Sensors & Actuators: B.

Chemical 309 (2020) 127832

Contents lists available at ScienceDirect

Sensors and Actuators B: Chemical

journal homepage: www.elsevier.com/locate/snb

Real time detection of Hg2+ ions using MoS2 functionalized AlGaN/GaN T

high electron mobility transistor for water quality monitoring
Adarsh Nigama, Neeraj Goela, Thirumaleshwara N Bhatb, Md. Tawabur Rahmanc,
Surani Bin Dolmananb, Qiquan Qiaoc, Sudhiranjan Tripathyb, Mahesh Kumara,*
a
Department of Electrical Engineering, Indian Institute of Technology Jodhpur, Jodhpur 342037 India
b
Institute of Materials Research and Engineering, A*STAR (Agency for Science, Technology and Research), Innovis, 2 Fusionopolisway, 138634 Singapore
c
Department of Electrical Engineering and Computer Science, South Dakota State University, Brookings, South Dakota 57007, United States

A R T I C LE I N FO A B S T R A C T

Keywords: A sensor for highly sensitive, selective, and rapid determination of the trace amount of toxic Hg2+ ions is
AlGaN/ GaN HEMT developed for the first-time using molybdenum disulfide (MoS2) functionalized AlGaN/GaN high electron mo-
MoS2 bility transistor (HEMT). The vertically aligned, flower-like MoS2 structures are synthesized through a simple
Hg2+ions hydrothermal route and applied on the gate region of AlGaN/GaN HEMT. The scanning electron microscopy,
Sensitivity
Raman spectroscopy, and X-ray diffraction are performed for structural characterization of MoS2. Further, the
Selectivity
sensing of Hg2+ ions is performed by electrical characterizations of MoS2 functionalized AlGaN/GaN HEMT. The
sensor showed an excellent sensitivity of 0.64 μA/ppb and detection limit of 0.01152 ppb with the rapid re-
sponse time of 1.8 s. The sensor exhibits the linear range of detection from 0.1 ppb to 100 ppb and highly
selective behavior towards Hg2+ ions. The results demonstrated that the MoS2 possess excellent Hg2+ ions
capture property, that could be attributed to the complexation of Hg2+ ions with sulfur and the electrostatic
interaction between MoS2 and Hg2+ ions alters the drain to source current (IDS) of the HEMT at a constant drain
to source voltage (VDS). Therefore, the MoS2 based AlGaN/ GaN HEMT devices have a huge potential for next-
generation ion sensing applications.

1. Introduction
Mercury (Hg) has been recognized as one of the most known toxic
metal as its trace amount also potentially dangerous. It causes both the
chronic and acute poisoning, and excessive exposure causes some se-
vere health problems such as irreversible neurological damage, cancer,
and motion disorders that can lead to death also [1,2]. To prevent the
toxicity of Hg2+ ions in water, the concentration of Hg2+ ions should
be below the guideline values of WHO (1 ppb), and EPA (2 ppb) [3,4].
Thus, it is necessary to monitor mercury at trace levels in the drinking
water and other water bodies rapidly and efficiently.
The significant efforts have been made for the detection of the
mercury at trace levels by various analytical approaches. These
methods include optical analysis like colorimetric, and spectroscopic
techniques [3,5], electrochemical techniques such as amperometry, and
voltammetry [6,7]. These approaches show good sensitivity but are
expensive, time-consuming complicated, and laboratory-based ap-
proaches, which requires specific operators for analysis [8]. Methods
like ion-selective electrodes (ISE) using gold (Au) as an electrode have
advantages that they can provide higher sensitivity and good detection
limit for different ion sensing applications. However, these Au elec-
trodes need a specific configuration, a filling solution, and a reference
electrode. This configuration limits its extensive use in the ion sensing.
The Si-based ion-sensitive field-effect transistors (ISFETs) were utilized
to solve the portability and robustness problems related to Au elec-
trodes [9]. However, the chemical instability in ionic solutions and the
necessity of the reference electrode not only limits the performance of
the Si-ISFETs but restricts the miniaturization of the device as well [10].
AlGaN/GaN HEMTs with its superior material characteristics like
higher chemical and thermal stability, wide bandgap, and piezoelectric
and spontaneous polarization properties provides an efficient way for
the development of the AlGaN/ GaN HEMT based ion sensors. AlGaN/
GaN HEMTs possess two-dimensional electron gas (2DEG) at the het-
erointerface of AlGaN and GaN, due to their spontaneous and piezo-
electric polarization properties [11]. The presence of 2DEG at the
channel region makes the device normally on, which makes it a re-
ference electrode free device and favors further miniaturization of the
device. In comparison to Si-ISFETs, AlGaN/GaN HEMTs have several

⁎
Corresponding author.
E-mail address: mkumar@iitj.ac.in (M. Kumar).

