A highly sensitive non-enzymatic glucose sensor based on nickel and multi-walled carbon nanotubes nanohybrid films fabricated by one-step co-electrodeposition in ionic liquids

Article abstract of DOI:10.1016/j.electacta.2012.01.007

In this paper, nickel was combined with multi-walled carbon nanotubes (Ni-MWNTs) to fabricate nanohybrid films on a conventional glassy carbon electrode using simultaneous electrodeposition of NiCl₂ and the MWNTs in ionic liquids (ILs). The morphologies and elemental compositions of the nanohybrid films were investigated with scanning electron microscopy and energy dispersive spectroscopy. A novel non-enzymatic glucose sensor based on the Ni-MWNT nanohybrid film-modified glassy carbon electrode was described, and its electrochemical behaviors were investigated. The proposed sensor exhibited high electrocatalytic activity and good response to glucose. Under optimal conditions, the sensor showed high sensitivity (67.2 μA mM^-1 cm^-2), rapid response time (<2 s) and a low detection limit (0.89 μM; signal/noise ratio of 3). In particular, the upper glucose concentration limit produced a linear response of 17.5 mM. Thus, the Ni-MWNT nanohybrid films represent promising sensor materials for non-enzymatic glucose sensing in routine analyses.

Full text of DOI:10.1016/j.electacta.2012.01.007

Electrochimica Acta 65 (2012) 64–69
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Electrochimica Acta
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A highly sensitive non-enzymatic glucose sensor based on nickel and
multi-walled carbon nanotubes nanohybrid films fabricated by one-step
co-electrodeposition in ionic liquids
Aili Suna,b, Jianbin Zhenga,∗, Qinglin Shenga
a Institute of Analytical Science/Shaanxi Provincial Key Laboratory of Electroanalytical Chemistry, Northwest University, Xi’an, Shaanxi 710069, PR China
b Department of Chemistry and Chemical Engineering, Xinxiang University, Xinxiang 453000, PR China
a r t i c l e i n f o
a b s t r a c t
Article history:
In this paper, nickel was combined with multi-walled carbon nanotubes (Ni–MWNTs) to fabricate
nanohybrid films on a conventional glassy carbon electrode using simultaneous electrodeposition of NiCl2
and the MWNTs in ionic liquids (ILs). The morphologies and elemental compositions of the nanohybrid
films were investigated with scanning electron microscopy and energy dispersive spectroscopy. A novel
non-enzymatic glucose sensor based on the Ni–MWNT nanohybrid film-modified glassy carbon electrode
was described, and its electrochemical behaviors were investigated. The proposed sensor exhibited high
electrocatalytic activity and good response to glucose. Under optimal conditions, the sensor showed
high sensitivity (67.2 ␮A mM−1 cm−2), rapid response time (<2 s) and a low detection limit (0.89 ␮M;
signal/noise ratio of 3). In particular, the upper glucose concentration limit produced a linear response of
17.5 mM. Thus, the Ni–MWNT nanohybrid films represent promising sensor materials for non-enzymatic
glucose sensing in routine analyses.
Received 20 September 2011
Received in revised form 1 January 2012
Accepted 4 January 2012
Available online 11 January 2012
Keywords:
Non-enzymatic glucose sensor
Nanohybrid films
Carbon nanotubes
Ionic liquids
© 2012 Elsevier Ltd. All rights reserved.
1. Introduction
used for the electrochemical oxidation of glucose with a linear-
ity range of 0.2 mM–10 mM and a detection limit of 0.16 mM [9].
The determination of glucose has attracted much attention
due to its significant index in clinical diagnoses, regulation of
metabolism, and biochemical analyses [1–3]. Although previous
studies regarding enzyme-modified electrodes have made some
considerable progress, common and serious disadvantages, such as
rigorous operating conditions, complicated immobilization tech-
niques, chemical instability, and high cost remain [4,5]. Therefore,
the pursuit of non-enzymatic glucose sensors with rapid responses
and precise measurements is a vigorous and competitive area of
research.
