Journal of Alloys and Compounds 694 (2017) 1061e1066

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Journal of Alloys and Compounds

journal homepage: http://www.elsevier.com/locate/jalcom

Fabrication and characterization of graphite oxide e nanoparticle

composite based field effect transistors for non-enzymatic glucose
sensor applications
Khadija Said a, Ahmad I. Ayesh b, *, Naser N. Qamhieh a, Falah Awwad c,
Saleh T. Mahmoud a, Soleiman Hisaindee d
a
Department of Physics, United Arab Emirates University, Al Ain, P.O. Box: 15551, United Arab Emirates
b
Department of Mathematics, Statistics and Physics, Qatar University, Doha, P.O. Box: 2713, Qatar
c
Department of Electrical Engineering, United Arab Emirates University, Al Ain, P.O. Box: 15551, United Arab Emirates
d
Department of Chemistry, United Arab Emirates University, Al Ain, P.O. Box: 15551, United Arab Emirates

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

Article history: Graphite-oxide based field-effect transistors (FETs) were fabricated and used as glucose sensors. Herein,
Received 9 August 2016 graphite-oxide was assembled between two electrical electrodes. The sensitivity of the sensor has been
Received in revised form enhanced by adding copper (Cu) and silver (Ag) nanoparticles. The nanoparticles were produced by
16 October 2016
sputtering and inert-gas condensation inside an ultra-high compatible system, and self-assembled on the
Accepted 17 October 2016
graphite-oxide. The sensitivity of the sensor was increased by an order of magnitude when the silver
Available online 18 October 2016
nanoparticles were added, while the low concentration could be detected more sensitively by adding
copper nanoparticles. The sensitivity of each FET was studied at different concentrations of non-
Keywords:
Field-effect transistor
enzymatic glucose for potential use in medical and industrial applications.
Graphite oxide © 2016 Elsevier B.V. All rights reserved.
Graphene
Sensors
Non enzymetic glucose

1. Introduction detection including electrochemical, fluorescent, acoustic, trans-

Recent reports highlighted that 20% of the world population are
affected by diabetes, thus, monitoring and diagnosis of diabetes are
highly demanded [1]. The development of sensitive and selective
glucose sensors with low power consumption and reliable cost has
been investigated rigorously recently [2]. Those sensors have many
applications in fields related to food safety, medical diagnostics,
and biotechnology [3]. Previous research efforts were focused on
fabrication of glucose sensors that are based on detecting glucose
oxide because of their high sensitivity [4]. Nevertheless, those
sensors suffer from a major selectivity issue since the sensors are
greatly affected by factors related to the surrounding environment
including humidity, temperature, and pH [5]. Therefore, sensors
that are based on non-enzyme glucose represent a reliable
alternative.
Different potential methods were investigated for glucose
* Corresponding author.
E-mail address: ayesh@qu.edu.qa (A.I. Ayesh).
dermal, and optical techniques. However, conductometric glucose
sensors have received great attention because of their enhanced
sensitivity and selectivity, as well as their low production cost
[2,6e8]. Herein, metal, metal-oxide, and alloy nanoparticles were
utilized as the sensitive part for non-enzyme glucose [9e14]. Yet,
many of those nanoparticles suffer from practical issues such as
their toxicity, low selectivity, slow kinetics, as well as poisoning
with chloride [15].
Graphite consists of hexagon layer sheets, where carbon atoms
in graphite layers are held together by covalent bonds. They are
intercalated by various atoms and molecules due to the weak
interaction of van der Waals forces [16]. The partial oxidation of
graphite produces graphite-oxide (GO) where oxygen atoms are
grouped on the edges of graphite and in the middle of planes. GO
has unique chemical, electronic, and structural properties such as
high mobility at room temperature that make it attractive for the
fabrication of various micro-electrical devices [17e19]. Therefore,
glucose sensor that include GO and nanoparticles would have
modified electrical properties that cause signal enhancement
[20e22]. Field effect transistor (FET) is an important type of