https://doi.org/10.1016/j.snb.2020.127832
Received 28 November 2019; Received in revised form 20 January 2020; Accepted 5 February 2020
Available online 05 February 2020
0925-4005/ © 2020 Elsevier B.V. All rights reserved.
A. Nigam, et al.
advantages. In enhancement mode Si-ISFETs, a reference electrode is
required to provide gate potential above the threshold voltage to form a
channel, whereas the AlGaN/GaN HEMTs can efficiently work as re-
ference electrode free devices. The depletion-mode Si-ISFETs possess
very less mobility and carrier concentration compared to AlGaN/GaN
HEMTs; therefore, the AlGaN/GaN HEMT based ion sensors can provide
100 times better performance than Si-ISFETs [12]. Moreover, the
electron density at 2DEG is highly sensitive for any change at the gate
region compared to Si-ISFETs. Hence, the AlGaN/GaN HEMTs have
superior advantages over other ion sensors to attain excellent sensitivity
and miniaturization without reference electrode utilization.
The AlGaN/GaN HEMTs were used as chemical and biosensors for
the detection of various elements such as glucose, prostate-specific
antigens, and ions like mercury, cadmium, and nitrate [10,13–15].
These sensors showed rapid response time with excellent sensitivity at
trace level. Therefore, some studies for Hg2+ ion detection were also
carried out using AlGaN/GaN HEMT based sensors. Wang et al. com-
pared bare Au and the Au with thioglycolic acid functionalization on
AlGaN/GaN HEMTs to detect Hg2+ ions and achieved fast response
time below 5 s and 27 ppb detection limit for Hg2+ ions [13]. Asadnia
et al. reported polyvinyl chloride (PVC) functionalized AlGaN/GaN
HEMT sensor to detect Hg2+ ions observed the limit of detection of
10−8 M [10]. Besides this, Chen et al. utilized the AlGaN/GaN HEMT
for detection of low concentration of Hg2+ ions using the thioglycolic
acid-functionalized gate and have observed a good limit of detection of
1.5 × 10-8 M, a magnitude lower than their previous work (10-7 M to
10-8 M) [11,13]. This lower detection of Hg2+ ions is required for many
applications. These reports suggest the vast applicability of AlGaN/GaN
HEMTs for Hg2+ ion detection.
In the last few years, MoS2, a transition metal dichalcogenide has
got much attraction owing to its distinct electrical, optical, chemical,
and mechanical properties such as tunable bandgap and high surface to
volume ratio [16]. So far, several research groups have synthesized
MoS2 by different processes like mechanical exfoliation [17], chemical
vapor deposition [16], sulfurization of Mo or MoO3 [16,18], and hy-
drothermal process [19,20] and prepared several morphologies of MoS2
in the form of different micro and nanostructures [16,20,21] for the
widespread sensing applications [17,22]. Among different micro and
nanostructures of MoS2, the three-dimensional (3D) micro and nanos-
tructures such as flowers and flower-like structures have received much
attention because of their unique structural properties. There were
several nanosheets gathered together to form the flower-like structures,
which can increase the number of adsorption sites on the sensing sur-
face and results in the enhanced sensitivity of the sensors for different
sensing applications [20]. Moreover, the remarkable advantages of
flower-like structures have plenty of active edges that play a prominent
role in electrochemical reactions [23]. In addition, the higher catalytic
activity was also observed in flower-like structures compared to basal
plane MoS2 films, which can improve the sensitivity of the sensors [24].
Some research groups also observed the applicability of MoS2 in Hg2+
ions detection. Jia et al. demonstrated MoS2 as an excellent adsorbent
of Hg2+ ions to remove them from water and showed adsorption stu-
dies of Hg2+ ions on natural MoS2 using atomic force microscopy
(AFM) [25,26]. Aswathi et al. reported solvent exfoliated synthesis of
MoS2 for Hg2+ ion sensing by an electrochemical route and observed
ultra-low-level detection of Hg2+ ions [22]. Liu et al. explains the de-
tection of Hg2+ ions by MoS2 nanosheet as fluorescent probes with
boron and nitride doping [27]. These reports showed the suitability of
MoS2 for low level Hg2+ ion detection.
In this work, a simple hydrothermal synthesis was carried out for
the preparation of MoS2. Furthermore, for the first time, this MoS2 was
drop cast on the gate region of AlGaN/GaN HEMT to use it as a func-
tionalizing material to sense Hg2+ ions in aqueous solutions. Hence, a
simple, novel, highly sensitive and selective MoS2 functionalized
AlGaN/GaN HEMT sensor was developed for Hg2+ ions detection
without the need of reference electrode.
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Sensors & Actuators: B. Chemical 309 (2020) 127832
2. Experimental details
2.1. Materials
The materials utilized here are Molybdenum (VI) oxide (MoO3),
Thiourea (CH4N2S), NaOH, for the hydrothermal process of MoS2. The
NaH2PO4, Na2HPO4 were used here for the preparation of phosphate
buffer solution. Other reagents such as Hg(NO3)2.H2O, Cr(NO3)3.9H2O
CuSO4, Cd(NO3)2.4H2O, Ni(NO3)2.6H2O, Zn(NO3)2.6H2O, Pb(NO3)2
were employed for the development of ionic solutions of respective
metals for sensing analysis.
2.2. Synthesis of MoS2
The synthesis of MoS2 was carried out by the simple hydrothermal
process. In this process, MoO3, NaOH, and CH4N2S were used as pre-
cursor materials in the ratio 0.6:0.2:2 g respectively. The homogenous
solution of these materials was prepared by mixing them in the pre-
scribed ratio in 40 ml DI (deionized) water through continuous stirring
for 1 h. The stirred mixture was moved in 50 ml Teflon lined hydro-
thermal autoclave and heated at 200 °C for 24 h. By this method, a black
colored solution was obtained and rinsed many times by DI water.
Further, this black colored product was centrifuged. Due to cen-
trifugation, the black precipitates were settled on the ground. These
precipitates were filtered and then dried at 80 °C till 1 h in the oven.
This process results in black colored MoS2 powder.
