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Controllable synthesis of silver nanodendrites on

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copper rod and its application to hydrogen peroxide

Cite this: CrystEngComm, 2013, 15,
1173 and glucose detection3
Xiaojun Zhang,*ab Rong Ji,ab Lingling Wang,ab Liutao Yu,ab Jie Wang,ab
Baoyou Gengab and Guangfeng Wang*ab

Received 6th August 2012,
Accepted 22nd November 2012
DOI: 10.1039/c2ce26255j
www.rsc.org/crystengcomm
Silver nanodendrites were synthesized on Cu rods by a simple and facile displacement reaction without
using any surfactants. The morphologies were investigated by scanning electron microscopy (SEM). The
phase analysis of the dendritic nanostructure was revealed by X-ray diffraction (XRD). The element analysis
was characterized by energy dispersive X-ray spectroscopy (EDS). Then a novel Ag nanodendrites/Cu rod
electrode (named Ag NDS/CRE) based non-enzymatic hydrogen peroxide (H2O2) and glucose (GO) sensor
was fabricated and evaluated by cyclic voltammetry (CV) and typical amperometric response (I–t) method.
Exhilaratingly, the electrode shows significant electrocatalytic activity toward the reduction of H2O2 and
oxidation of GO. Its advantage lies in its wide linear range from 0.2 mM to 19.2 mM for the detection of
H2O2 with a low detection limit of 0.1 mM (S/N = 3) and also has a good response for GO with a linear
range from 0.02 mM to 7.4 mM with the optimized detection limit of 0.1 mM (S/N = 3). The response time
of the proposed electrode is less than 3 s. What’s more, the proposed sensor displays excellent selectivity,
good stability, and satisfying repeatability.

Introduction temperature or surfactants; some reductants are toxic like

Silver nanomaterials have attracted extraordinary attention
due to their remarkable physicochemical properties and
numerous applications,1,2 particularly in catalysis and electro-
catalysis. To date, many morphologies of nano-silver have
been obtained, for instance, nanocubes,3,4 nanoplates,5,6
nanowires,3,7,8 nanorods,9,10 nanoparticles11,12 and so on.
Among various specific nanostructures, dendritic silver struc-
tures receive attention because of their large surface area,
which provides good connectivity and makes them useful in
diverse applications such as biosensors, chemical sensors,
plasmonics and superhydrophobic films13–18 and dendritic
materials with self-assembled hierarchical and repetitive
superstructures.19–21 Recently, many methods have been
reported to obtain silver nanodendrites by electrochemical,
chemical, and physical means, such as electrochemical
metallic deposition,16,22–24 wet-chemical route,25,26 micro-
wave-assisted method,27 and so forth. However, most synthetic
methods have been reported to need reductants, high
a
College of Chemistry and Materials Science, Anhui Key Laboratory of Chem-
Biosensing, Anhui Normal University, Wuhu, 241000, P. R. China
b
Key Laboratory for Functional Molecular Solids of the Education Ministry of China,
Wuhu, 241000, P. R. China. E-mail: zhangxiaojun173@yahoo.com.cn;
Fax: +86-553-3869302; Tel: +86-553-3937138
3 Electronic supplementary information (ESI) available. See DOI: 10.1039/
c2ce26255j
sodium borohydride, which are not only harmful to the
laboratory technician but also to the environment. Hence, a
method of facile operation, precise control, low cost and
environmental-friendliness is highly desirable. Herein, we
report a simple and low-cost route to synthesise silver
nanodendrites and the effects of the concentration of reagent
(AgNO3) as well as the reaction time have been investigated in
some detail.
Diabetes is a disease where blood glucose is vulnerable to
excessive accumulation. It is known as a ‘‘silent killer’’,
especially adult-onset diabetes. Men in their forties are
affected with a very high rate (accounted for 10%) in Japan
and suffering from diabetes will reduce the lifespan due to
complications throughout the body, so we need to detect the
excessive glucose in blood as early as possible and control the
concentration in time. Up to now, H2O2 has obtained
considerable interest in the accurate determination as well
as GO because it is widely used in modern medicine,
environmental control, and various branches of industry.
Electrochemical sensing of H2O2 and GO28–37 has had
considerable attention because of its low cost, high sensitivity,
easy operation, and high efficiency. It is well know that
conventional electrodes are nanomaterial-modified glass
carbon electrodes, but it is waste of time and the nanomater-
ials on electrode can easily fall off.

