Journal of Inorganic and Organometallic Polymers and Materials

https://doi.org/10.1007/s10904-020-01541-6

Development of Highly Sensitive Ag NPs Decorated Graphene FET

Sensor for Detection of Glucose Concentration
R Archana1 · BS Sreeja1 · KK Nagarajan1 · S Radha1 · P BalajiBhargav2 · C Balaji2 · G Padmalaya1

Received: 8 February 2020 / Accepted: 8 April 2020

© Springer Science+Business Media, LLC, part of Springer Nature 2020

Abstract
In this research work, non-enzymatic FET sensor using silver nanoparticles (Ag NPs) decorated graphene has been fabricated
for the detection of various glucose concentration levels. Graphene was deposited using chemical vapour deposition technique
and Ag NPs was decorated on the surface of graphene via sputtering technique. FET glucose sensor was tested under optimal
conditions (pH 7.4) in linear range 0.1 µM–0.25 µM of glucose concentration levels. It was observed that, developed FET
glucose sensor delivers high sensitivity which was compared with previously reported electrodes. The reproducibility of
FET based glucose sensor was tested using different interfering species along with glucose concentrations. On examining
the behavioural characteristics of FET sensor towards glucose detection it was found to offer a potential device for further
real-time clinical applications.
Graphic Abstract

Keywords FET sensor · Glucose levels · Graphene · Silver nanoparticles · Chemical vapour deposition · Thermal
evaporation technique

* G Padmalaya
padmalayag@ssn.edu.in
1 Introduction
1
Materials and MEMS Laboratory, Department of Electronics
and Communication Engineering, SSN College Diabetes mellitus is one of the most incurable disease in
of Engineering, Kalavakkam, Tamil Nadu 603110, India worldwide and caused by a lack of insulin hormone secretion
2
SSN Research Centre, SSN College of Engineering, in the human body. Improper level of glucose in the blood
Kalavakkam, Tamil Nadu 603110, India