2.3. Measurements and characterization
The crystalline nature and phases of the MoS2 were examined using
X-ray diffraction approach (XRD) on X-ray diffractometer. The MoS2
morphologies were identified using field emission scanning electron
microscopy (FESEM) of Tecnai G2 20 (FEI) S-Twin. Further, the vibra-
tional spectrum of the MoS2 was observed by performing the Raman
spectroscopy. After the functionalization of MoS2 on the gate region of
AlGaN/GaN HEMT, the electrical characterizations were performed
using Keithley-4200 semiconductor characterization system. The de-
tection of the Hg2+ ions was observed by performing a similar process,
as explained in our previous report [14]. In this work, the range of
Hg2+ ion concentration was used from 0.1 ppt to 10 ppm for experi-
mental analysis. The phosphate buffer solution (PBS buffer) was uti-
lized for the preparation of Hg2+ and other heavy metal ion solutions.
The pH of the solutions was kept constant at 7.
3. Results and discussion
In order to detect Hg2+ ions at different concentrations, a stock
solution of Hg2+ ions of 100 ppm was prepared by adding 2.56 mg Hg
(No3)2.H2O in 15 ml phosphate buffer solution. The stock solution was
diluted for different solution range by using solution dilution equation:
M1V1=M2V2 (1)
Where M1, V1 represent the concentration and volume of stock solution
respectively, and M2 and V2 represent the desired concentration and
volume of the required solution, respectively. This equation estimates
the volume of stock or higher concentration solution that should be
added in the solvent to realize a specified concentration solution of
Hg2+ ions. By utilizing the Eq. (1), solutions of different of the Hg2+
ions from 10 ppm to 0.1 ppt were prepared. The concentration of as-
prepared solutions was verified by performing atomic absorption
spectroscopy (AAS) on three different concentrations of Hg2+ ions
(0.1 ppb, 1 ppb, and 10 ppb), and the results were shown in Table 1.
The analysis reveals the good agreement between as-prepared solutions
and AAS measurement, and hence the solution preparation procedure
of the different concentrations of Hg2+ ions has been verified.
A. Nigam, et al.
Table 1
Concentration analysis of Hg2+ ions.
Concentration of Hg2+ ions in as prepared Concentration observed by AAS
solutions (ppb) (ppb)
0.1 0.103
1 1.061
10 10.049
3.1. Preparation of MoS2 functionalized AlGaN/GaN HEMT ion sensor
The HEMT fabrication process was described in detail in our earlier
reports along with structural analysis [28,29]. For the contact forma-
tion on AlGaN/GaN HEMT, the drain and source terminals were fab-
ricated by the deposition of Au (200 nm) /Cr (30 nm)/Al (150 nm)
metals. The metal stack was further patterned by optical lithography to
form the drain and source contacts. The separation between source and
drain was 100 μm. Further, the annealing of these contacts was per-
formed (850 °C, 60 s). Then, the source and drain contacts were en-
capsulated by Si3N4. For this process, the silicon nitride (Si3N4) with
250 nm thickness was deposited using RF sputtering process, which is
further patterned by photolithography. Since the adhesiveness of Au is
very poor on the GaN surface, thus a thin film of Ni has been deposited
prior to Au deposition because Ni has superior adhesion to GaN as well
as the work function of the Ni is close to Au [30,31]. Hence, the gate
region was fabricated by the deposition of Au/Ni with the 50/10 nm
thickness, which was further patterned by optical lithography. The
length of the gate was 50 μm.
After the fabrication of AlGaN/GaN HEMT and synthesis of MoS2,
the gate region of HEMT was functionalized by self-assembled MoS2
layers. In this approach, the as-synthesized MoS2 powder was grind for
30 min. After grinding, a solution of 20 mg/ml was prepared in IPA
(isopropyl alcohol) of MoS2 powder. This solution was ultrasonicated
for 2 h. Subsequently, this solution was drop cast on the gate region of
the HEMT. After that, the device was annealed for 15 min at 80 °C. In
this process, when MoS2 forms layer on the gate terminal, it adsorbed
on the Au – gated HEMT.
3.2. Structural analysis of MoS2
The scanning electron microscopy (SEM) was performed to analyze
the morphology of as-synthesized MoS2. Fig. 1(a) shows a generalized
view of SEM results of MoS2 structures, and the magnified view showed
in Fig. 1(b). These results reveal the formation of the flower-like MoS2
nanostructures. Fig. 1(b) demonstrate that the nanostructures consist of
many curved nanoflakes or nanopetals with the length of several nan-
ometers. These nanopetals are very thin and can form relatively open
and porous nanostructures, which makes excellent use of the grain
surfaces that are easily accessible to the ionic solutions. These porous
nanostructures can also beneficial for electron transport during ion
sensing [32].
The X-ray diffraction (XRD) pattern of the as-prepared MoS2 flower-
like structures prepared by hydrothermal route is depicted in Fig. 1(c).
The XRD peaks observed at 2θ = 14.124, 33.465, 39.36 and 58.688
represents the (002), (100), (103) and (110) phase of MoS2 respectively
(JCPDS - 37–1492) [27,33]. It can be realized that the diffraction peak
at 2θ = 14.124 is higher than other phases, which indicate that the
flower-like MoS2 structures show good crystalline behavior towards
(002) phase of MoS2 and structure is well developed. In the XRD pat-
tern, there were no impurity peaks observed, which means a pure MoS2
was formed by hydrothermal route.
Further, the Raman analysis of the as-prepared MoS2 was also per-
formed at room temperature, and it is shown in Fig. 1 (d). Raman
spectra explain about the thickness and layer alignment of the syn-
thesized MoS2. There were two peaks observed at 376 and 401 cm−1,
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attributes the E2 g1, and A1g vibration modes of MoS2, respectively
[34–37]. In the observation of MoS2, the vibrational modes E2 g1 and
A1g signifies in-plane vibration and out-of-plane vibration of Mo and S