In recent years, carbon nanotubes (CNTs) have shown great
potential for use as sensing materials owing to their unique
advantages, including good biocompatibility, enhanced electronic
properties, and rapid electrode kinetics [6,7]. Recently, CNTs have
been successfully combined with nanoparticles and applied to the
fabrication of enzyme-free glucose sensors. Jiang et al. developed
a novel glucose biosensor based on electrodeposition of cupric
oxide (CuO) nanoparticles onto MWNTs arrays [8]. In addition,
Shamsipur et al. demonstrated that a glassy carbon disc elec-
trode modified with MWNTs and nickel (II) oxide (NiO) could be
The methods used to construct this non-enzymatic glucose sensor
were time consuming or technically complex and often involved
surface immobilization, which formed nanoparticles and were
therefore unstable. However, to date, few reports have demon-
strated the one-step electrodeposition of metals combined with
MWNT nanohybrid films to construct non-enzymatic glucose sen-
sors. The reason for this is that MWNTs are largely inert and cannot
disperse well in aqueous solutions, which makes uniform depo-
sition of the MWNTs in the metal composites difficult without the
addition of surfactants or dispersants [10]. Therefore, exploring the
possibilities of finding a compatible conductive solvent that can
simultaneously show good dispersion stability for MWNTs remains
significant.
To the best of our knowledge, MWNTs and NiCl2 form stable dis-
persions in ethaline ionic liquids. Recent studies demonstrated that
composite films synthesized in ILs possessed superior properties
of significantly enhanced electrochemical activity, greater conduc-
tivity, and superior mechanical behavior [11–13]. These methods,
the simultaneous electrodeposition of NiCl2 and MWNTs in ILs, are
simpler and time efficient. Ni–MWNT nanohybrid films have not
been explored in sensor applications and may prove to be a novel
approach for fabricating novel non-enzymatic sensors.
In this study, we present
electrodeposition method to deposit Ni and MWNTs in ionic liquid
a novel, simple, one-step co-
∗
Corresponding author. Tel.: +86 29 88302077; fax: +86 29 88303448.
E-mail address: zhengjb@nwu.edu.cn (J. Zheng).
0013-4686/$ – see front matter © 2012 Elsevier Ltd. All rights reserved.
doi:10.1016/j.electacta.2012.01.007

A. Sun et al. / Electrochimica Acta 65 (2012) 64–69
65
onto a glassy carbon electrode (GCE). A novel non-enzymatic
glucose sensor was constructed based on Ni–MWNT nanohybrid
films for the first time. A comparative study regarding Ni and the
Ni/MWNT-modified electrodes were performed using the same
conditions. The sensors fabricated with Ni–MWNT nanohybrid
films demonstrated enhanced electrocatalytic activity, selectivity
for glucose detection and a wide linearity range.
ethaline. The Ni/GCE was similarly prepared, without the MWNTs.
These modified electrodes were stored at 4 ◦C for further use.
3. Results and discussion
3.1. Ni–MWNTs/GCE characterization
SEM was used to characterize the morphologies of the
Ni–MWNT nanohybrid films. From Fig. 1B, the majority of the Ni
nanoparticles were spherical and clearly had an average diame-
ter of approximately 50 nm. The MWNTs were combined with Ni
for each other and the Ni nanoparticles showed good adhesion to
the MWNT surfaces. The EDS spectrum (Fig. 1C) indicted the pres-
ence of Ni and C. These results demonstrated that the Ni–MWNT
nanohybrid films were successfully electrodeposited onto indium
oxide glass (elements Ca, Si, O and In were detected due to the
indium oxide glass).
The mechanism of electrodeposition was previously described
[16]. Firstly, nickel cations could be reduced and generated as Ni
nanoparticles on the GCE under cathodic polarization. Secondly,
the well-dispersed MWNTs that were close to the Ni nanoparti-
cles were deposited on it and entrapped as individual nanotubes
or aggregates. Then, increasing amounts of nickel cations were
electrodeposited onto the Ni nanoparticles and also onto the incor-
porated MWNTs. Finally, increasing amounts of the MWNTs were
deposited along with the Ni nanoparticles and were then pro-
gressively linked together to form the Ni–MWNT composites. The
electrodeposition process of the nanohybrid films is shown in
Scheme 1.