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Paper CrystEngComm

In this paper, we report a simple method to synthesize

silver nanodendrites on Cu rod and it is used as an electrode
directly. The electrode can be regenerated effectively without
extra treatment under the hydrodynamic condition, and it
indicates good reproducibility. We study the electroreduction
ability toward H2O2, to our great surprise, it has ultralow
detection limit of 0.1 mM (S/N = 3) compared with a previous
report.38 The electrooxidation ability of GO also demonstrated,
and showed excellent performance, so the silver nanoden- Fig. 1 Typical SEM image of the dendritic Ag nanostructure.
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drites can be potentially used in some novel electrochemical

sensors and other electronic devices.
Experimental section
Chemicals and apparatus
AgNO3, Cu rod, NaOH, ascorbic acid (AA) and dopamine (DA)
were purchased from the Sinopharm Chemical Reagent Co.,
Ltd. (Shanghai, China). Phosphate buffer solution (PBS, pH
7.0, 0.1 M) was prepared by varying the ratio of KH2PO4 to
K2HPO4. GO was purchased from Sigma. All chemicals are
analytical grade and used as received without any further
purification. Millipore water was used in all experiments.
The morphologies of the products were studied by using
Hitachi S-4800 scanning electron microscopy (SEM) and a
field-emission transmission electron microscope (FE-TEM,
Philips, Tecnai G2 F20) equipped with an energy-dispersive
X-ray spectroscopy analyzer. X-ray powder diffraction (XRD)
patterns of the as-prepared materials were recorded on a
Shimadzu XRD-6000 employing a scanning rate of 0.05u s21
with the 2h range from 10u to 80u, with high-intensity Cu KR
radiation (l) 0.154178 nm. Cyclic voltammetry (CV), ampero-
metric experiments and scanning rates were performed on a
model CHI 760D electrochemical analyzer (CHI, Instruments,
Shanghai, China) coupled to a computer.
Synthesis of the silver nanodendrites on Cu rod
A Cu rod (cross-section = 2.5 mm2, L = 4 cm) was cleaned by
consecutive ultrasonication in acetone, ethanol and distilled
water, the bottom of Cu rod was immersed in 0.05 M AgNO3
for 50 s, the product was then washed with distilled water and
ethanol several times to remove the impurities before
characterization.
Electrochemical measurements
Electrochemical signals were measured and recorded with a
CHI760D potentiostat–galvanostat electrochemical worksta-
tion. The electrode was put into the three-electrode cell to
characterize its electrochemical properties. Coiled Pt wire
electrode and Ag/AgCl (saturated with KCl) were applied as the
auxiliary and reference electrode, respectively, Ag NDS/CRE as
working electrode was put into a cell with 5 mL of 0.1 M
phosphate buffer solution (PBS, pH = 7) to check the
electroreduction ability to H2O2. The CV scanning rate was
set to be 50 mV s21. The amperometric curves were obtained
after adding a certain concentration of H2O2 with the solution
stirred constantly. We also do the same experiments in a cell
with 0.1 M NaOH to check the electrooxidation ability to GO.
Results and discussion
Preparation and characterization of silver dendritic structures
The product obtained with 0.05 M AgNO3 for 50 s was
characterized by SEM. It is clearly seen that the Ag dendrites
have a long main trunk with short side branches all decorated
by small leaves and have a large output, the overall length of
the dendrite is about 3–8 mm (see Fig. 1a and 1b). The identity
and crystal structure of the Ag nanodendrites were verified by
XRD analysis. All the major diffraction peaks can be indexed to
the monoclinic Ag phase with lattice constants according to
the reported date (JCPDS Card 75-1532) (see Fig. 2a). The
element analysis of our materials was further characterized by
EDS technique, as can be seen in the Fig. 2b, showing the
peaks of Ag appear at about 3 KeV, confirming that the
products have a ‘‘clean’’ surface and these nanostructures are
composed only of pure silver (C and Cu peaks can be assigned
to the carbon film Cu grid).
We also investigated the relationship between the morphol-
ogy of the silver nanostructures and various reaction para-
meters including the silver ion concentration and reaction
time which is highly determining of the product’s morphology,
since it controls the speed of the growth of nanostructures (see
Table 1). As we can seen in the Fig. 3, for the product obtained
with 0.001 M AgNO3 for 240 s, the density of the depositions is
thicker but the morphology is irregular. When the reaction
time becomes shorter, the density of the depositions is thinner
with irregular morphology. When the concentration increased
to 0.01 M, the SEM images of the product under different
periods are clearly illustrated in Fig. 4. The sample obtained at
5 s is shown in Fig. 4a and 4b, where it could be seen that the
deposition is made up of nanoparticles with thinner thickness
and irregular morphology. At 10 s (see Fig. 4c and 4d), the
Fig. 2 (a) XRD pattern of the Ag nanodendritic nanostructure, (b) EDS of the Ag
nanodendritic nanostructure.