atoms [16,32,34]. It can be observed from Fig. 1 (d) that A1g vibration
mode has higher intensity than E2 g1 mode, which demonstrates that the
nature of as-deposited MoS2 layers is vertically standing [38–40].
3.3. Structural characterization of MoS2 functionalized layer on AlGaN/
GaN HEMT
The structural characterizations such as field emission scanning
electron microscopy (FESEM), AFM, and Raman spectroscopy were
performed to observe the evidence of the MoS2 on the gate region of
AlGaN/GaN HEMT. These characterizations were executed after drop-
casting the MoS2 on the gate region of AlGaN/GaN HEMT and has
shown in Fig. 2. The FESEM was performed to analyze the morphology
of MoS2 on the gate region. Fig. 2 (a) and (b) shows the lateral and
cross-sectional view of MoS2 functionalized AlGaN/GaN HEMT. Fig.2
(a) demonstrates the flower-like structure on the gate terminal of
AlGaN/GaN HEMT, where the petals of the flower-like structures are
looking vertically standing. The cross-sectional view is shown in Fig. 2
(b) also confirms the vertical alignment of the petals of the flower-like
structure of MoS2. Moreover, AFM analysis was further performed on
the device, and the topographical AFM image has been shown in Fig. 2
(c). The AFM image also reveals the quantitative height and flower-like
morphology on the surface of the Au-gated AlGaN/GaN HEMT. The
presence of MoS2 on the AlGaN/GaN HEMT was further confirmed by
utilizing Raman spectroscopy analysis, as shown in Fig. 2 (d). In this
observation, the presence of E2 g1 and A1g vibrational modes was si-
milarly observed as Fig. 1 (d), which confirms the presence of MoS2 on
Au-gated AlGaN/GaN HEMT. Based on the Raman spectra and the
FESEM images, it can be said that the flower-like MoS2 structures
possess the rich few-layers structures in the form of petals, which
provides a large number of active edge sites.
3.4. Electrical characterization of MoS2 functionalized AlGaN/GaN HEMT
for Hg2+ ion sensing
The electrical behavior of the developed HEMT sensor is demon-
strated in Fig. 3. The electrical behavior of the fabricated HEMT was
examined by measuring drain to source current (IDS) with respect to
applied drain to source voltage (VDS) as shown in Fig. 3(a). Here VDS
was changed from 0 V to 3 V. The I–V characteristics were observed
before functionalization (as-fabricated HEMT), after MoS2 functionali-
zation on the gate terminal and after applying 10 ppm concentration of
Hg2+ ions. A distinct variation in IDS can be seen in Fig. 3(a) after each
step. The IDS was decreased by employing MoS2 on the gate terminal. It
was due to the fact that, when MoS2 was self-assembled on Au gated
region, the metal-semiconductor interface was formed. Since the work
function of Au is 5.1 eV, and MoS2 has ∼ 4.7 eV [16,17], therefore
when the contact is made between MoS2 and Au, the electrons trans-
ferred from MoS2 to Au due to difference in Fermi levels, which would
increase the electrons density in Au. This excess of electrons increases
the negative charge on the Au gated region and make the gate more
negative, which ultimately reduce the drain current as follows:
εn μW 2
IDS = [2((VG − VT ) VDS − VDS )]
2dL (2)
Where εn is the total permittivity of GaN cap layer, Al0.23Ga0.77N bar-
rier layer, and AlN spacer layer, VG is gate potential, W is width and L is
length of the gate, μ is the electron mobility in 2DEG, VT is the
threshold voltage of the device, and d is the 2DEG and surface distance.
The device parameters εn, d, L, W, and VT would be constant.
Fig. 3(b) showed real-time sensing response of Hg2+ ions on MoS2
functionalized AlGaN/GaN HEMT. In the sensing process, the analysis
was carried out by introducing the Hg2+ ion solution on the MoS2
A. Nigam, et al.
Fig. 1. (a), (b) SEM images of MoS2 flower like structure (c) XRD pattern of the flower-like MoS2 (d) Raman Spectrum of as-deposited MoS2.
functionalized surface of the gate. Here the concentration of the ionic
solution of Hg2+ was varied from 0.1 ppt (parts per trillion) to 10 ppm.
The sensing response was observed for 300 s for each Hg2+ ion con-
centration. After applying different concentrations of Hg2+ ions, the
apparent variation in the IDS was observed. This alteration in IDS reflects
the detection of Hg2+ ions. Interestingly, it was found that initially, the
IDS was increased by applied Hg2+ ion concentration from blank to 10
ppt, and it starts decreasing by applying a higher concentration of Hg2+
ions from 100 ppt to 1 ppm. The reason behind the increment in the
drain current could be the electron transfer from MoS2 to Hg2+ due to
the chemical adsorption phenomenon. In general, Hg2+ ions possess a
high binding affinity toward sulfur. When Hg2+ ions interact with the
sulfur group on the MoS2 surface, the S2− group may donate electrons
to the adsorbed Hg2+ ions and makes the Hg-S complex with it [25,26].
In this process, the negative surface charges get decreases, which in
turn increases the VG, and hence the IDS increase initially by Eq. (2). By
further increment in Hg2+ ion concentration, the drain current starts
decreasing. The decrement in the drain current may be observed due to
electrostatic interaction at the gate terminal, which induces negative
charges towards the MoS2 functionalized gate region, which can make
the gate potential more and more negative and hence drain current
starts decreasing. It can also be seen from Fig. 3(b) that after applying a
higher concentration of Hg2+ ions of 10 ppm, no change was observed
in the IDS, implies that the saturation of MoS2 functionalized surface
due to the higher concentration of Hg2+ ions.
The sensing parameters like the limit of detection (LoD) and sensi-
tivity were calculated by observing IDS vs. Hg2+ ion concertation plot,
as depicted in Fig. 3(c). Here, the limit of detection was calculated by
the standard 3-sigma approach. The limit of detection was calculated by
the following expression:
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Sensors & Actuators: B. Chemical 309 (2020) 127832
LoD= 3σ/m (3)