http://dx.doi.org/10.1016/j.jallcom.2016.10.168
0925-8388/© 2016 Elsevier B.V. All rights reserved.
1062 K. Said et al. / Journal of Alloys and Compounds 694 (2017) 1061e1066
transistors that is used for switching or amplification [23]. It can be
utilized for sensor applications were the sensor signal is repre-
sented as the drain current (ID) at a constant gate to source voltage
(VGS) [24].
In this work, graphite-oxide based FETs are fabricated, and used
as non-enzymatic glucose sensors by utilizing the variation of GO
resistivity when it is exposed to different concentrations of non-
enzymatic glucose. Moreover, detecting low concentration from
non-enzymatic glucose solution is facilitated using graphite oxide
devices decorated with (Cu and Ag) nanoparticles to enhance their
sensitivity [25]. The nanoparticles are produced by the inert-gas
condensation technique since it is a novel technique that pro-
duces nanoparticles of high quality [25]. Copper and silver are
classified as good electrical conductors at low potential. In addition,
the large surface-volume ratio and (chemical/physical) properties
of Cu and Ag nanoparticles play an important role in the interaction
and absorption of chemical species for glucose sensor applications
[26].
2. Experimental
Fig. 1 shows a schematic diagram for a FET based on graphite-
oxide that has been fabricated and used as a glucose sensor. The
device is based on a commercial heavily doped p-type silicon wafer
with 300 nm SiO2 top layer. The wafers were cleaned first with
acetone, then with ethanol, and finally with deionized water, fol-
lowed by a drying process using drayed nitrogen gas. Electrical
contact electrodes were deposited by thermal evaporation of ~5 nm
thick layer of NiCr and then on top of it ~50 nm layer of Au through
a shadow mask [27]. The lower NiCr layer was used for better
adhesion of the electrodes with the wafer [28]. The wafer was then
diced into a proper size (1 cm
0.5 cm), and cleaned again.
Graphite oxide was synthesized from graphite using a modified
Hummers method [29]. 5.00 g of graphite and 2.50 g NaNO3 were
mixed with 120 mL of concentrated H2SO4 in a 500 mL flask. The
mixture was stirred for 30 min in an ice bath, and 15.0 g potassium
permanganate (KMnO4) was added, in portions, to the suspension
under vigorous stirring. The rate of addition was carefully
controlled to keep the reaction temperature below 20  C. After
addition was completed, the mixture was stirred overnight at room
temperature and then 150 mL of H2O was slowly added under
vigorous stirring. The suspension was further stirred at 98  C for
6 h. The mixture was cooled and 50 mL of 30% H2O2 was slowly
added to destroy excess KMnO4. The mixture was centrifuged, and
the residue was washed several times with 5% HCl and then with
deionized water. After filtration and drying under vacuum, 5.80 g of
solid graphite oxide was obtained [30]. Finally 5 mg/mL of graphite
oxide was prepared by grinding 5 mg in 1 mL of distilled water and
then exposed to the sonication for 45 min.
A 0.05 mL droplet of the solution was dropped between the gold
electrodes on the SiO2/Si substrate, and the device is left to dry for
24 h at room temperature. The resistance of the device was
Fig. 1. Schematic diagram of a graphite oxide based FET.
measured during the deposition process of graphite-oxide solu-
tions using an electrometer (Keithley 617) to confirm the estab-
lishment of percolation path(s). The doped Si substrate was used as
a bottom gate of a field effect transistor. The current-voltage (IeV)
measurements were measured to characterise the device using a
computer-controlled Keithley 236 source measuring unit [31]. The
source measuring unit was also used to measure the variation of
electrical current upon exposure to glucose for the sensitivity ex-
periments. To prepare glucose solution for sensor test, glucose
powder was diluted in distilled water to form solutions with
different concentrations of glucose. Moreover, different nano-
particles such as Ag and Cu were deposited on the surface of
graphite-oxide to enhance their sensitivity [25]. Copper and silver
nanoparticles were fabricated using magnetron sputtering and
inert-gas condensation inside an ultrahigh vacuum compatible
system (UHV) [32,33]. The base pressure in the system can reach
10-8 mbar by using a dry-rotary and two turbo pumps. Cu and Ag
metals with a purity of 99.99% were used as targets, individually,
and fixed on the sputter head. Argon gas with 99.999% purity was
used to generate the plasma and also for nanoparticles condensa-
tion. It was found that the size of nanoparticles produced by this
method is proportional to the fabrication parameters such as argon
flow rate and sputtering discharge power [34]. For both Cu and Ag
nanoparticles' production the argon gas flow rate used was 60
sccm. The power discharge used for sputtering to produce Cu and
Ag nanoclusters were 97.47 W and 115.41 W, respectively. The
thickness of deposited nanoparticles was measured using a quartz
