Materials Research Bulletin 100 (2018) 295–301

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Materials Research Bulletin

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Synthesis and electrochemical properties of silver dendrites and silver T

dendrites/rGO composite for applications in paracetamol sensing
⁎
S. Dhanusha, M. Sreejesha, K. Bindua, P. Chowdhuryb, H.S. Nagarajaa,
a
Materials Research Laboratory, Department of Physics, National Institute of Technology, Karnataka Surathkal, 575 025, India
b
Nanomaterials Research Laboratory, Surface Engineering Division, National Aerospace Laboratories, Council of Scientific and Industrial Research, Bangalore, 560 017,
Karnataka India

A R T I C L E I N F O A B S T R A C T

Keywords: Electrochemical sensors are one of the important applications of electrochemistry. In this paper, synthesis,
Silver dendrites characterization and application of Silver Dendrites and Silver Dendrites/rGO sensors for simple and fast de-
Galvanic replacement method termination of Paracetamol are described. Silver dendrites and their composite with graphene oxide were
Paracetamol synthesized by galvanic replacement method. The synthesized samples were characterized by XRD, SEM and
Cyclic voltammetry
TEM. XRD reveals the FCC structure of silver and TEM images show the formation of dendritic silver wrapped in
Chronoamperometry
the graphene sheets. The Electrochemical paracetamol sensing properties of these samples were tested using
cyclic voltammetry and chronoamperometry. The silver dendrites exhibit a sensitivity of 2.807 × 105μA/mM/g
and a lower detection limit of 2.5 μM, whereas, the composite with graphene oxide exhibits a high sensitivity of
2.511 × 106μA /mM/g with a lower detection limit of 0.025 μM.

1. Introduction
Shape controlled synthesis of various nanostructures has drawn the
attention of scientific community because of their novel properties and
applications in various fields [1]. Among different metal nanos-
tructures, silver nanostructures have gained considerable importance
due to their unique electrical [2], optical [3] and catalytic performance
[4] and intriguing applications in electrochemical sensors, catalysis,
magnetic devices, hydrophobic surface and Surface Enhanced Raman
Scattering (SERS) [5–8]. Since intrinsic properties of these structures
can be tuned by changing their shape, size, composition, morphology
and structure, a large number of synthesis methods have been explored
to perform shape controlled synthesis of Ag nanostructures [9]. Various
researchers have successfully synthesized the different morphological
Ag nanostructures viz. wires [10], cubes [11], triangles [12], disks
[13], rods [14], prisms [15] and dendrites [16]. Among a variety of
different morphologies, the dendritic structure have a particularly at-
tractive structure for catalysis and electrochemical systems due to its
unique properties such as numerous active sites, hierarchical structure,
high surface area and sharp edges.
Silver dendrites are composed of a central stem and many hier-
archical branches and attached leaves. The synthesis methods for silver
dendrites include Template method [17], Electrochemical method [18],
Sono-chemical method [19], photo reduction [20], microwave method
[21]. Apart from these methods, galvanic replacement reaction has
come up as a promising synthesis technique in past decade as it is
simple to perform and gives a high yield.
Galvanic replacement reaction involves simultaneous electro-
chemical redox reaction on the substrate. The sacrificial substrate
(generally Cu, Zn and Al) gets oxidised and dissolves in solution and
another metal ion in solution phase is reduced and plated on top of the
substrate. The electrochemical potential difference between the two
metals is the driving force for the galvanic replacement reaction. Even
though a lot of work has been done on synthesis of Ag dendrites by
galvanic replacement reaction, there is large scope for studies on Ag
dendrites based composite materials and their applications.
Graphene has shown great promise owing to its extraordinary
properties like high electrical conductivity, large surface area, me-
chanical strength and finds applications in electronics, energy storage
and development of bio-sensors [22–24]. Biosensors fabricated using
Graphene based composites find applications in detection of molecules
such as H2O2, Dopamine, Ascorbic Acid, Nitrite ions, Paracetamol etc.
[25,26] Graphene- metal composites give a novel synergism and offer
utility in enhancing the lifetime, selectivity, sensitivity and efficiency of
the core functioning material in electrochemical sensing and catalysis
[27,28].
Paracetamol or N-acetyl-p-aminophenol is a widely used antipyretic
and analgesic drug all over the globe. Paracetamol does not show much

⁎
Corresponding Author.
E-mail address: nagaraja@nitk.edu.in (H.S. Nagaraja).