Here σ, and m are the standard deviation (SD) of least concentration of
the Hg2+ ions, and the sensitivity of the sensor respectively. The sen-
sitivity (m) of the sensor was calculated as the slope of the fitting curve,
and it was observed as 0.64 μA/ppb. The values of parameters such as σ
and linear regression coefficient were derived from the Fig. 3(c) as
0.00246 and 0.9997 respectively, and hence the limit of detection was
determined from Eq. (2) as 0.01152 ppb or 11.52 ppt. This limit of
detection of the Hg2+ ions on MoS2 functionalized AlGaN/GaN is suf-
ficiently below than the standard limit set by WHO for drinking water
standards for Hg2+ ions (1 ppb). The linear detection range of the
sensor was observed from 0.1 ppb to 100 ppb. The response time of the
sensor was also derived by employing a similar process used in our
previous report. By this process, the sensor demonstrated an ultra-fast
response of 1.8 s at 1 ppt. It is the fastest response time observed by
MoS2 functionalized AlGaN/GaN HEMT at low concentration of Hg2+
ions. Thus, the ultra-low-level detection of Hg2+ ions with rapid re-
sponse can be realized using MoS2 functionalized AlGaN/GaN HEMTs.
The selectivity of MoS2 functionalized AlGaN/GaN HEMT towards
Hg2+ ions, and other heavy metal ions were further examined by se-
parate solution method, [41] and the results are shown in Fig. 3(d), (e).
In this method, the response of the sensor for Hg2+ and other heavy
metal ions like Cd2+, Ni2+, Cu2+, Pb2+, Zn2+, and Cr3+ were observed
at the concentration range from 1 ppt to 10 ppm. For efficient se-
lectivity study, the observed current response for Hg2+ ions and other
interfering metal ions were subtracted from the base current i.e. the IDS
observed in deionized water termed as IDS0. Thus, the selectivity coef-
ficient for separate solution approach (also termed as response ratio)
RHg2+
, j can be given as [41]:
A. Nigam, et al.
Fig. 2. (a) FESEM (b) cross-sectional FESEM and (c) AFM images of MoS2 functionalized surface of AlGaN/GaN HEMT (d) Raman spectra of the MoS2 functionalized
Au-gated AlGaN/GaN HEMT.
(|IDS 0 − IDSj |) C Hg 2 +
R Hg 2 +, j =
(|IDS 0 − IDSHg 2 + |) Cj (4)
Where IDSjis drain to source current of interfering metal ion at con-
centration Cj, and IDSHg2+ is drain to source current at concentration
CHg2+. Here, the sensing response of interfering heavy metal ions and
Hg2+ ions were measured at identical concentration of 1 ppm. Hence,
the response ratio from Eq. (4) can be rewritten as:
|IDS 0 − IDSj |
R Hg 2 +, j =
|IDS 0 − I Hg 2 + | (5)
The calculated response ratio from Eq. (4) at 1 ppm concentration is
shown in Fig. 3(e), reveals that, lower the value of RHg2+
, j , higher the
selectivity. It can be seen from Fig. 3(d) that MoS2 functionalized
AlGaN/GaN HEMT sensor showed the measurable response for Hg2+
ions whereas no other meal ions gave any significant response. Further,
Fig. 3(e) also confirms that the selectivity of the sensor is very high
towards Hg2+ ions. The high selectivity towards Hg2+ ions is observed
mainly because of the strong soft–soft interactions between Hg2+ ions
and S as the metal ions with higher softness have a stronger affinity to
sulfur [42,43]. There was slight interference of Pb2+ ions and Cu2+
ions, indicates that they are softer than other cations such as Cd2+,
Ni2+, and Zn2+ ions [44]. However, Hg2+ ions possess significantly
higher softness than Pb2+and Cu2+ ions [43,44], which preferably
adsorb on the S binding sites and makes the sensor highly selective
towards Hg2+ ions.
Subsequently, the recovery, repeatability and reproducibility of the
AlGaN/GaN HEMT sensor were also explored. Fig. 3(f) shows the re-
sponse and recovery of the sensor. In the sensing process, the Hg2+ ions
were chemically adsorbed on the MoS2 surface by strong Hg-S bonding.
Thus, in order to remove adsorbed Hg2+ ions from the surface of MoS2,
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Sensors & Actuators: B. Chemical 309 (2020) 127832
more activation energy is required [45]. Hence, the PBS buffer was
heated at 150 °C and applied to the sensor for rinsing. The developed
sensor was rinsed in hot PBS buffer for 100 s to recover from the
bounded Hg2+ ions. During this process, the recovery was achieved by
99.15 %. The optimization of the recovery process was performed si-
milarly to our previous report [14]. Thus, it can be said that the utili-
zation of hot PBS buffer provides sufficient activation energy to remove
Hg2+ ions from the MoS2 surface, and hence excellent recovery of the
sensor was observed. Furthermore, the repeatability of the sensing re-
sponse was also observed by keeping all the operating conditions as
same as 1 st sensing response. It has been seen from Fig. 3(g) that the
sensor showed excellent repeatability of the sensing response under the
same operating conditions. Moreover, the reproducibility of the sensor
was realized by the fabrication of another AlGaN/GaN HEMT device
with the same device dimension as a proposed device and keeping the
same MoS2 functionalization process. The sensing analysis was also
performed under the same operating conditions as the proposed sensor.
The response of the new device has been shown along with the response
of the proposed sensor in Fig. 3(h). The slight change in the drain to
source current in the new device can be due to the internal resistance of
the device. The analysis of the reproducibility of the sensor was con-
ducted by the coefficient of variation (CV) method. The coefficient of
variation for both the senor was calculated as [46]:
Standard Daviation of the values of IDS
CV=
Average of the values of IDs (6)
Table 2 shows the average and standard deviation (SD) of the values
of IDS for both the sensors. Here the sensor-1 and sensor-2 are termed as
the proposed device and the newly fabricated device, respectively. The
calculated values of CV for both the sensor are very close to each other,
which indicates the excellent reproducibility of MoS2 functionalized
A. Nigam, et al. Sensors & Actuators: B. Chemical 309 (2020) 127832