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leads to a number of life-threading conditions resulting lot
of risks such as cardiac problems, nervous problems, stroke,
etc,. In a recent survey, reports show more than 400 million
people are suffered from this disease. Type-1 diabetes (T1D)
is a metabolic disease, which was caused by instable secre-
tion of insulin hormone and that can be managed through
insulin injection. Also T1D individuals suffer from serious
and chronic disorders, such as blindness and tissue damage.
Type-2 diabetes (T2D) results with resistance to insulin and
relative secretion of immune deficiency. These types of dia-
betes suffer from major diseases like heart and kidney stone
problems. Thus, it is necessary to monitor and measure the
blood glucose levels for type 2 based diabetes [1, 2].
With the rising demand glucose plays important role in
day-to-day human metabolism process. It is very impor-
tant to develop high-performance glucose sensors carrying
high sensitivity, stability and low cost found to exhibit most
promising traditional research in medical and healthcare
applications [3, 4]. Among the glucose monitoring sensors,
electrochemical sensor and optical sensors are readily con-
tinuing the research area for glucose sensing applications.
In general, traditional electrochemical sensor uses three
electrodes that involve working electrode, a counter elec-
trode and a reference electrode. For enhancing the practical
requirements, the reference electrode of the sensor needs to
be miniaturized which unavoidably degrades the sensitivity
and stability due to reduction of sensing area [5]. Consider-
ing the traditional electrode criterion, in 1970 the concept
based on ion selectivity FET (ISFET) was introduced for
detecting biomolecules such as penicillin, DNA, proteins,
enzymes, and cells [6–8]. Interestingly, conventional metal
wire electrode is considered as ion-selective electrode (ISE)
which was directly coated using ion-selective membrane
(ISM) such as nanoparticles, carbon nanotubes (CNT), gra-
phene, nanocomposites and nanostructures resulting with the
simpler arrangement, smaller and inexpensive. These FET
sensors using nanomaterials are found to have considerable
attention because of its potential properties such as minia-
turization, parallel sensing, fast response time, high sensi-
tivity and seamless integration with electronic manufactur-
ing processes [9–15]. However, multilayer coating process
using nanomaterials involved with challenging fabrication
procedures.
Among these materials, graphene is found to provide
excellent membrane activity coated on electrode device
(FTO) since their tuneable and unique properties are capa-
ble of providing excellent electronic signals for presenting
novel functions. In addition, graphene is a two-dimensional
hexagonal arrangement of ­sp2 bonded carbon atoms occur-
ring within a carbon material structure. It has an amazing
electronic and a mechanical property that provides excellent
thermal conductivity, zero band-gap, fastest electron mobil-
ity, biocompatible and large surface area so it was used as
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Journal of Inorganic and Organometallic Polymers and Materials
active material in energy harvesting, biomedical and biosen-
sor applications [11, 12, 16, 17]. Moreover, large surface
area and excellent electrical conductivity of graphene allow
it to act as “electron wire” between redox centers of analytes
and electrode surface. These single layer graphene could
provide decreased overlapping band which ultimately has
tendency to act as zero-gap semiconductor so graphene may
be best possible metal for transistor applications [18, 19].
Many nanomaterials have been reported for non-enzy-
matic electrochemical and FET sensors for glucose sensing
applications. Rafiq Ahmad et al. (2017) reported on CuO
decorated ZnO nanorods on non-enzymatic electrochemical
glucose sensor. The nanostructure CuO-ZnO hybrid exhib-
ited on potential outcomes on sensor sensitivity due to their
high surface to volume ratio. The externally modified CuO
has capacity to possess excellent electrochemical and cata-
lytic properties which enables the surface oriented electro-
chemical anodization for glucose detection (glucoseglucono-
lactone) [21]. Jung, Ahmad et al. narrated on non-enzymatic
flexible FET glucose sensor which conveyed enhanced sens-
ing behaviour in different linear range of glucose concentra-
tions. They used NiO QDs-ZnO NRs on Polyimide substrate
that facilitates I­ d–Vg responses for different glucose concen-
trations at room temperature. At high potential, NiO leads to
NiOOH production that assisted in improving the sensor per-
formance [20]. In order to reduce the structural instability of
metal oxides during detection processes they are externally
coated using metal oxides, polymers or metals. Ensaf et al.
described on silver nanoparticle decorated organic function-
alized MWCNTs for non-enzymatic electrochemical glucose
detection. In this, MWCNTs was functionalized with organic
ligands for effective loading of Ag NPs for improved elec-
trochemical performance [22].
It is worth to mention that previous research works
brings into the knowledge on nanostructural modification
with metal oxides or polymers for operative electrochemical
processes that proceeds for glucose and other biomolecules
detection [23, 24]. These metal oxides or polymeric loading
facilitates for effective redox properties for eminent detec-
tion. A significant importance has to be brought into con-
sideration for effortless and impressive progress towards the
sensor performance for glucose detection. For better execu-
tion of FET sensor, Ag NPs decorated graphene was used
as glucose sensor which was reported in this research work
and believed that generation of oxide layer on the surface of
metal NPs has been taken into consideration. This may be
due to the accumulation of biomolecules (analytes) on the
surface of Ag NPs results rendering to metal oxide layer. The
possible generation of metal oxide (AgO) on the graphene
network during the sensing aids in superior performance and
this phenomenon has not reported previously.
To evaluate our research view, silver nanoparticles (Ag
NPs) was employed to provide good conductivity and high
Journal of Inorganic and Organometallic Polymers and Materials
performance for detecting the analytes. In addition, graphene
deposition was carried out on FTO using CVD process and
silver NPs was loaded on graphene using sputtering process
and enabled as glucose monitoring FET sensor. For elec-
tronic FET sensors, silver nanoparticles helps to improve the
surface area in sensitive signal transduction during sensing
process which further helps in evaluating sensing and stabil-
ity behaviours.
2 Materials and Methods
Graphene was grown on Cu foil by using CVD method and
transferred/deposited onto the targeted substrate and the
similar procedure was adopted from reported articles [25].
Aluminium sheet was purchased from Sigma Aldrich with
diameter 3.0 inch*0.125 inches for creating the contacts on
the substrate through thermal evaporation technique. The
structural and morphological analysis of graphene and silver
Nanoparticles deposition was tested using X-ray diffraction
(RigakuMiniflux), Japan and Field emission scanning elec-
tron microscopy (Carl Zeiss SUPRA-55), Germany. Glucose
and Silver nanoparticles was purchased from Sigma Aldrich.
Silver Nanoparticles were sputtered using vacuum coating
unit (model 12A4D), Bangalore.
2.1 Fabrication Procedure for Glucose FET Sensor
and Electrical Measurements
Fabrication procedure for FET sensor was illustrated sche-
matically as shown in Fig. 1. Fluorine-doped tin oxide (FTO)
coated glasssubstrates were washed twice using alkali and
Fig. 1  Schematic representation
for fabrication of developed
FET sensor
concentrated acid solutions. They were dried in hot air oven
under mild temperature. Initially three electrode terminals
such as source drain and gate was taken using aluminium
(Al) using thermal evaporation technique on FTO substrate.
The active surface area was masked before taking the elec-
trode terminals. Then active surface area was coated with
graphene using chemical vapour deposition process.Single
layer graphene with 2 dimensional (2D) extended the coat-
ing with silver nanoparticles (Ag NPs) in order to decorate
the surface of graphene for improving the performance of
FET glucose sensor. 1 gm of Ag NPs powder was made
into pellet form for undergoing sputtering process on the
surface of graphene layer. Ag NPs used on graphene layer
for increasing the sensitivity of the sensor with increased
order of magnitude.
The fabricated glucose FET sensor potential (V) was
measured across drain-source ­(Vds) through the Ag NPs dec-
orated graphene membrane channel as function of applied
gate voltage ­(Vg). The sensing behaviour was measured as
direct current measurements performed with two-terminal
FET having conductive gate. The drain current (­ Id) was
recorded when the device was exposed to different concen-
trations of glucose in the assigned gate voltage ­(Vg) range.
The glucose sensing behaviour was performed at room tem-
perature under optimized conditions to test the operation
performance of non-enzymatic FET glucose sensor. In order
to test the developed FET sensor, an initial assessment has
been made using the available equipment which was shown
in Fig. 2.
13