Previous studies have revealed that the electrocatalytic activ-
ity of Ni-constructed electrodes for glucose oxidation was based
on the formation of a nickel oxyhydroxide surface film [17]. To
reach a stationary state before being used for glucose detection
measurements, the Ni–MWNT nanohybrid films were explored in
an aqueous solution containing 0.1 M NaOH by 50 consecutive CV
scans over the potential range of +0.0 V to +0.8 V at a scan rate of
0.1 V s−1. From Fig. 2, both the anodic and cathodic current densi-
ties progressively increased after consecutive potential-sweeping
cycles. Changes in the peak current density were likely due to the
changes in the crystal structures of the nickel hydroxide and nickel
oxyhydroxide [18,19].
2. Experimental
2.1. Reagents
Multi-wall carbon nanotubes (MWNTs, >95% purity) were pur-
chased from Chengdu Organic Chemicals Co. Ltd. Prior to use, the
MWNTs were treated with concentrated nitric acid to introduce
carboxylic acid groups according to Ref. [14]. NiCl2·6H2O was dried
in a vacuum oven at 120 ◦C for 24 h. Sodium hydroxide, ethylene
glycol, choline chloride, glucose, l-ascorbic acid (AA), uric acid (UA)
and all other chemicals were of analytical grade and were used
without further purification. Distilled water was used in all exper-
iments.
2.2. Apparatus
All of the electrochemical experiments were performed using a
CHI660D electrochemical workstation (Shanghai Chenhua Instru-
ment Co. Ltd., China) using a three-electrode system. A silver–silver
chloride electrode (Ag/AgCl) as reference electrode (SCE), a plat-
inum wire electrode as the auxiliary electrode, and a modified
glassy carbon electrode (GCE) as the working electrode. All the
potentials given in this paper were referred to the SCE. Scanning
electron microscopy (SEM) and energy dispersive spectroscopy
(EDS) images were acquired with a JEOL JEM-3010 (JEOL, Japan)
high-resolution transmission electron microscope using an accel-
erating voltage of 200 kV.
2.3. Preparation of the nanohybrid films coated electrode
2.3.1. Nanohybrid film-coated electrode preparation
The ionic liquids, ethaline, were synthesized according to pre-
vious work [15] with a slight modification. Briefly, ethylene glycol
and choline chloride (2:1) were heated while stirring constantly for
20 min until a homogeneous, colorless liquid formed. Prior to use,
a GCE (˚ = 4 mm) was polished with 0.3-␮m and 0.05-␮m alumina
slurries to obtain a mirror-like surface and was then ultrasoni-
cally and thoroughly cleaned in ethanol and water. The material
was then allowed to dry at room temperature. Ten mg of the acid-
treated MWNTs and 3.0 mmol NiCl2 were ultrasonically dispersed
within 10 mL ionic liquid ethaline for 30 min to obtain a homo-
geneous black-blue solution. Then, stable dispersions of MWNTs
and NiCl2 in ionic liquids were used for the electrodeposition of
the Ni–MWNT nanohybrid films. The potential for multiple cyclic
voltammetry (CVs) experiments ranged from 0.0 V to 1.6 V (vs. SCE)
with a scan rate of 20 mV s−1 and scan number of 20, similar to
previously reported [16]. The resulting electrode was washed with
distilled water. The effect of the Ni–MWNT nanohybrid film elec-
trodeposition cycles on the electrochemical response of glucose
was investigated after injecting the same amount of glucose under
the same condition. As a result, the peak current changed with the
cycles. At 20 cycles, the peak current reached its maximum. Thus,
the optimal cycles for further studies were selected in 20 cycles.
For comparison, a Ni/MWNT/GCE was prepared as follows: 5 ␮L
(1 mg·mL−1) of MWNTs were delivered to a cleaned GCE surface
and dried with air; Ni was then electrodeposited in ionic liquid
3.2. Electrocatalytic oxidation of glucose
The electrochemical responses of the Ni–MWNT/GCE films were
further investigated with the scan rates (v) ranging from 0.1 V s−1
to 1.4 V s−1, and the results are shown in Fig. 3. The peak current
was proportional to the square root of the scan rate (Fig. 3, inset)
with a linear regression equation of Ipa (␮A) = −75.37 − 440.1 v1/2
(m V1/2
(m V1/2
s
s
−1/2) (n = 14, r = 0.9992) and Ipc (␮A) = 71.98 + 239.0 v1/2
−1/2) (n = 14, r = 0.9989). These results indicated that the
electrochemical kinetics signified a diffusion-controlled process
rather than a surface-controlled process at these scan rates, which
is an ideal case for quantitative analyses in practical applications.
