of the magnesium electrode (anode), resulting in a reduction in the stirring at 30  C. To this solution, 250 ml distilled water was again
operating life [5]. The reduced battery life is considered to be added and stirred for 5 days, after which the stirring was turned off
because of generation of gaseous hydrogen during discharge cycle, and the reactants were allowed to settle. From this final solution,
resulting in a well-known “negative difference effect”. This nega- surplus water was removed using a syringe and the remaining
tive difference effect and anodic break down are thus the inherent solution with the reactants was centrifuged at 10,000 rpm using a
limitations of a Mg-air battery. Charging of Mg-air battery is the centrifuge (C-24BL; REMI, India) for 1 h. The reactant sample after
reverse of oxygen reduction reaction, which is difficult to achieve centrifugation was dried in an oven at 120  C, yielding 3 g black
practically [11e15]. In addition, the reduction reaction occurring at graphite oxide powder.
air cathode is slower than anodic oxidation resulting in reduction of
the battery performance. To overcome these limitations of Mg-air 2.2. Preparation of graphene
battery, a catalyst is added in 3.5% NaCl electrolyte, which im-
proves the battery performance [16]. After the synthesis of graphite oxide in the powder form, gra-
Recently, nanomaterials of carbon have attracted considerable phene was prepared using 2 g graphite oxide powder mixed with
attention for their improved performance in fields of catalysis, 200 ml distilled water and glass beads (5 mm in diameter) in a
energy and environmental technologies [17,18]. Mixing of salts in round bottom flask. A hollow glass tube was secured to the mouth
an electrolyte solution forms partial oxide layer which results of the round-bottom flask to facilitate water flow, aided by an inlet
reduced corrosion over the anode [19]. Graphene is a single-layered and outlet valve assembly. The graphite oxide suspension was
carbon atom having hexagonal honey comb lattice structure [20], heated to 80  C aided by a heating mantle. The water flow through
provides very good electrical conductivity, and is immune to cor- the hollow tube condensed the vapours arising from the heated
rosive effects [21]. In addition, carbon-based anodes deliver high suspension. The volume of the graphite oxide suspension was
discharge capacities (320 mAh g 1) [17,22e25], can be used as gas maintained by continuous flow of water through the hollow tube.
adsorbent, and serve as a heterogeneous catalysis [26]. Graphene After 15 min, 2 ml hydrazine hydrate (N2H2OH) [28] was drop-wise
materials used as an electrocatalyst have a large surface area, added to the suspension with the help of a pipette. The suspension
resulting in high electrical conductivity and high mechanical and was maintained at 80  C for 6 h and then allowed to cool. The
thermal stability [15,27]. Graphene is also chemically inert and suspension was then dried using hot-air chamber and the resulting
stable at temperature up to 400  C. Graphene sheets have tensile graphene powder collected for the next step [29].
modulus and their ultimate strength values are similar to those of Graphene powder (0.1 g) was suspended in 100 ml distilled
single-walled carbon nanotubes [27]. water and kept in suspension (A). In addition, 2 g sodium hydroxide
The aim of this study was to investigate the utility of water- (NaOH) pellets dissolved in 50 ml distilled water (B). The suspen-
soluble graphene (WSG) as a catalyst additive in a salt electrolyte sion sample A was sonicated followed by the addition of solution B
for Mg-air battery and to determine its impact on the performance in a drop-wise manner to achieve a final pH value of 8. Finally, the
of battery. Doping of graphene sheets with poly (sodium 4- graphene powder solution was dried at 80  C in hot-air chamber
styrenesulfonate) has been carried previously to disperse gra- until all the moisture was removed, yielding a finely dried WSG
phene in aqueous solution [28]; however this study did not powder [30].
investigate the utility of using graphene as a catalyst in an elec-
trolyte in Mg-air battery to enhance the discharge capacity of the 2.3. Characterisation techniques
WSG-based Mg-air battery.
In this regard, we specifically examined the efficiency of Mg-air 2.3.1. XRD
battery in 3.5% NaCl and WSG-based 3.5% NaCl electrolytes by The structure of the WSG powder was analysed using an X-ray
studying the discharge behaviour of magnesium anode in the diffractometer (X'Pert PRO; PANalytical, the Netherlands). The
performance of electrolytes at various discharge current densities. powdered sample was analysed through CuKa radiation source
We furthermore investigated the morphology of the WSG samples with 1.5406 Å wavelengths. Here the sample was scanned at a rate
used. Corrosion resistance and electrochemical impedance studies of 0.05 min 1, starting at an angle 10 and ending at an angle of 80 .
(EIS) were also performed to determine the impact of WSG catalyst
in enhancing the discharge performance of the WSG-based Mg-air 2.3.2. FTIR
battery. The quality of WSG sample was analysed using a Fourier
transform infrared spectrophotometer (Spectrum 100; Perkin
2. Experimental procedure Elmer, USA). The WSG sample was mixed with potassium bromide
(KBr) in 1:100 ratio and the pellet was formed under a hydraulic
2.1. Preparation of graphite oxide pressure of 120 kg cm 2. The sample was irradiated with IR radi-
ation (4000e400 cm 1) to obtain the FTIR spectrum based on the
Graphite oxide was prepared by modified Hummer's method transmission characteristics of the sample.
[20]. The preparation was carried out in a 500-ml beaker covered
with ice packs. In this procedure, 2.5 g graphite powder and 1 g 2.3.3. SEM
sodium nitrate (NaNO3) were mixed and then 46 ml concentrated The morphology of the WSG sample was determined experi-
sulphuric acid (H2SO4) was gradually added under constant stirring mentally using a scanning electron microscope (SEM; JSM-6390LV;
conditions. To this mixture, 8 g potassium permanganate (KMnO4) JEOL, Japan) operated at a potential of 20 kV. An example SEM
powder was gradually added. The colour of the solution during this image of the sample was captured at the magnification of 15,000
procedure changed from deep pink to dark brown. The solution was with the focal length maintained at 1 mm between the lens and the
stirred for an additional 30 min, after which 250 ml of distilled sample surface.
34 M. Mayilvel Dinesh et al. / Journal of Power Sources 276 (2015) 32e38