Fig. 2  Initial testing of developed glucose FET sensor system
Fig. 3  XRD Pattern of the fabricated Ag NPs decorated graphene
FET sensor
3 Result and Discussion
3.1 Structural Analysis
The structural presence of graphene and Ag NPs was con-
firmed using X-Ray Diffraction technique as shown in Fig. 3.
Graphene possess hexagonal carbon structure exhibited at
(002) displayed the wide peak pattern centred at 2ϴ = 25.72˚
which is compared with corresponding data card JCPDS No.
75–1621 [26] and its corresponding d-spacing found to be
­d002 = 3.4Å. The narrow peak at 2ϴ = 38.33˚ (111) denotes
aluminum electrode terminals with d-spacing ­d111 = 2.34Å
and compared with existing data card JCPDS No.85-4148
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Journal of Inorganic and Organometallic Polymers and Materials
[27]. The silver nanoparticles peaks patterns (200), (220)
and (311) corresponding d-spacing d = 2.03Å, 1.44Å, 1.23Å
respectively and their peaks are compared with data card
JCPDS No.04-0783 [28]. The XRD patterns containing Ag
NPs decorated graphene deposition on FTO substrate sup-
ported with sustainable glucose detection.
3.2 Morphological Analysis
The surface morphology of the fabricated device was con-
firmed by Field Emission Scanning Electron Microscopy
(FESEM) as shown in Fig. 4. The images showed the sheet
like structure of graphene material with uniform distribution.
Monolayer graphene sheet can be clearly seen at moderate
and high magnification FESEM images as shown in Fig. 4a,
b respectively. Figure 4c indicated the wrinkled graphene
sheets deposited on Cu foil substrate using CVD method.
The textured graphene sheet deposition decorated with sil-
ver nanoparticles (Ag NPs) on the targeted substrate was
shown in Fig. 4d. These non-enzymatic Ag NPs/graphene
FET sensor found to possess highly interacted super facial
surfaces on the substrate exhibiting high sensing behavioural
performances towards glucose detection.
3.3 FET Sensor Behavioural Characteristics Towards
Glucose Detection
As the concentration of analyte increases on the sensor
interface, the conductivity of the transistor changes accord-
ingly. This happens due to the generation of charges from the
analyte concentration which in turn produces electrostatic
force of attraction. In other words, the degree of depletion
changes within the channel due to the charges from analytes
in the solution [6]. It is worth to mention, the sensitivity of
the electrode increases due to the Dirac voltage shifting and
further increases the conductivity of channel for transporting
the charge carriers for detecting the glucose levels. In addi-
tion, the unique thin film transistor (TFT) (graphene) carry-
ing silver (metal) provides excellent conducting capability
and universal catalytic properties for enhancing the sensor
performance and also helps in promoting possible electronic
movement at the electrode interface.
The sensing behaviour was verified for bare FET and var-
ying glucose concentration levels of developed FET sensor
under room temperature as shown in Fig. 5. The resulting
performance of fabricated FET sensor was examined using
­Id–Vg measurements in 0.1 M of phosphate buffer solution
(PBS) (pH 7.4) for different glucose concentration levels
(0.1 µM–0.25 µM). From the figure, it was also observed
that current generation (charge carriers) was increased for
increasing glucose concentration levels. This may be possi-
bly due to the effect of surface to volume ratio and geometric
effect which further increased the dirac voltage shifting and
Journal of Inorganic and Organometallic Polymers and Materials