Meanwhile, the cathodic and anodic peaks shifted to high poten-
tials, and the peak currents shifted to lower values with the increase
in scan rates. These results were due to the nucleation of NiO(OH)
and the following increase of activation sites (Ni2+ or Ni3+) [20–24].
Ni(OH)2 + OH− → NiO(OH) + e− + H2O
Applied potential strongly affects the amperometric response of
a biosensor. To improve the performance of the sensor, the effect
of the applied potential on the response current of the sensor is
illustrated in Fig. 4. When the applied potential was increased from

66
A. Sun et al. / Electrochimica Acta 65 (2012) 64–69
Fig. 1. (A) SEM images of MWNT and (B) Ni–MWNT nanohybrid films, and (C) EDS analyses of Ni–MWNT nanohybrid films.
Scheme 1. An illustration describing the electrodeposition process of modified electrodes.

A. Sun et al. / Electrochimica Acta 65 (2012) 64–69
67
150
200
100
0
b
a
0
-150
-300
a
e
-100
-200
0.2
0.4
0.6
0.8
1.0
E/V (vs. Ag/AgCl)
0.0
0.2
0.4
0.6
0.8
Fig. 2. CVs of the Ni–MWNT/GCE films in 0.1 M NaOH at 0.1 V s−1 after (a) 1 and (b)
50 consecutive CVs.
E/V (vs. Ag/AgCl)
Fig. 5. CVs of the Ni–MWNT/GCE films at different concentrations of glucose: (a)
0.0, (b) 0.5, (c) 1.0, (d) 2.0, (e) 3.0 mM in 0.1 M NaOH.
500
n
in the oxidation peak currents and decreases in the cathodic peak
currents. These results indicated that glucose had been oxidized by
the active Ni–MWNT nanohybrid films via a cyclic mediation redox
process. The reason that the anodic peak potential shifted to a high
potential might be attributed to the diffusion limitation of glucose
at the electrode surface [25]. The current deviated from linearity at
higher glucose concentrations, most possibly due to the passivation
of the electrode and formation of glucose isomers, which is known
to occur in alkaline media [26]. The mechanism of electrocatalytic
oxidation of glucose due to the existence of Ni(II) ions are described
with the following reactions [27]:
250
a
0
600
300
-250
0
-300
-600
-500
0.4
1/2
0.8
1.2
/
V1/2 s-1/2
Ni(OH)2 + OH− → NiO(OH) + e− + H2O
0.0
0.4
0.8
E/V (vs. Ag/AgCl)
NiO(OH) + glucose → Ni(OH)2 + glucolactone
Fig. 3. CV responses of the Ni–MWNT/GCE films at various scan rates in 0.1 M NaOH.
Scan rates (from a to n): 0.1, 0.2, 0.3, 0.4 0.5, 0.6, 0.7, 0.8, 0.9, 1.0, 1.1, 1.2, 1.3 and
1.4 V s−1, respectively. The inset represents the plots of Ipc and Ipa vs. scan rates.
The inset represents the corresponding calibration curve at (a)
Ni–MWNT/GCE, (b) Ni/MWNT/GCE and (c) Ni/GCE modified glucose
sensors.
0.80V
-60
80
0.70V
80
a
-40
-20
0.60V
0.50V
60
60
b
40
a
20
c
40
b
0
0
3000 6000 9000
/( M)
0.40V
400
0
C
Glucose
20
c
100
200
300
Time/s
0
Fig. 4. Steady-state current–time responses of the Ni–MWNT/GCE films to 0.01 mM
glucose in 0.1 M NaOH at various potentials.