crystal monitor (QCM) placed next to the graphite-oxide/Si/SiO2
sample. The thickness of nanoparticles was fixed to 2.5 nm for
each nanoparticle type. The distance between the target and the
outlet nozzle of the source (aggregation length) was 40 mm. Be-
sides the graphite-oxide/Si/SiO2 wafers, nanoparticles were
deposited on glass and TEM grides to be used for nanoparticles'
characterization. Herein, electron dispersive spectroscopy (EDS)
was performed for elemental analysis. X-ray diffraction (XRD) using
a Shimadzu 6100 X-ray diffractometer (XRD) with Cu-Ka radiation
(l ¼ 1.5406 Å) has been performed to study the structure and size of
the nanoparticles. The nanoparticles were imaged by scanning
electron microscopy (SEM), and the nanoparticles size has been
determined using transmission electron microscopes (TEM).
3. Results and discussion
Fig. 2 shows the transmission electron microscope (TEM) image
and size distribution of silver nanoparticles (Ag-NPs). TEM image
shows relatively spherical shape of silver nanostructures. These
nanostructures are either individual or agglomerations of nano-
particles (the dark spheres). The TEM image was used to determine
nanoparticle size distribution, where the diameter of each indi-
vidual nanoparticle is the average of the major and minor elipps
diameters. The size distribution of Ag-NPs is in the diameter range
of 2 nme7 nm as shown in Fig. 2(b), and the average diameter of
Ag-NPs is around 7 nm. While the TEM image and the size distri-
bution of Cu-NPs produced is shown in Fig. 3. Also the relatively
spherical shape appears for Cu-NPs as shown in the TEM image of
Fig. 3(a). The figure shows more aglomration of nanoparticles
compared with that of Ag-NPs due to the higher density of nano-
particles. From Fig. 3(b), the average diameter of Cu-NPs is around
6 nm and mostly the large size of copper nanoparticles were ranged
from 5 nm to 9 nm.
The energy dispersive spectroscopy confirmed the existence of
both elemental silver and copper nanoparticles as illustrated in
Fig. 4(a) and Fig. 5(a), respectively. The same figures show also the
amount of mass percentage for silver nanoparticles, about 0.75%,
while for copper nanoparticles the mass percentage was about
 K. Said et al. / Journal of Alloys and Compounds 694 (2017) 1061e1066
Fig. 2. (a) TEM image of Ag nanoparticles. (b) Size distribution of Ag nanoparticles.
2.62%. Silicon, carbon, oxygen and other elements appeared due to
the sputtering nanoparticles on the glass substrate that was used
for the EDS analysis. The insets of the figures show SEM images of
the nanoparticles and they reveal aglomration of the nanoparticles.
XRD measurement analysis the composition of the produced Ag
and Cu nanoparticles as illustrated in both Figs. 4(b) and 5(b),
respectively. The corresponding angles are 2q1 ¼ 38.1375,
2q2 ¼ 43.9316, 2q3 ¼ 64.3226, and 2q4 ¼ 77.445 represent the
peaks of face centered cubic (fcc) at (111), (200), (220), and (311)
planes related to the Ag-NPs in Fig. 4(b), as discussed in referance
[35]. While the corresponding angles for Cu-NPs are 2q1 ¼ 43.9877,
2q2 ¼ 64.3527, and 2q3 ¼ 77.4711 represent the peaks of face
centered cubic peaks at (111), (200), and (220) planes as shown in
Fig. 5(b), and it is well agree with the data of referance [36].
XRD measurements can be used to calculate the average nano-
particle size (D) using Scherrer's equation:
kl
D¼
bcosq
Where k is a dimensionless constant related to the shape of
nanoparticles, and it is taken 0.94 in the present calculations since
the nanoparticles are almost spherical [37], l is the wavelength of
X-ray, b is the full width at half maximum of an X-ray peak, and q is
the Bragg's angle.
1063
Fig. 3. (a) TEM image of Cu nanoparticles. (b) Size distribution of Cu nanoparticles.
Realizing the average spherical size of nanoparticles is per-
formed using Scherrer's equation at the diffraction peak (200) and
(111) for Ag-NPs and Cu-NPs, respectively, that have the highest
intensities. The average size is equal to 14.2 ± 2.3 nm for Ag-NPs,
while it is 15.7 ± 2.5 nm for Cu-NPs. The overestimation of nano-
particle size compared with the results obtained from the TEM
images can be assigned to the agglomeration of nanoparticles in the
samples prepared for the XRD measurements (where sample
thickness for XRD experiments is ~100 nm). It should be noted that
the Williamson-Hall's method was also found to further over-
estimate nanoparticle size.
Fig. 6 shows ID-VDS characteristics at different gate voltages for
a graphite oxide FET. The drain source voltage varies from
VDS ¼ 40 to 40 V, and the measurements were performed at room
temperature. The curves are nonlinear and ID increases with
increasing VDS for each value of VGS. Moreover, the n-type nature
of charge carriers in the conducting channel between the drain and
(1) the source explains the effect of varying VGS on the ID-VGS curves.
Decreasing the value of VGS leads to a reduction in the density of
conducting charge carriers (electrons) in the channel, and conse-