https://doi.org/10.1016/j.materresbull.2017.12.044
Received 7 June 2017; Received in revised form 14 December 2017; Accepted 28 December 2017
Available online 29 December 2017
0025-5408/ © 2018 Elsevier Ltd. All rights reserved.
S. Dhanush et al. Materials Research Bulletin 100 (2018) 295–301

harmful side effects, hence it is recommended by doctors for reduction
of fever of any origin and mild to moderate pain associated with
headache, arthritis etc [29]. However, an over dose of paracetamol will
lead to liver and nephrotoxic metabolites, which in some cases leads to
renal failure [30]. Hence developing sensitive, selective and cost ef-
fective sensors to detect paracetamol in human serum and quality
control in pharmaceuticals is of great importance.
To the best of our knowledge, there are no reports available on
electrochemical sensors for paracetamol based on Ag dendrites and
Graphene oxide composite. In this study, we have synthesized silver
dendrites and Silver dendrites/ graphene oxide composites via galvanic
replacement reaction. A simple, cost-effective electrochemical sensor
for paracetamol is fabricated by modifying the glassy carbon electrode
(GCE) with synthesized samples.
sample was named GAgD.
2.5. Preparation of the modified glassy carbon electrode (GCE)
Prior to fabrication of modified GCE for sensing application, GCE
was mechanically polished on a velvet cloth with alumina slurry (0.05
μM) followed by electrochemical polishing in 0.1M H2SO4 in the po-
tential window of 0–1 V at a scan rate of 100 mV/S and sonicated in
ethanol and DD water for 5 S each. 1mg of AgD was dispersed in 1ml of
distilled water and ultrasonicated for 15 min to ensure a uniform dis-
persion. 4μl of this dispersion was drop-casted on cleaned GCE and
dried in room temperature to obtain a proper coating (GCE/AgD). Same
process was followed for fabrication of modified GCE with GAgD
sample (GCE/GAgD).

2. Experimental
2.6. Characterization
2.1. Chemicals and materials
The structural studies of the prepared samples were done using X-
ray diffractometer (Rigaku miniflex 600) with CuKα radiation with an X-
Graphite flakes, Sodium nitrate, Sulphuric acid, Potassium per-
ray wavelength of 1.5406Å. The morphological and compositional
manganate, Hydrogen peroxide (30%), and Hydrochloric acid were
studies of the samples were done by Scanning Electron Microscope
used in synthesis of Graphene Oxide. Silver nitrate, Sodium chloride,
(JEOL, JSM 6380 LA) using an electron beam of kinetic energy 20 keV
Aluminium foils and Ammonia hydroxide (28–30% NH3 basis) were
and Transmission Electron Microscope (JEOL JEM 2100) equipped with
used in synthesis of Silver Dendrites and Silver Dendrites/rGO com-
an Oxford Energy Dispersive Spectrometer.
posite. All the above chemicals were purchased from Sigma Aldrich and
The electrochemical paracetamol sensing properties have been
used without any further purification. Double distilled (DD) water
studied using cyclic voltammetry (CV), chronoamperometry (CA) and
prepared at the lab using double distillation unit, was used throughout
electrochemical impedance spectroscopy (EIS) techniques using BIO-
the experiments.
LOGIC (SP-150). A conventional three-electrode system was employed
to study the paracetamol sensing. Platinum electrode and Ag/AgCl
2.2. Synthesis of graphene oxide (GO)
electrode were used as counter electrode and reference electrode re-
spectively. Modified Glassy Carbon Electrode was used as working
The graphene oxide was prepared using the modified Hummer’s
electrode. 0.1M phosphate buffer solution (PBS) was used as an elec-
method [31]. In brief, weight equivalents of graphite flakes (3 g) and
trolyte throughout the experiments. The concentration of paracetamol
NaNO3 (3 g) were mixed with 46 mL of concentrated H2SO4 in an ice
in the electrolyte was varied by injecting the paracetamol from stock
bath for about 30 min. Thereafter, 3 wt equivalents of KMnO4 was
solution using micropipette.
added to the solution. The solution was then stirred at room tempera-
ture till it became a thick paste. Later, 46ml of water was slowly added
to the solution. After 30 min, 140ml of DD water and 10 ml of H2O2 3. Results and disscussions
(30%) were poured into the mixture in sequence. This solution was
filtered and washed with 3% HCl and distilled water several times till 3.1. X-ray diffraction
the sample pH is neutral. The solution of Graphite oxide was ultra-
sonicated for 1 h to obtain graphene oxide [31]. The X-ray diffraction (XRD) patterns of AgD and GAgD synthesized
by galvanic replacement method are shown in Fig. 1. The XRD pattern
2.3. Synthesis of silver dendrites (AgD) of both AgD and GAgD clearly reveals four sharp intense peaks of (1 1
1), (2 0 0), (2 2 0) and (3 1 1) planes of face centered cubic (fcc) Ag
The Silver Dendrites were synthesised using galvanic replacement (a = 4.09) at 2θ = 38.24°, 44.5°, 64.8° and 77.7° respectively. All the
method with aluminium as scarifying material. 1.5 ml of ammonia so-
lution and 1.5 ml (0.1M) NaCl were added to 30ml of AgNO3 (20mM)
solution and stirred well for 15 min. Thereafter, 40 pieces of Al foils
(1*1 cm2) were immersed into this mixture. This was transferred to
Teflon lined stainless steel autoclave (50ml capacity) and heated to
120 °C for 2 h. This mixture was naturally cooled down and precipitate
was collected and washed several times by DD water. Final sample was
obtained by drying in an oven for 60 °C for 6 h. This sample was named
AgD.