Fig. 3. (a) IDS-VDS characteristics of the device after different steps of functionalization and sensing. (b) Real time Hg2+ ion sensing on MoS2 functionalized AlGaN/
GaN HEMT. (c) Sensor response and calibration curve for Hg2+ ion detection using MoS2 functionalized AlGaN/GaN HEMT (inset: sensor response at lower
concentration) (d) Relative sensing response of the sensor for various heavy metal and Hg2+ ions from 0.01 ppt to 10 ppm concentration (e) Response ratio of the
sensor for Hg2+ ions and other interfering heavy metal ions for selectivity analysis (f) Response and recovery of the proposed sensor (g) Repeatability and (h)
Reproducibility of the MoS2 functionalized AlGaN/GaN HEMT sensor.

Table 2
: Reproducibility of the MoS2 functionalized AlGaN/GaN HEMT.
Device Average IDS (μA) SD of IDS (μA) CV
Sensor-1 144.1428 1.50863 1.05E-02
Sensor-2 157.2251 1.42724 9.08E-03
AlGaN/GaN HEMT sensor for Hg2+ ion detection.
3.5. Sensing mechanism of Hg2+ ions by MoS2 functionalized AlGaN/GaN
HEMT
The sensing mechanism of MoS2 functionalized AlGaN/GaN HEMT
for Hg2+ ions is shown in Fig. 4. The functionalized MoS2 on the Au
gated AlGaN/GaN HEMT has exposed Sulfur atoms to attract the Hg2+
ions, as shown in Fig. 4(a). When the device was exposed to Hg2+ ion
solution, Hg2+ ions were strongly adsorbed on the surface of MoS2.
Initially, Hg2+ ions adsorb on the most sites on the MoS2 surface and
form Hg–S complexation, as shown in Fig. 4 (b). This formation of
chemical complexion is kept going on until Hg2+ ions fully occupy the
binding sites of MoS2 functionalized surface. In this process, the re-
duction of Hg2+ ions may occur on the surface of MoS2 by Sulfur (S) as
Hg2+ ions are the strong oxidizing agent while S is a natural reducer.
Thus, the S2− in MoS2 can donate its electrons to interact with Hg2+
ions to form Hg-S complex [22,26]. Hence, the formation of Hg-S
complex ultimately reduces the electrons from MoS2 surface, which in
CV (%) turn increase the gate potential of the device and hence the IDS rises.
By further increment in Hg2+ ions concentration, the binding sites
1.05 on the top of the first Hg2+ ion layer can be further engaged by Hg2+
0.91
ions, which can also form second Hg2+ ions layer. It is because the
MoS2 may still have negative charges due to higher S atoms and n-type
behavior, and the physical electrostatic interaction phenomenon causes
further Hg2+ ions adsorption as depicted in Fig. 4(c). The electrostatic
interaction further induces negative charges towards MoS2 surface.
Thus, while increasing more Hg2+ ion concentration, more negative
charges induce towards MoS2 surface. This process decreases the gate
potential simultaneously, and hence, IDS starts reducing by a further
increase in Hg2+ ion concentration. Some reports have reported that
the MoS2 layer was negatively charged in the complete sensing process;
only the potential associated with MoS2 would be less or more negative
[25,26]. Thus, these two-adsorption mechanisms which can happen one
after other to unwrap the role of MoS2 for ultra-low-level determination
of the Hg2+ ions. In addition to the affinity of Hg2+ ions to MoS2
surface, the ultrahigh surface to volume ratio, and the electronic
transport properties of MoS2 may also fasten the Hg-S complex for-
mation and electrostatic interaction appearing over the gate terminal.
Hence the AlGaN/GaN HEMT with MoS2 functionalization provides an
ultra-fast response for detection of Hg2+ ions.
The performance of proposed MoS2 functionalized AlGaN/GaN