0
400
800
1200
Time/s
1600
2000
0.4 to 0.8 V, very little current was observed at an applied potential
0.4 V; however, a large increase was observed from 0.5 to 0.7 V.
Therefore, 0.6 V was selected as the optimum applied potential for
the amperometric detection of glucose in subsequent studies.
The electrochemical oxidation of glucose was investigated in
0.1 M NaOH at the modified electrodes using CVs. As shown in Fig. 5,
increased glucose concentrations induced apparent enhancements
Fig. 6. Amperometric responses of (a) Ni–MWNT/GCE, (b) Ni/MWNT/GCE and (c)
Ni/GCE modified electrodes stirring in 0.1 M NaOH after successive glucose additions
at an applied potential of 0.60 V. The inset represents the corresponding calibration
curve at (a) Ni–MWNT/GCE, (b) Ni/MWNT/GCE and (c) Ni/GCE modified glucose
sensors.

68
A. Sun et al. / Electrochimica Acta 65 (2012) 64–69
Table 1
Performances of the different glucose biosensors.
Electrode
LR
2 ␮M–2.5 mM
100 ␮M–2.5 mM
0.5 ␮M–5 mM
DL
Sensitivity
Stability
References
NiCFP electrode
Nickel electrode
Ni powder modified electrode
NiO/MWCNTs electrode
Ni nanoparticle modified carbon paste electrode
Au/MNE
1 ␮M
3.30 ␮A mM−1
–
[28]
[21]
[29]
[30]
[31]
[32]
This work
0.04 mM
0.2 ␮M
2 ␮M
0.3 ␮M
0.5 ␮M
0.89 ␮M
–
–
–
40 ␮A mM−1 cm−2
1768.8 ␮A mM−1 cm−2
–
10 ␮M–7 mM
1.0 ␮M–1.0 mM
100 ␮M–3.0 mM
3.2 ␮M–17.5 mM
1 week
3–20 days
30 days
2978 ␮A mM−1 cm−2
67.19 ␮A mM−1 cm−2
Ni–MWNTs
NiCFP, Ni nanoparticle-loaded carbon nanofiber paste; NiO, nickel(II) oxide; MNE, mesoporous nickel electrodes; LR, linearly range; DL, detection limit.
Fig. 6a shows a typical current–time sensor curve at a constant
potential of +0.6 V after the addition of successive glucose in stir-
ring 0.1 M NaOH. A comparative study of injecting the same amount
of glucose was conducted by fabricating three types of different
modified sensors under the same conditions, using Ni–MWNT/GCE,
Ni/MWNT/GCE and Ni/GCE films (Fig. 6a–c, respectively). The
amperometric response curves demonstrated that the Ni–MWNT
nanohybrid film-modified electrodes presented well-defined, sta-
ble and rapid amperometric responses within 2 s and that the
sensitivity was higher than that of the Ni/MWNT/GCE and Ni/GCE
films. The Ni–MWNT/GCE films better performed the Ni/GCE films,
proving that the MWNTs have greatly improved the sensitivity of
the electrode. At the same time, when using the Ni/MWNT/GCE
films as a control, the results showed that the one-step electrode-
position of metal combined with MWNT nanohybrid films is better
than the traditional drop-coating of MWNTs with metal. Thus, the
sensors that were constructed with a one-step electrodeposition of
metal combined with MWNT nanohybrid films demonstrated bet-
ter performance. Meanwhile, the calibration curve for the glucose
sensor at the Ni–MWNT/GCE was generated and shown in Fig. 7.
The sensor displayed a linear range from 3.2 ␮M to 17.5 mM glucose
with a linearly regression equation of I (mA) = 4.16 + 0.0081 Cglucose
(␮M) (R2 = 0.9954, in Fig. 7B) and detection limit of 0.89 ␮M (sig-
nal/noise = 3). The linear range for glucose determination at the
Ni–MWNT nanohybrid film-modified electrode was comparable
and even better than previously reported non-enzymatic glucose
sensors [21,28–32]. The results are summarized in Table 1. The
wider linear ranges could be explained as follows. Firstly, ionic liq-
uids were used as solvents. MWNTs are inert and cannot disperse in
water. The traditional method is to drop carbon nanotubes or film-
forming materials to disperse carbon nanotubes onto electrodes.