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Table 1 Summary of various morphologies of Ag nanostructures fabricated at

different experimental conditions

Ag+ concentration (M) Time (s) Morphology

0.001 240 Fig. 3a and 3b

0.01 5 Fig. 4a and 4b
0.01 10 Fig. 4c and 4d
0.01 50 Fig. 4e and 4f
0.01 120 Fig. 4g and 4h
0.05 5 Fig. 5a and 5b
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0.05 10 Fig. 5c and 5d

0.05 50 Fig. 1a and 1b
0.05 120 Fig. 5e and 5f
0.1 5 Fig. 6a and 6b
0.1 10 Fig. 6c and 6d
0.1 50 Fig. 6e and 6f
0.1 120 Fig. 6g and 6h

depositions became thicker, but there are very few dendrites

that could be observed. When the reaction time is further
increased to 50 s (see Fig. 4e and 4f), a small amount of
dendritic structures with well-defined morphology are pro-
duced. When the reaction time is extended up to 120 s (see
Fig. 4g and 4h), some particles started to grow on the branch,
which lead to transform the dendritic structures.
The typical SEM images of the samples obtained at different
periods using the affirmative concentration of AgNO3 (0.05 M)
are shown in Fig. 5. A large number of particles and some Fig. 4 Typical SEM images of Ag nanostructures obtained at different periods: (a
and b) 5 s, (c and d) 10 s, (e and f) 50 s, and (g and h) 120 s with silver ion
trunks are observed at 5 s (see Fig. 5a and 5b). When the time
concentration of 0.01 M.
increases to 10 s (see Fig. 5c and 5d), the coexistence of
particles and dendritic structures is exhibited and the amount
of dendritic structures is increased. Fig. 1a and 1b shows high
density yet regular dendrites when the time is 50 s. With the surface diffusion of adatoms. Subsequent free Ag atoms will be
reaction time increased to 120 s, the side branches become captured to form dendrites under an appropriate concentra-
shorter and the dendrites are out of shape (see Fig. 5e and 5f). tion (0.05 M).
It is also studied when the concentration of AgNO3 increased
to 0.1 M. Fig. 6 shows the coexistence of particles and
dendrites at 5 s (see Fig. 6a and 6b) as well as 10 s (see Fig. 6c
and 6d), where dendrites tend to be larger with the increase of
time. At 50 s (see Fig. 6e and 6f) and 120 s (see Fig. 6g and 6h),
the branches have become shorter and particles accumulate
on it. It is demonstrated that a homogeneous morphology
cannot formed when the silver ion concentration is too high
due to the quick reaction rate.
Based on the experiments above, a possible formation
process is speculated. AgNO3 is rapidly reduced to form Ag
adatoms (Agu) via replacement reaction. Silver nucleus will
then formed at random positions on Cu rod because of the

Fig. 5 Typical SEM images of Ag nanostructures obtained at different periods: (a

Fig. 3 Typical SEM image of product obtained with 0.001 M AgNO3 for 240 s. and b) 5 s, (c and d) 10 s, (e and f) 120 s with silver ion concentration of 0.05 M.