6
A. Nigam, et al. Sensors & Actuators: B. Chemical 309 (2020) 127832

Fig. 4. Sensing mechanism of MoS2 functionalized AlGaN/ GaN HEMT for Hg2+ ion detection (a) HEMT with MoS2 functionalization (b) Hg-S complex formation on
the gate region of HEMT at low concentration of Hg2+ ions (c) electrostatic interaction between Hg2+ ions and MoS2 layer at high concentration of Hg2+ ions.

Table 3 complex due to interactions between the S of MoS2 at low concentration

Comparison of different sensing techniques for Hg2+ ion detection. of Hg2+ ions and the electrostatic iteration between MoS2 and Hg2+
Methods Functionalization LoD (ppb) Response time References
ions at high concentration of Hg2+ ions. Thus, the superior binding
properties of MoS2 for Hg2+ ions with an ultra-high surface to volume
ISFET rGO/TGA-AuNP 5 < 10 s [9] ratio in conjunction with AlGaN/GaN HEMTs makes the feasibility of
SERS Mesna/ AgNP 0.0024 9 min. [1] highly selective and sensitive Hg2+ ion sensor with ultra-low-level
Colorimetry DMSO: water 1 ̶ [47]
detection and rapid response time.
Electrochemical L-cysteine 0.995 ̶ [48]
Electrochemical CB/SPE 1 < 3 min [6]
AlGaN/GaN HEMT TGA/Au 27; 3 5 s; 15–20 s [11,13] Declaration of Competing Interest
AlGaN/GaN HEMT PVC 2 ̶ [10]
AlGaN/GaN HEMT MoS2/Au 0.01152 1.8 This work
They declare that there is no conflict of interest.
rGO: reduced graphene oxide; TGA: thioglycolic acid; AuNP: gold Nano par-
ticle; AgNP: Silver Nanoparticle; Mesna: sodium 2-mercaptoethanesulfonate; Acknowledgements
SERS: Surface Enhanced Raman Spectroscopy; DMSO: dimethyl sulfoxide; CB/
SPE: carbon black/ screen printed electrode; Polyvinyl chloride. This work is an outcome of the R&D project under the Visvesvaraya
PhD Scheme of the Ministry of Electronics and Information Technology,
HEMT sensor was compared with previously reported Hg2+ ion sensors Government of India, being implemented by Digital India Corporation
and showed in Table 3. The comparative analysis was made in terms of and has been supported by NSF MRI (1428992) and EDA University
limit of detection of the sensors and their response time for Hg2+ ion Center Program (ED18DEN3030025). In this work, the SEM analysis for
detection, observed that the MoS2 functionalized AlGaN/GaN HEMT MoS2 synthesis and AAS for Hg2+ ion concentration was carried out at
showed excellent detection limit with rapid response time as compared materials research facility (MRC) MNIT Jaipur, India.
to previously reported Hg2+ ion sensors.
References