Fig. 4  FESEM images of a–c Graphene deposited FET sensor and d Ag NPs decorated graphene FET sensor

conductivity of the developed FET sensor. From the graph

it was also studied that, there is a higher noticeable voltage
shift for higher glucose concentration which was tabulated
inset table in Fig. 5 and happened due to the surface oxidi-
zation of Ag decorated graphene ion selective membrane
(ISM) leading to AgO-graphene production due to reac-
tion with biomolecules (analytes). The possible mechanism
behind the significant sensing behaviour was indicated in
Eq. 1. Further aimed in exposing the state that oxidation of
Ag NPs that have tendency to dissolute as ­Ag+when gets
reacted with oxidizing agents. The ­Ag+metal gets affected by
oxygen that is present in medium and glucose environment.

Fig. 5  FET sensor transfer characteristics towards glucose detection

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 Journal of Inorganic and Organometallic Polymers and Materials

The linear regression curves for varying potential have
been plotted for both bare and treated FET sensor. To
evaluate the sensing behaviour of developed FET sensor,
the average current response were calculated in the range
0.68–1.21 V for each concentration and their corresponding
calibration curve has been plot as shown in Fig. 6.In gen-
eral, graphene has stretchable 2 dimensional (2D) crystalline
form of carbon and helps in providing high degree of flex-
ibility enabling high surface area i.e., 2630 ­m2/g for single
layer graphene thus assists in delivering sensitivity for devel-
oped sensor system [19]. Figure 6a reports the sensitivity of
bare FET sensor was determined to be 2.624 µA/µM ­cm−2.
With increasing the gate voltage levels, their characteristic
electronic behavior was investigated across the drain-source

Fig. 6  Linear plot characteristics of a bare FET and b different glucose concentration levels

Table 1  Sensitivity and limit of S.No Type of sensors developed Sensitivity Linear range LOD References
detection (LOD) comparison of
proposed glucose FET sensor 1 CuNPs/SWCNT/GCE 0.256 mA/mM 5*10–4-0.5 mM 0.3 μM [30]
with previously reported sensors
2 Graphene/FET 0.256 μA/mM – 1.25 mM [31]
0.12 mA/mM – 30 nM [32]
0.5 mA/mM – 0.5 μM [14]
3 CuO NFs/GCE 0.43 mA/mM Upto 2.5 mM 0.8 μM [33]
4 Graphene/CuNPs/GCE 607 μA/mM 5 μM-0.2 mM 200 nM [34]
5 Graphene/Au(metal) – 0.001–1.0 mM 0.03 μM [35]
6 ZnO nanorod FET 1.6 mA/(μM cm2) – – [5]
7 Ag NPs decorated Graphene FET 9.9596 μA/μM 0.1–0.35 μM 0.0262 μM [This Work]