2.4. Synthesis of GAgD composite

0.8 ml of ammonia solution and 0.8 ml (0.1M) NaCl were added to

16ml of AgNO3 (20mM) solution. After this, 16ml of GO dispersion
(0.6mg/ml) was added and stirred well for 15 min. Thereafter, 4 pieces
of Al foils (1 × 1 cm2) were immersed into this mixture. This was
transferred to Teflon lined stainless steel autoclave (50ml capacity) and
heated to 120 °C for 2 h. This mixture was naturally cooled down and
the precipitate was collected and washed several times by DD water.
Fig. 1. XRD patterns of AgD and GagD.
Final sample was obtained by drying in an oven for 60 °C for 6 h. This

296
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peaks are consistent with JCPDS No: #04-0783. Apart from these peaks,
a broad hump around 25° is observed for GAgD which can be attributed
to the presence of reduced Graphene Oxide (S1 in Supplementary
reading). XRD results confirm that the preferential growth direction of
Ag dendrites is along (1 1 1) plane.
3.2. Scanning electron microscopy
Fig. 2(a) and (b) correspond to the Scanning Electron Microscope
images of Silver dendrites (AgD) and Silver dendrites/rGO composite
(GAgD) at same magnification. In Fig. 2(a), dendritic structure of silver
with one main trunk and large number of side branches are clearly
observed. Length of main trunk varied from 1μm to 10μm and they
were found to be interconnected with each other. In silver dendrites/
rGO composite (Fig. 2(b) the silver dendrites were wrapped by the
Fig. 3. (a–c) TEM micrographs of GAgD at different magnifications. Inset of Fig. 3.c shows SAED pattern. Fig. 3.d is corresponding EDS spectrum.
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Materials Research Bulletin 100 (2018) 295–301
Fig. 2. (a–b) SEM micrographs of AgD and GAgD respec-
tively.
graphene sheets, which may provide the structural stability to den-
drites.
3.3. Transmission electron microscopy
TEM and HRTEM analysis were carried out to study the morphology
and orientation in GAgD sample and are shown in Fig. 3a, b and c. In
Fig. 3.b silver dendrites wrapped with graphene sheets can be clearly
seen. Side branches are arranged parallel on both sides of the main
trunk and they were evolved at an average angle of 52° as shown in
Fig. 3.a. Even the tertiary branch growth was observed in Fig. 3.b. Inter
planar fringe spacing from HRTEM image given in Fig. 3.c was calcu-
lated to be d = 0.23nm, which is in match with (1 1 1) plane of fcc
silver. Inset of Fig. 3.c displays the selected area electron diffraction
(SAED) pattern, in which discontinuous concentric rings with bright
S. Dhanush et al.
spots are observed. Both inter planar spacing and SAED pattern corre-
spond to characteristic planes of fcc Silver. EDS spectrum shown in
Fig. 3.d reveals presence of silver, carbon and oxygen peaks. In addition
to this, peak corresponding to copper is observed which is due to copper
grid used for TEM.
3.4. Growth mechanism
Even though many mechanisms are proposed [32] for the formation
of dendritic structure, exact mechanism is not yet known as it involves
various factors. Diffusion Limited Aggregation (DLA) model and or-
iented attachment are widely accepted for the growth of dendritic
structures by galvanic replacement [33,34]. As soon the Al foil is im-
mersed in the [Ag(NH3)2]Cl solution, Ag+ ions accepts the electron lost
by Al foil and deposits as Ag metal on Al foil. This Ag deposit, Al foil
and [Ag(NH3)2]Cl comprise a primary cell and displacement reaction
will continue [35]. The parallel growth of the (1 1 1) stacking fault
plane leads to the formation of diskette shaped Ag nanoplates. These
stacking faults act as active sites and boost the reduction of Ag+ ions
and also serve as secondary nucleation sites. In the second stage, the
deposition of Ag metal depletes the Ag+ ions near the surface of the
nanoplate. Then, sequential nucleation and preferential growth under
non equilibrium condition will dominate leading to the formation of
silver dendrites [32].
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Materials Research Bulletin 100 (2018) 295–301
Fig. 4. (a–b) shows the CV response to successive
addition of paracetamol for AgD/GCE and GAgD/
GCE respectively.
The reduction of GO to rGO during the reaction is feasible because
the standard potential of GO, which is -0.40V vs standard hydrogen
electrode (SHE) is higher than that of Al metal (-1.66V vs SHE). Thus
GO is reduced by accepting the electrons lost by Al metal.
Hydrothermal reaction condition also facilitates the reduction of GO
which is already reported by various researchers [36,37]. The Ag+ ions
and GO in the solution can be reduced according to the following redox
reaction [38],
Al + [Ag (NH3)2] + Cl− + GO → Ag + NH3 + AlCl4 + rGO
3.5. Electrochemical properties
3.5.1. Cyclic voltammetry
The electrochemical properties were studied using conventional
three electrode system as mentioned in the characterization section.
Fig. 4.a and 4.b shows the CV curves of AGD/GCE and GAgD/GCE
sensors on successive addition of paracetamol. Electrodes were cycled
between 0.2V to 1V at a scan rate of 50mV/s. Two set of anodic/
cathodic peaks were observed from voltammograms. The first one, at
0.7V was a sharp and high redox peak and the other, at 0.4V was a
weak and broad redox peak. These peaks were attributed to adsorption
and desorption of hydroxide ion on Ag, which follows the reaction:
Fig. 5. CV curves of 5.0mM paracetamol on AgD/GCE at different
scan rates (20mV/s, 50 mV/s,100 mV/s,200 mV/s,400 mV/s). Inset is
the plot of peak current vs square root of scan rate.
S. Dhanush et al. Materials Research Bulletin 100 (2018) 295–301