2.4. Magnesium-air battery construction our actual battery, as shown in Fig. 1b, was very thin around 3 mm
wide and 8 cm long, finely polished using emery paper (100 grade)
The Mg-air battery was constructed using a magnesium anode and capable of supporting a high discharge current. This enabled
and an air cathode, and immersed in a 3.5% NaCl electrolyte by the corrosion rate of the magnesium to be more readily monitored
weight. The electrochemical reaction driving the Mg-air battery compared to a bulk rod electrode. Approximately 5.5 cm of the strip
[19] can be denoted as follows: was immersed in 3.5% NaCl electrolyte during discharge cycle
Anodic reaction measurements with a total effective electrode surface area of ~
3.3 cm2. For the air cathode, a stainless steel mesh was used
Mg / Mg2þ þ 2e (i) because it is electrochemically inert for the electrolyte used. The
pore size of this mesh was ~0.1 cm, and it plays a predominant role
Cathodic reaction during redox reaction. The SS mesh was rolled into a single turn and
housed inside the circumference of the beaker of cell structure. For
O2 þ 2H2O þ 4e / 4OH (ii) Mg-air battery, 200 ml 3.5% NaCl contains 0.2 g WSG catalyst
powder solution, which served as the electrolyte. The additions of
Overall reaction WSG powder helped to increase the conductivity of the electrolyte
solution and, furthermore, helped to control and minimize the
2 Mg þ O2 þ 2H2O / 2Mg(OH)2 (iii) corrosion of the magnesium anode. To obtain a uniform current
distribution in the cell, the magnesium anode was located in the
The schematic representation of Mg-air battery is shown in centre of the Mg-air battery cell, as shown in Fig. 1b.
Fig. 1a illustrating the energy liberated by an electrochemical re-
action. For this Mg-air battery setup, the magnesium electrode
shown in the figure represents the anode. This magnesium strip in 2.5. Electrochemical measurements