quently to a decrease in the drain current ID. Eventually, when the
value of VGS becomes negative electrons are depleted from the
channel leading to a reduction in the channel conductivity. The
positive gate voltage abundances the density of conducting
1064 K. Said et al. / Journal of Alloys and Compounds 694 (2017) 1061e1066
Fig. 4. (a) EDS spectrum that reveals the composition of the produced Ag nano-
particles. The inset is an SEM image of the Ag nanoparticles. (b) XRD spectrum of Ag
nanoparticles.
electrons in the channel and enhances the channel conductivity,
and consequently the drain current ID.
The sensitivity of graphite oxide to non-enzymatic glucose is
tested by measuring the current ID (at a constant VDS) and moni-
tors the change in its value when exposed to glucose. A typical
measurement is shown in Fig. 7. The gate voltage VGS ¼ 0 V and
VDS ¼ 0.1 V, the current started at Imax ¼ 3.01
10-5 H. 189 A.
When the graphite oxide is exposed to 30 mM non-enzymatic
glucose solution at time t ¼ 3.9663 s, a sharp drop in the current
is observed and reach a value about Imin ¼ 0.32
10-5 H. 185 A
Imin ¼ 1:27E  5 A. a then it becomes nearly constant. Neverthe-
less, since the values of Imax and Imin are device dependent, the
value of the change in current (DI) was used to determine the
sensitivity of the fabricated graphite oxide sensor to glucose using:
DI ¼ Imax  Imin
The test was repeated for different concentrations of glucose,
Fig. 5. (a) EDS spectrum that reveals the composition of the produced Cu nano-
particles. The inset is an SEM image of the Cu nanoparticles. (b) XRD spectrum of Cu
nanoparticles.
from 1 mM to 30 mM, in the solution and the data is plotted in Fig. 8.
The curve shows that the sensitivity of the sensor increases with
increasing the glucose concentration with an abrupt increase at
about 1 mM glucose concentration. The comparative sensitivity
between GO and GO/Cu-NPs shows that the sensitivity increases by
adding Cu nanoparticles on GO. It's worth noting that the sensi-
tivity of the sensor has been increased sharply by adding Ag-NPs on
the top of GO as shown in the same figure. According to the TEM
images, the average size of Ag nanoparticles is larger than that of Cu
nanoparticles that tend to the small size particles [38]. The figure
shows that sensors based on GO and Cu-NPs are more suitable for
detection of low concentrations of glucose. Cu nanoparticles can be
easily a container to the functional group of oxygen in GO [39]. Also,
the spherical shape of Cu nanoparticles provides active surface for
the oxidation of glucose and large specific surface area for further
reactive cites. The minimum sensitivity of the GO/Cu-NPs sensors is
(2)
1 mM which is good compared to previously published results for
GO based sensors [4,8,20e22]. The reproducibility was tested to
 K. Said et al. / Journal of Alloys and Compounds 694 (2017) 1061e1066
Fig. 6. ID-VDS characteristics for the graphite oxide gate measurements.
Fig. 7. Change in the current (DI) at 30 mM non-enzymatic glucose.
three devices of each type, and similar trend was obtained. It
should be noted that further may be conducted to investigate the
selectivity of the current sensors. Moreover, low cost, high sensi-
tivity, wide range detection, high electrochemical reactions, fast
Fig. 8. Change in the current (DI) at different concentrations of non-enzymatic glucose
solution for GO, GO/Cu-NPs, and GO/Ag-NPs.
1065
electron transfer at low potential, and easy chemical - physical
interaction with the glucose solution [25], support the choice of
GO/Cu-NPs for non enzymetic glucose sensor at low concentrations
compared with GO/Ag-NPs. This can be rationalized since Ag
nanoparticles are classified as weak to detect low concentration of
glucose [39].
4. Conclusions
Graphite oxide based on field-effect transistors (FETs) were
fabricated. IeV measurements revealed n-type nature of charge
carriers in the conducting channel of the FETs. The positive gate
voltage increases the density of conducting electrons in the channel
which promotes the channel conductivity, and consequently the
drain current ID. The graphite-oxide FETs were used for sensing
glucose concentration in a solution with low concentration as low
as 1 mM. Adding different Cu and Ag nanoparticles (NPs) have
enhanced the sensor's sensitivity with better performance for the
sensor based on graphite oxide and Cu at low glucose concentra-
tions. The beneficial properties of using GO/Cu-NPs are that they
have good reproducibility, stability, instantaneous with low
detection sensitivity at about 1 mM, and wide range detection from
1 mM to 30 mM. Those sensors are promising and their sensitivity
can be further enhanced by testing different nanoparticle systems
which promotes their utilization for practical field applications.
Acknowledgment
This work is financially supported by UAEU-SQ grant with
number 31S085 and UAEU grant with number 31R006.
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