Fig. 6. (a) Chronoamperometric response of AgD/

GCE electrode for the successive addition of
Paracetamol. (b) Chronoamperometric response of
GAgD/GCE electrode for the successive addition of
Paracetamol.

−
2OHads + 2Ag → Ag2 Osurf + H2 O + 2e− Randles-Sevcik Equation [42],

After the addition of successive concentration of paracetamol, it can 1 1

Ip = (2.99 × 105) n (αna ) 2ACD 2ν
1
2
be seen that the current at edge potential varies significantly and si-
multaneously the cathodic peaks vanish and anodic peaks shifted to- Where, α is the transfer coefficient and na is the number of electrons
wards higher potential. The electrochemical oxidation reaction may involved in the charge
take place in the presence of paracetamol as follows to generate the N-
acetyl – p-quinoneimine in the first step,

Table 1
It is also observed that the anodic current change is significantly Comparison of reported works with different electrochemical platforms for electro-
chemical detection paracetamol.
higher in case of GAgD/GCE than that of AgD/GCE. High electro-
catalytic behaviour of GAgD can be attributed to synergistic effect of Ag Modified Electrode pH used Limit of Linear range Reference
dendrites and presence of graphene sheets [35]. The presence of gra- detection (μM)
phene sheets increases the surface area which leads to better adsorption
C60/GCE 7.2 50 50 μM–1.5mM [43]
of ions, thus facilitating the electrocatalytic reaction [36]. Since gra-
PANI-MWCNT/GCE 5.5 0.25 1 μM–100 μM [44]
phene increases the electronic conductivity, GAgD/GCE shows better C-Ni/GCE 3.0 0.6 2 μM–230 μM [45]
sensitivity than AgD/GCE electrode. Nafion/TiO2- 7.0 0.21 1 μM–100 μM [39]
The effect of scan rates on electrochemical response to paracetamol Graphene/GCE
by AgD/GCE was studied by cyclic voltammetry. The cyclic voltam- SiO2-MWCNT/GCE 7.0 0.098 1.33 μM–4.64 μM [46]
Au-MWCNT/GCE 6.0 0.03 0.09 μM–35 μM [47]
mograms at different scan rates are shown in the Fig. 5. A small shift in Graphene–chitosan 7.0 0.3 1 μM–100 μM [48]
the peak with increase in the scan rate indicates the irreversible reac- (GR–CS)/GCE
tion [39]. The linear fit between the oxidation peak current and the Pd/GO/GCE 6.8 0.002 0.005 μM–0.5 μM [49]
square root of scan rate indicates the diffusion controlled reaction and 0.5 μM–80 μM
b-Cyclodextin/RGO/ 7.0 2.3 10 μM–800 μM [50]
[40,41].The regression equation in AgD/GCE is
GCE
1 1 AgD/GCE 7.0 2.5 2.5 μM–10mM Present work
IP / μA = 0.06106 ν 2 /(mV / S ) 2 + 0.00963 (R = 0.9997) GAgD/GCE 7.0 0.025 0.025 μM–0.5mM Present work
and 0.5mM–10mM
The diffusion coefficient of paracetamol is calculated using the