The discharge performance and operating life of the Mg-air
battery was analyzed for the discharge currents of 5, 10, 15 and
20 mA, controlled by varying the load resistance. The battery
discharge performance was determined by plotting current den-
sities under various load conditions rather than the total battery
drain current. The operating life of the battery in hours was
determined using the discharge current data at when the battery
voltage reached 0.2 V and was plotted for various current densities.
In addition to the above variable load condition, the Mg-air
battery was then tested further under short-circuit condition. In
these experiments, both the current and the voltage were moni-
tored at a regular interval (5 min) during the discharge cycle for
30 min in 3.5% NaCl and WSG-based 3.5% NaCl electrolytes.
The corrosion behaviour of magnesium anode was examined by
using a three-electrode configuration a working electrode (mag-
nesium strip), a platinum counter electrode and a calomel reference
electrode. The corrosion behaviour was studied for both NaCl and
WSG-based NaCl electrolyte solution in electrochemical work sta-
tion (PGSTAT302N; Metrohm Autolab, the Netherlands). The
applied potential window for corrosion study was in the range

Fig. 1. Schematic representation of magnesium-air battery. Fig. 2. FTIR pattern for water soluble graphene.
M. Mayilvel Dinesh et al. / Journal of Power Sources 276 (2015) 32e38 35

between 1.8 and 1.0 V at a scan rate of 3 mV s 1. Tafel slope was CeH bonds in the WSG sample. The quality of the WSG sample has
constructed from the measurement data, and a Potentiodynamic been determined from the nature of vibrations occurred at corre-
polarization graph obtained for the negative potential window sponding bonding.
versus Icorr rate. The presence of corrosion peak obtained at a
negative potential indicates corrosion of the magnesium anode. 3.3. SEM
In addition, the corrosion inhibition property of WSG was
evaluated by EIS at the electrochemical work station The SEM image of the WSG sample is shown in Fig. 4. The sur-
(PGSTAT302N). EIS was carried out for a magnesium anode face morphology of WSG has been determined, and it exhibits a
immersed in 3.5% NaCl as well as WSG-based 3.5% NaCl electrolyte flake-like structure. Furthermore, Fig. 4 shows that these thin flake-
using the three-electrode cell configuration under open-circuit like features are due to minimal arrangement of a carbon layers. In
potential. The impedance data was measured in the frequency addition, these thin flakes are well interconnected, which indicates
range of 100 kHz to 1 mHz at an amplitude of 0.1 V. that the WSG samples have a high electrical conductivity and are
metallic in nature [31].
3. Results and discussions
3.4. Magnesium-air battery discharge investigation
3.1. XRD
Discharge study has been performed in Mg-air battery at
The diffraction pattern for WSG sample as shown in Fig. 2, ex- different current densities of 1.5, 3, 4.5 and 6 mA cm 2 in 3.5% NaCl
hibits a sharp peak at 26.3 (002) and a broader peak at 43.7 (101). and WSG-based 3.5% NaCl electrolytes. The open-circuit voltages
The peak observed at 26.3 (2q) is attributed to the crystal nature of obtained in 3.5% NaCl and WSG-based 3.5% NaCl electrolytes were
WSG due to high concentration of sulphuric acid, whereas the less 1.47 and 1.57 V, respectively, which are higher than 1.42 V obtained
intense, broad peak at 43.7 represents the partial crystalline na- in sea-urchin like nanostructure of a magnesium anode [10]. Fig. 5
ture of the WSG sample. The diffraction peaks were compared with shows the discharge performance of Mg-air battery in 3.5% NaCl
a JCPDS file no. 411487, which exhibits a maximum at 26.2 , thus electrolyte solution. The battery life measured in hours obtained
suggesting that a presence of hexagonal structure carbon atoms in from the discharge plots are 16.38, 10.55, 8 and 4.96 h at discharge
the WSG sample [20]. current densities of 1.5, 3, 4.5 and 6 mA cm 2, respectively. In
comparison, for WSG-based Mg-air battery, the battery life ob-
tained from discharge plots (as shown in Fig. 6) are 21.45, 12.25,
3.2. FT-IR
9.62 and 6.17 h for load current densities of 1.5, 3, 4.5 and
6 mA cm 2, respectively.
The qualitative analysis for the WSG sample using FTIR is shown
The results show that for current densities 1.5, 3, 4.5 and
in Fig. 3. A stretching vibration peak observed at 1390 cm 1 may be
6 mA cm 2, the operating life of anode is increased by 30.95%,
attributed to the presence of CeC bonds, whereas the peaks
16.11%, 20.25% and 24.39%, respectively. Furthermore, the WSG-
observed at 1378 cm 1 [20], and 1518 cm 1 correspond to C]O
based Mg-air battery achieved discharge capacity of
bonds. Another sharp but less pronounced stretching vibrational
1030.71 mAh g 1 compared to 822.85 mAh g 1 achieved by 3.5%
peak is due to the presence of CeC bond, which illustrates a few
NaCl-based Mg-air battery. Thus, we may conclude that the Mg-air
layer availability of carbon and the quality of bonds has been
battery holds more discharge capacity than a comparable Mg/
studied based on their shapes. Another weak stretching vibration
MnO2-based battery (768 mAh g 1) [32]. The discharge curve for
observed at 1165 cm 1 is considered to be due to the presence of
the WSG-based Mg-air battery exhibits elongated discharge
CeO bonding, a similar behaviour is observed at 1163 cm 1 for
plateau and gradual decrease in voltage, whereas an abrupt drop in
graphene [30]. A sharp symmetrical peak observed at 590 cm 1 is
voltage is observed for the 3.5% NaCl-based Mg-air battery. This
due to CeH bonding, which denotes the significant presence of
observation suggests that the mixture of WSG and NaCl present in
an electrolyte maintains an almost constant conductivity. Further-
more, the hydrogen gas evolution and the anodic corrosion are