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Fig. 6 Typical SEM images of Ag nanostructures obtained at different periods: (a
and b) 5 s, (c and d) 10 s, (e and f) 50 s and (g and h) 120 s with 0.1 M AgNO3.
Electrochemical experiments
In order to evaluate the Ag dendrites as an electrode material
for practical applications, we studied the electroreduction
ability of the Ag NDS/CRE toward H2O2 and the electrooxida-
tion ability of GO in aqueous solution. In all electrochemical
experiments, Ag NDS/CRE obtained with the silver ion
concentration of 0.05 M at 50 s was used as working electrode
without any modification. Fig. 7 shows the contrastive
photograph of a bare Cu electrode (see Fig. 7a) and Ag NDS/
CRE (see Fig. 7b). As a test of the good electrocatalytic
properties of the Ag nanodendrites, cyclic voltammetry (CV) is
a useful tool to characterize the sensing behavior. As shown in
Fig. 8a, it exhibits an obvious cathodic current increment for
Ag NDS/CRE and the peak appears near 20.3 V, which is due
to the reduction of H2O2. However, the response of H2O2 for
Fig. 7 Photograph of bare Cu rod (a) and Ag NDS/Cu rod (b) which used as
working electrode.
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Fig. 8 (a) CV images for Ag NDS/CRE and bare Cu at different concentrations of
H2O2 in 0.1 M pH 7.0 PBS at a scan rate of 50 mV s21. (b) CV images for Ag NDS/
Cu and bare Cu in 0.1 NaOH at various concentrations of GO. The scan rate was
50 mV s21.
the bare Cu rod electrode was weak. These results are
demonstrating the catalytic effects of the Ag NDS/CRE toward
the reduction of H2O2 efficiently. As for Fig. 8b, we can see that
the current increased with increasing the concentration of GO
to Ag NDS/CRE. At the same time, the response for bare Cu rod
is so weak that it can be ignored. Therefore, Ag NDS/CRE also
has good catalytic effects toward the oxidation of GO. The
related material, Ag nanoparticles, was compared to the
prepared Ag dendrite electrode, which is shown in Fig. S1,
ESI.3 It is clearly shown the Ag dendrite electrode has a better
response than others.
Amperometric responses of the Ag NDS/CRE and bare Cu
rod electrode were measured at an applied potential of 20.3 V
in a continuously stirred 7.0 PBS solution. With the H2O2
added into electrolyte, the response is recorded, shown in
Fig. 9A. For the bare Cu electrode (see Fig. 9A curve b), a
detectable but comparatively small current response is
Fig. 9 (A) Typical amperometric response of Ag NDS/CRE (a) and bare Cu (b) to
successive injection of H2O2 into 0.1 M pH 7.0 PBS with stirring, the working
potential was 20.3 V, inset is the response of 0.1 mM H2O2; (B) corresponding
calibration curve and linear plot of response current vs. H2O2 concentration; (C)
typical amperometric response of Ag NDS/CRE (a) and bare Cu (b) to successive
injection of GO into 0.1 M NaOH with stirring, the working potential was 0.6 V,
inset is the response of 0.1 mM GO; (D) corresponding calibration curve and
linear plot of response current vs. GO concentration.
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observed with the addition of H2O2. In contrast, the Ag NDS/
CRE responds sensitively to the changes of H2O2 concentra-
tion, reaching a steady-state signal within 3 s (see Fig. 9A curve
a). The corresponding calibration plots for the two ampero-
metric response curves are shown in Fig. 9B. The sensitivity of
Ag NDS/CRE is 273.3 mA mM21, which is 6 times than that of
bare Cu electrode (45 mA mM21). The amperometric responses
of the Ag NDS/CRE and bare Cu electrode upon successive
addition of GO to 0.1 M NaOH at an applied potential of 0.6 V
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are shown in Fig. 9C, Compared with the bare Cu rod
electrode, the Ag NDS/CRE is more sensitive to GO. The
calibration plots of the sensor under the optimized experi-
mental conditions is shown in Fig. 9D, The linear response of
Ag NDS/CRE corresponds to an ultrahigh value of 728.2 mA
mM21, in contrast to bare Cu electrode where the sensitivity is