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Journal of Inorganic and Organometallic Polymers and Materials
Fig. 7  Behaviour of the selectivity characteristics of glucose sensor
with different interfering species
current which helps for detection purposes. Then with
increasing the concentration levels of glucose, their sens-
ing behavior was examined across the drain-source current.
It was evidencing from graphene—arrangement of carbon
carries two-dimensional monolayer surface was interfaced
with Ag NPs forming a compatible surface binding capacity
[29] for the detection of glucose molecules.
The linear plot for untreated FET sensor performance was
observed based on current response for different potential
responses and found to empower the sensing behavioural
characteristics of developed transistor. Enhanced sensitiv-
ity performance was observed for difference glucose con-
centration levels treated FET sensor found to be 9.959 µA/
µMcm−2as shown in Fig. 6b. The improved glucose sensor
performance was compared with previously reported sen-
sors as shown in Table1. It was inferred from Table 1 that,
[34] reported using Graphene/Cu NPs/ GCE in linear range
5 μM−0.2 mM with high sensitivity 607 μA/mM indicat-
ing the greater sensing characteristics due to carbon- metal
NPs combinations on GCE. It was noticed that, graphene
excellent support on Cu nanoparticles could provide inspired
detection towards glucose oxidation. Similar interfacial
effect was observed for our glucose sensor and reported in
this research work with extended great performance towards
linear range, sensitivity and stability based properties. More-
over, FET sensor with required surface area deposited using
Ag NPs/graphene helps in facilitating enhanced interaction
between targeted analytes and materials. Thus our glucose
sensor witnessing high sensitivity with small dimensions
enables fast adsorption characteristics towards the analytes
(glucose concentration levels).
3.4 Selectivity Analytical Test
In order to evaluate the selective behaviour of the FET
sensor, their performance was tested using two samples of
PBS solution i.e. sample (a) contains 0.25 µM of glucose
concentration and sample (b) contains 0.25 µM glucose
and low concentration (0.1 µM) of each inferring species
(formaldehyde, melamine and uric acid) as shown in Fig. 7.
The response of a sensor is evaluated using the presence of
glucose as a major contribution of a sample which has to be
added with sample containing a low concentration of inter-
fering species. The interference ions arising from the other
electro-active compounds and oxygen-containing inorganic
species [36, 37] are expected to coexist in the sample solu-
tion. The impact towards the interference ions have slight
decrease in response level due to the inter compounds inter-
action between the existing glucose compound. From our
existing analytical interference data, electroactive species
of glucose and other oxygen containing compounds do not
interfere with the glucose but the stripping current varies
slightly. Supplementary experiments have been performed in
our laboratory and it was observed that, the developed sen-
sor avoids the other compounds (-COOH, -OH). Also it was
noticed to ponder about the behavioural response towards
the electroactive species (glucose) whose potentials found
to be more than 0.6 V and it gets increased for increasing
concentration levels. Thus developed sensor showed signifi-
cant satisfactory effects towards the interfering ions which
helped to proceed for stability tests. In addition to selectiv-
ity behaviour, reproducibility of fabricated FET sensor was
evaluated by repetitive laboratory tests twice a week which
was carried out for 10 weeks. On continuous testing, sen-
sor maintained the response for about maximum weeks of
storage suggesting the developed electrode is flexible with
several environmental measurement conditions.
4 Conclusion
In summary, non-enzymatic glucose based FET sensor using
Ag NPs decorated graphene has been successfully imple-
mented for the detection of glucose concentration levels.
The potential was measured between source-drain terminals
on FTO substrates. The surface modification of Ag NPs on
graphene helps in increasing the surface area for enhanced
glucose sensing. The fabricated sensor showed a wide-linear
range, high sensitivity and low detection limit. The favour-
able selective behaviour towards the glucose concentration
was tested with presence of different interference species.
Furthermore, FET glucose sensor with affordable high per-
formance analytical results helps in potential practical clini-
cal and industrial applications.
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 Journal of Inorganic and Organometallic Polymers and Materials

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