Fig. 3. XRD pattern for water soluble graphene. Fig. 4. SEM image for water soluble graphene.
36 M. Mayilvel Dinesh et al. / Journal of Power Sources 276 (2015) 32e38

Fig. 5. Discharge performance of magnesium-air battery in 3.5% NaCl.
Fig. 7. Short circuit study of magnesium-air battery in 3.5% NaCl and WSG based 3.5%
NaCl.

in electrolyte. The graphene-rich OH suppose to be deposited over
the magnesium anode, which acts to protect it and hence reduces
its corrosion.

3.5. Short-circuit studies

The short circuit study of the Mg-air battery is carried out in
both 3.5% NaCl-based and WSG-based 3.5% NaCl electrolyte solu-
tions. Table 1 summarizes the short-circuit voltages, currents, and
current densities measured during this test. The short-circuit
voltages measured in 3.5% NaCl-based and WSG-based 3.5% NaCl
battery are 1.54 and 1.25 V, respectively. Fig. 7 shows the self-
discharge curves for the WSG-based Mg-air and 3.5% NaCl-based
electrolyte battery obtained from the current measured over
0.5 h. It is readily apparent that the WSG-based Mg-air battery with
a higher electrical conductivity exhibited a discharge current
plateau that decreased from 63.8 to 51.9 mA, whereas the discharge
Fig. 6. Discharge performance of magnesium-air battery in 3.5% NaCl with WSG.
plateau decreased from 43.7 to 23.9 mA in case of 3.5% NaCl elec-
trolyte battery. Thus, the discharge current drain increased by
45.99% in case of WSG-based Mg-air battery compared to the NaCl
decreased by the partial formation of oxide layer over the magne- electrolyte counterpart. Furthermore, the magnesium anode is
sium anode due to WSG. As an electrolyte additive, the WSG totally consumed by 3.5% NaCl electrolyte, but in case of the WSG-
enhanced the electrical conductivity in an electrolyte, resulting in based NaCl, anodic breakdown is avoided as result of the reduced
the observed improvement in the battery discharge performance. self-corrosion of the magnesium anode. The current density is
This is due to the transformation of OH along with WSG particles furthermore improved from 13.24 to 19.33 mA cm 2 due to the
addition of WSG to NaCl electrolyte.