Fig. 7. Calibration curves for the linear response of

current to the concentration of paracetamol to (a)
GCE/AgD and (b) GCE/GAgD.

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S. Dhanush et al.
Fig. 8. (a). Selectivity test for GAgD/GCE electrode on addition of 0.5mM paracetamol (PM), 0.5mM Ascorbic acid (AA) and 1mM Uric acid (UA). Fig. 8 (b) Repeatability graph of GAgD/
GCE.
The diffusion coefficient of paracetamol in AgD/GCE is found to be
8.366 × 10−6 cm2/s.
3.5.2. Chronoamperometric detection of paracetmol
The Paracetamol detection and response characteristics of the sen-
sors were studied by chronoamperometric (CA) at applied potential of
0.8V. Upon addition of paracetamol into the PBS, modified electrodes
respond quickly (less than 3 s) and the incresase in corresponding cat-
alytic current is observed as a step in Current vs Time graph. Fig. 6 (a)
and (b) show the change in current with respect to the increase in
paracetamol concentration for AgD/GCE and GAgD/GCE respectively.
For the same concentration of paracetamol, increase in current value is
higher in case of GAgD/GCE than that of AgD/GCE.
The sensor shows a linear response when Paracetamol concentration
was varied from 0.5mM to 10mM as shown in the Fig. 7(a and b), and
the current versus concentration graph is fitted with a linear fit. The
regression equations for AgD/GCE and GAgD/GCE are
IP / μA = 1.1234 CP /mM − 0.888 (R = 0.9878) and IP / μ
A = 10.046 CP / mM + 4.856 (R = 0.9992) respectively.
The sensitivity of AgD/GCE and GAgD/GCE are 2.807 × 105μA/
mM/g and 2.511 × 106μA /mM/g respectively. The lower limit of de-
tection of AgD/GCE sensor is calculated to be 2.5 μM and surprisingly a
significant lower value of 0.025 μM with S/N = 3 were obtained for
GAgD/GCE. A comparison of linear range, sensitivity and lower limit of
detection with the reported values are given in Table 1.
3.5.3. Selectivity and repeatability
The selectivity of the modified electrodes were studied using the
chronoamperometry(CA) by adding paracetamol, ascorbic acid and uric
acid at 0.8 V applied potential. The selectivity graph is provided in the
Fig. 8(a). From CA curves we can see that the modified electrodes are
selective towards paracetamol.
The repeatability was tested using five individual modified elec-
trodes to sense paracetamol using chronoamperometry. The modified
electrodes show the good repeatability and the RSD was calculated to
be 3.2%.
4. Conclusions
In summary, we have successfully synthesized Silver dendrites
(AgD) and composite of Silver dendrites-Reduced graphene oxide
(GAgD) by Galvanic replacement method taking Aluminium as sacrifi-
cial element. The electrochemical sensor for Paracetamol was fabri-
cated by coating the synthesized samples on GCE. Chronoamperometric
paracetamol sensor of AgD/GCE exhibits a sensitivity of
2.807 × 105μA/mM/g with a low detection limit of 2.5μA, whereas,
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Materials Research Bulletin 100 (2018) 295–301
GAgD/GCE exhibits a better sensitivity of 2.511 × 106μA/mM/g and a
lower detection limit of 0.025 μM.
(No. SB/S2/CMP-105/2013) project.
Acknowledgements
HSN acknowledges the Government of India for the financial sup-
port through DST-SERB
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