The method used to construct the sensor were time consuming
or technically complex. However, MWNTs and NiCl2 can disperse
in ILs. Thus, one-step co-electrodeposition in ionic liquid can be
achieved. MWNTs can then serve as effective sites to facilitate the
electrodeposition process and nickel matrix reinforcement, which
makes the Ni–MWNT nanohybrid films more stable. Meanwhile,
direct electrodeposition without using an immobilization matrix
offers close contact of the Ni–MWNT nanohybrid films, which is
also aids in rapid and sensitive catalytic performance. Secondly,
Ni–MWNT nanohybrid films that are electrodeposited in ILs possess
potential features, such as enhanced hardness, protection against
corrosion and catalytic performance. Finally, the large surface and
roughness on the surface of Ni–MWNT nanohybrid films, which
is a desirable material for a sensor, also provides more reaction
sites.
proposed sensor was responsible for good selectivity towards the
detection of glucose.
The reproducibility of the sensor was determined by conducting
eight successive amperometric measurements of 2.0 mM glucose
with a modified electrode. The relative standard deviation (R.S.D.)
of the reproducible current was 4.2%. The experimental results
confirmed that the electrode was not poisoned by the oxida-
tion products and was highly reproducible. The batch-to-batch
reproducibility was estimated from the current responses of six
different sensors toward 2.0 mM glucose, and an RSD of 4.5% was
obtained, indicating that the proposed method was reliable. The
long-term stability is also a significant parameter for evaluating the
A
120
4.0
4 M
3.6
80
8 M
3.2
200 M
0
400
800
1200
40
0
Time/s
20 M
0
500
1000
1500
2000
2500
Time/s
B
120
80
40
0
Oxidizable compounds, such as AA and UA, typically co-exist
with glucose in physiological fluids on different electrodes, espe-
cially on non-enzymatic glucose sensors [33]. According to normal
values (physiological), the interference effect of 0.1 mM AA and
0.1 mM UA on the amperometric response of 1 mM glucose was
studied. At this level, the current responses produced by AA and DA
were 0.21 ␮A and 0.23 ␮A, only 3.81% and 4.18% when compared to
that of glucose (5.5 ␮A), respectively. The results showed that the
0
5000
10000
15000
C
/( M)
Glucose
Fig. 7. (A) Amperometric responses of the Ni–MWNT/GCE films to increasing the
glucose concentrations with an applied potential of 0.60 V. (B) The corresponding
calibration curve at the Ni–MWNT/GCE films.

A. Sun et al. / Electrochimica Acta 65 (2012) 64–69
69
Table 2
Determination of glucose in human plasma samples by the proposed sensor.
Samples
Measured (mM)
Added (mM)
Measured (mM)
Recovery (%)
1
2
3
4
5.65
5.61
5.56
5.62
2.00
2.50
3.00
4.00
7.62
8.20
8.61
9.70
98.5
103.6
101.6
102.0
performance of the sensor. A response current of 0.2 mM glucose
was determined each week. The results showed that the response
current was 95% of its initial value after 30 days, which indicated
that the stability of the sensor was very good.
The applicability of this glucose biosensor was performed after
determining the glucose concentration in real samples, utilizing
both the calibration curve and standard addition method. The
recovery of glucose was testified using the standard addition
method with three times the addition of pure glucose to solutions
containing serum samples. The results showed that the sensor pro-
duced recoveries in the range of 98.5–103.6%, indicating that the
as-prepared Ni–MWNT nanohybrid films hold great potential in
real sample analyses (Table 2).
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In this paper, novel Ni–MWNT nanohybrid films were prepared
by the one-step electrodeposition of Ni and MWNTs in ILs and were
successfully applied to fabricate a non-enzymatic glucose sensor
for the first time. Meanwhile, the experimental results showed that
this sensor exhibited rapid responses and a wide linearly range (up
to 17.5 mM) when compared to most of the existing non-enzymatic
glucose sensors. The high electrocatalytic activity likely raised from
the specific large surface area of the Ni–MWNT nanohybrid films.
Thus, the present sensors were suitable for glucose determination
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