Table 1
Short circuit study of magnesium-air battery in 3.5% NaCl and water soluble graphene based 3.5% NaCl electrolyte.

Duration (min) In 3.5% of NaCl electrolyte In 3.5% of NaCl electrolyte with water soluble graphene (WSG)
2 2
Observed voltage (V) Observed current (mA) Current density (mA cm ) Observed voltage (V) Observed current (mA) Current density (mA cm )

0 1.54 43.7 18.20 1.25 63.8 26.58
5 1.05 32.2 13.41 0.86 57.8 24.08
10 0.90 26.7 11.12 0.76 53.8 22.41
15 0.72 25.9 10.79 0.72 53.2 22.16
20 0.68 24.4 10.16 0.71 52.8 22.00
25 0.68 23.9 9.95 0.71 52.5 21.87
30 0.68 23.9 9.95 0.65 51.9 21.62
M. Mayilvel Dinesh et al. / Journal of Power Sources 276 (2015) 32e38 37

3.6. Corrosion studies

Comparative corrosion studies are carried out for both the
magnesium anode in 3.5% NaCl electrolyte and the WSG-based 3.5%
NaCl electrolytes. The potential is applied at 1.8 V and the
corrosion is started at magnesium anode. The potential tends to
move towards 1 V with interval of 3 mV s 1. Fig. 8 shows the
corrosion curves plotted for magnesium anode in 3.5% NaCl and
WSG-based 3.5% NaCl electrolyte. The solid line curve indicates the
corrosion behaviour of magnesium anode in 3.5% NaCl electrolyte.
The dotted line curve indicates the corrosion behaviour in the
WSG-based 3.5% NaCl electrolyte. The extreme slope is observed
during corrosion measurement at 1.57 V [33] in 3.5% NaCl envi-
ronment whereas it is observed at 1.65 V for the WSG-based 3.5%
NaCl environment. The slope is observed to be shifted toward more
negative potential. The above statement assured that low self-
corrosion rate and high electrochemical behaviour are achieved
due to nano-layered coating of WSG over the surface of magnesium
anode and also due to the suspended WSG nanoparticles in an
electrolyte that provides continuous electrochemical behaviour.

3.7. Impedance studies

Fig. 9 shows the electrochemical impedance analysis in the form
of Nyquist plots of (i) magnesium anode immersed in 3.5% NaCl
electrolyte and (ii) magnesium anode in WSG-based 3.5% NaCl
electrolyte. The measurements are conducted on a magnesium
anode for an open-circuit voltage of 1.65 V. The solution resistance
Rs of 2.8 U and the charge transfer resistance Rt of 31.9 U are ob-
tained from the low-frequency impedance data obtained for the
3.5% NaCl electrolyte cell.
Similarly, the solution resistance Rs of 6 U and the charge
transfer resistance Rt of 83.6 U are obtained for the WSG-based 3.5%
NaCl electrolyte. The charge transfer resistance has been increased
from 31.9 to 83.6 U due to the impact of WSG in 3.5% NaCl elec-
trolyte. The liberal discharge of electrons from the magnesium
anode is controlled using WSG that forms the protective coating
over anode surface. As a result, the charge flow and resistance
offered during charge transfer increased. The Nyquist plot for the
WSG-based 3.5% NaCl shows a large semi-circular diameter than

Fig. 9. Electrochemical impedance curve for magnesium in 3.5% NaCl and WSG based
3.5% NaCl.

Fig. 8. Potentiodynamic polarization curve for magnesium in 3.5% NaCl and WSG
based 3.5% NaCl.
38 M. Mayilvel Dinesh et al. / Journal of Power Sources 276 (2015) 32e38

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