4. Conclusion
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1.8 s and excellent detection limit of 11.52 ppt. The proposed sensor
demonstrates excellent selectivity towards Hg2+ ions. The possible
reasons of the outstanding sensitivity were the formation of Hg-S
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Adarsh Nigam received the M.E. degree in Embedded
System and VLSI Design from Rajiv Gandhi Prodyougiki
Vishwavidyalaya, Bhopal, India. He is currently working
toward the Ph.D. degree in Electrical Engineering from the
Indian Institute of Technology Jodhpur, Jodhpur, India. His
current research interests include simulation and fabrica-
tion of GaN HEMTs and III-Nitride devices.
Neeraj Goel received the B.Tech. degree in electronics and
communication engineering fromUttar Pradesh Technical
University, Lucknow, India, and the M.Tech. degree in
electronics and communication engineering from IIT (ISM)
Dhanbad, Jharkhand, India. He is currently pursuing the
Ph.D. degree in electrical engineering at IIT Jodhpur,
Jodhpur, India. His current research interests include 2-D
materials-based photodetectors and gas sensors.
Thirumaleshwara N Bhat received the B.Sc. degree in
physics, mathematics, and chemistry and the M.Sc. degree
in materials science from Mangalore University, Mangalore,
India, in 2005 and 2007, respectively, and the Ph.D. degree
from the Indian Institute of Science, Bangalore, India, in
2012. He joined the Institute of Materials Research and
Engineering, Agency for Science, Technology, and
Research, Singapore, in 2013, as a Research Scientist.
A. Nigam, et al. Sensors & Actuators: B. Chemical 309 (2020) 127832

Md Tawabur Rahman received the bachelor’s and master’s
degrees in electrical and electronic engineering from the
Khulna University of Engineering and Technology,
Bangladesh, in 2011 and 2014, respectively. He is currently
pursuing the Ph.D. degree in electrical engineering with
South Dakota State University, USA. His research interests
include sensors for precision agriculture
research projects include manufacturing of 150 and 200 mm diameter GaN epitaxial
wafers for high frequency and high power applications.
Surani Bin Dolmanan received his B.Sc. (Honours) degree
and M. Sc. Degree in Materials Science and Engineering
from National University of Singapore. He was a senior
engineer with the Systems on Silicon Manufacturing
Company (SSMC), Singapore, where he specializes in thin
film processing technology, new technology development,
and optimization of silicon wafer processing at various
technology nodes. During the initial years at SSMC, he had
successfully managed and oversaw qualification and tran-
sition of new equipment and processes from pilot produc-
tion to full manufacturing capability. He is currently with
the Institute of Materials Research and Engineering, Agency
for Science, Technology, and Research, Singapore, where
he is involved in R & D of wide bandgap semiconductors. His research interests include
GaN on Si epitaxy, nano-fabrication, and structural characterization of semiconductor
materials
Sudhiranjan Tripathy received the B.Sc. degree from
Maharaja Purna Chandra College, Baripada, Odisha, India,
the M.Sc. degree from the Indian Institute of Technology,
Delhi, India, and the Ph.D. degree from the Indian Institute
of Technology, New Delhi, India. His doctoral research fo-
cused on the optical properties of novel semiconductor
materials. In 2002, he joined the Institute of Materials
Research and Engineering (IMRE), Agency for Science,
Technology, and Research (A*STAR), Singapore. At IMRE,
he is currently a senior Scientist and a Project Leader en-
gaged in research and development of GaN-on-silicon
technologies. He has collectively contributed to 230 re-
search papers in various international journals. His current
Mahesh Kumar received the M. Tech. degree in solid state
materials from IIT Delhi, New Delhi, India, and the Ph.D.
degree from the Indian Institute of Science, Bangalore,
India. He is currently an Assistant Professor with the
Department of Electrical Engineering, IIT Jodhpur,
Jodhpur, India. His current research interests include
electronic materials, semiconductor devices, ferroelectric
thin films, and wide band gap semiconductors.

Qiquan Qiao is currently a Harold C. Hohbach Professor

and a Graduate Coordinator in Electrical Engineering with
South Dakota State University (SDSU). He has published
more than 130 peer reviewed papers in leading journals,
including Energy and Environmental Science, the Journal of
the American Chemical Society, Advanced Materials, Advanced
Energy Materials, Advanced Functional Materials, Nanoscale,
and Nano Energy. His current research focuses on polymer
photovoltaics, dye-sensitized solar cells, perovskite solar
cells, lithium ion batteries, and sensors. He has received
over $ 6.5 million research grants as PI or Co-PI. He re-
ceived the 2015 Distinguished Researcher Award from
SDSU, the 2014 F O Butler Award for Excellence in
Research at SDSU, the 2010 U.S. NSF CAREER, and the 2009 Bergmann Memorial Award
from the U.S.-Israel Bi-National Science Foundation.