very weak (21.4 mA mM21), which is much better than some
reported work39–48 (see Tables S1 and S2, ESI3). The Ag NDS/
CRE responds sensitively both toward H2O2 and GO, which
could be due to the excellent catalytic activity of Ag dendrites
and their large surface areas.
In order to demonstrate the function of the dendritic
morphology, we compare the Ag NDS with an ordinary Ag
electrode in the terms of the electrochemical and electro-
catalytic behaviors under the same conditions (see Fig. S2,
ESI3). According to the following equation:
n2 F 2 vACc
IP ~
4RT
where Ip was the peak current, A was the electrode surface area,
the other symbols had their usual meanings, the surface coverage
concentration tc for NDS/CRE was calculated to be 2.77 6 1028
mol cm22, and the Ag electrode was 0.32 6 1028, which indicated
that NDS/CRE possess a much larger surface coverage than the Ag
electrode, so NDS/CRE has bigger area to come into contact with
the test.
The influence of scanning rates on the cyclic voltammogram
response of the Ag NDS/CRE in 7.0 PBS was also evaluated and
the results are displayed in Fig. 10a. It can be seen that the Ag
NDS/CRE redox peak current rises with an increase of the scan
rates and the scan rates ranging from 50 to 150 mV s21.
One of the most important analytical factors for an
amperometric biosensor is the selectivity of the sensor to the
target analyte. Here, we investigated interferences from AA, DA
Fig. 10 (a) CVs of Ag NDS/CRE electrode in 7.0 PBS at different scan rates. (b)
Amperometric response for successive injection of 0.01 mM H2O2 and
interfering species (0.1 mM AA, 0.1 mM DA, 0.1 mM L-Cys) into 7.0 PBS with
stirring, the working potential was 20.3 V.
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and L-cysteine (L-Cys) toward the determination of H2O2 as
they are common existing interfering species in physiological
samples. The interfering effect of 0.1 mM AA, 0.1 mM DA and
0.1 mM L-Cys compared to 0.01 mM H2O2 was evaluated at the
potential of 20.1 V. As shown in Fig. 10b, there is obvious
current response with the addition of 0.01 mM H2O2. On the
contrary, no obvious current response is observed with the
addition of 0.1 mM AA, the same applies after 0.1 mM DA, and
0.1 mM L-Cys being consecutively added, demonstrating that
interference from the interfering species was completely
avoided.
The reproducibility and stability of the sensor was evaluated.
Five Ag NDS/CRE were made and their current responses to 0.1
mM glucose were investigated. The relative standard deviation
(RSD) was 4.22%, confirming that the fabrication method was
highly reproducible. Five successive measurements of 0.1 mM
glucose on one sensor yielded an RSD of 3.59%, demonstrat-
ing that the sensor was stable. The long term stability of the
sensor was evaluated by measuring its sensitivity to 0.1 mM
glucose within a 30 days period. The sensor was stored in air at
ambient conditions and its sensitivity was tested every 10 days.
Conclusions
Silver dendrites have been synthesized on Cu rod by a method
of facile operation, precise control, low cost and friendliness
towards the environment without introducing any surfactant.
The density and the morphology of the Ag nanostructures can
be easily controlled by changing reaction parameters, such as
precursor concentration and reaction time. Satisfyingly, the Ag
NDS/CRE could not only respond sensitively to H2O2 and GO
but also effectively avoid interference from common interfer-
ing species such AA and DA. High sensitivity, excellent
selectivity, good stability and repeatability give it potential
for future development of H2O2 and GO sensors.
Acknowledgements
This work was financially supported by National Natural
Science Foundation of China (20901003, 20971003, 21073001
and 21005001), the Key Project of Chinese Ministry of
Education (209060), Anhui Provincial Natural Science
Foundation (1208085QB28), Natural Science Foundation of
Anhui (KJ2012A139) and the Program for Innovative Research
Team at Anhui Normal University.
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