Inorganic Chemistry Communications 159 (2024) 111833

Contents lists available at ScienceDirect

Inorganic Chemistry Communications

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

Short communication

Hydrothermal synthesis of MoS2 with tunable band gap for future

nano-electronic devices
Priyanka Berwal a, Suman Rani a, Smriti Sihag a, Paul Singh a, Rita Dahiya a, Ashwani Kumar b, c,
Amit Sanger d, Ajay Kumar Mishra e, f, *, Vinay Kumar a, *
a
Department of Physics, COBS& H, CCS Haryana Agricultural University, Hisar, Haryana-125004, India
b
Institute Instrumentation Centre, Indian Institute of Technology Roorkee, Uttarakhand 247667, India
c
Department of Physics, Graphic Era (Deemed to be University), Dehradun, Uttarakhand 248002, India
d
Department of Physics, Netaji Subhas University of Technology, Dwarka Sector-3, Dwarka, Delhi, 110078, India
e
Department of Chemical and Metallurgical, Vanderbijlpark Campus, Vaal University of Technology, Private Bag X021, Vanderbijlpark, South Africa
f
Department of Chemistry, Durban University of Technology, Steve Biko Road, 4001, Durban, South Africa

A R T I C L E I N F O A B S T R A C T

Keywords: Transition metal dichalcogenides (TMDs) have been explored in various domains of science and technology in
Transition metal dichalcogenides the past few years. Among the numerous transition metal dichalcogenides, MoS2 has sparked the interest of
Hydrothermal approach researchers owing to its peculiar, layered structure and associated intriguing optical and electrical properties
Morphology
which can be utilized in diverse applications including catalysts, gas sensing, energy storage, hydrogen storage
Fourier transform spectroscopy
etc. In recent work, the hydrothermal approach is employed to make two distinct morphologies of MoS2, namely
Nano-sheets and Nano-flowers, by utilizing ammonium molybdate as a precursor. Herein, X-Ray Diffraction
(XRD), Field Emission Scanning electron microscopy (FE-SEM), Transmission electron microscopy (TEM), X-ray
photoelectron spectroscopy (XPS), Fourier Transform Infrared spectroscopy (FTIR), and UV–Visible techniques
were utilized to validate the crystallographic structure, morphology, chemical composition, and band gap value
of as-synthesized samples. The MoS2 synthesized nanostructures showed a good response for 100 ppm NO2 gas at
100 ◦ C. The synthesized flower-based sensor showed a 24.03 % response and the sheet-based sensor showed a
15.64 % response value for 100 ppm NO2 gas at 100 ◦ C. The versatile morphology of MoS2, coupled with its
tunable band gap, open new avenues in the field of gas sensing.

1. Introduction
Nanotechnology has enabled the modification of material size and
composition at the nanoscale to provide a wide range of applications. In
recent years, the production of Nanomaterials with desirable features
and attributes has become the primary concern of the scientific com­
munity. After the discovery of graphene, 2D nanomaterials have become
increasingly relevant in nanotechnology. Transition metal dichalcoge­
nides are semiconducting materials, which were among the 2D nano­
materials, have recently attained attention due to their fascinating
properties. The photo-corrosion resistance of these 2D TMDs nano­
materials is particularly impressive. Chemical inertness, anisotropy,
electrical properties [1,2], strong catalytic capabilities with vacuum
resistance, and so forth are all desirable features. The general formula
used for transition metal dichalcogenides is MX2, where M denotes the
transition metal atom and X denotes the chalcogen. They are made up of
sandwich-like layers (X–M− X) that are only weakly attached. The
Vander Waals forces connect the layers that are next to each other. M is
covalently bound to X atoms in each layer. Among these, MoS2 has been
identified as the most promising material since it can be used to replace
graphene-based devices and other semiconductors at the nanoscale.
Molybdenum disulfide (MoS2) is a transition metal dichalcogenide
which consists of layering in its structure, analogous to graphite. It has a
hexagonal atomic structure and a trigonal prismatic geometry formed by
Mo and S atoms piled on top of one another. The spacing between the
two layers of MoS2 nano-sheets is 6.5 Å. MoS2 occurs in several crys­
talline forms, including hexagonal (H), tetrahedral (T), and rhombohe­
dral (R). The semiconducting 2H and 3R phases, as well as the 1 T
metallic phase of MoS2 are the most common configurations, with 2H
being more stable but less conductive than 1 T. Two Sulfur-

* Corresponding authors.
E-mail addresses: ajaykmishraedu@gmail.com (A.K. Mishra), vinay23@hau.ac.in (V. Kumar).

https://doi.org/10.1016/j.inoche.2023.111833
Received 27 July 2023; Received in revised form 25 November 2023; Accepted 30 November 2023
Available online 5 December 2023
1387-7003/© 2023 The Author(s). Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-
nc-nd/4.0/).
P. Berwal et al.
Molybdenum-Sulfur layers composed of edge-sharing MoS6 trigonal
prisms make up the 2H phase, whereas one Sulfur-Molybdenum-Sulfur
layer made up of edge-sharing MoS6 octahedral prisms which makes
up the 1 T phase [3,4]. Because there is no interlayer hybridization in
single-layer MoS2, it has very different physical properties than bulk
MoS2. At ambient temperature, MoS2 is a two-dimensional semi­
conductor with a high on/off current ratio and a high mobility value of
200 cm2 (Vs)-1. Its band gap changes from an indirect value of 1.2 eV to a
direct value of 1.9 eV when its transition occurs from bulk to nanoscale
[5,6]. Because of its high surface-to-volume ratio and quantum effects,
MoS2 is a potential resource for electrical and optoelectronic device
applications. 2D MoS2 has developed as a viable Nano electronics ma­
terial with applications in a variety of fields such as solid-state lubricants
[7], super-capacitors [8,9], hydrogen generation [10], gas sensing
[11,12] and as a photocatalyst to break pollutants or make hydrogen
[13,14]. Nano-MoS2 has diverse performance based on its size structure,
shape, and composition. Also, the synthesis process has a significant
impact on the uses of TMDs in diverse fields. MoS2 with various nano­
structures, like nano-tubes [15,16], nano-rods [17], nano-wire [18],
nano-sheet [19], nano-flowers [20–22] have been created using a large
number of methods, including both types of approaches (top-down, and
bottom-up) such as micromechanical exfoliation [23], physical vapour
deposition, chemical vapour deposition [24] and hydrothermal process
[25,26]. Among all techniques, the hydrothermal method is utilized to
synthesize MoS2 with various morphologies such as nano-sheets and
nano-flowers. It is the most convenient and easiest method with a high
yield of product. The hydrothermal method is also popular due to its
ease of morphological control, high homogeneity and crystalline prop­
erties, and low cost. Initial components, hydrothermal temperature,
molar ratios and process length are all well-known influences on mor­
phologies, crystal phase, and performance during hydrothermal pro­
cesses.Table 1.
In the present work, an attempt is made to synthesize MoS2 nano­
structures with different morphologies via the hydrothermal method.
The prepared nanostructures were characterized for their structural,
morphological, and optical properties. In addition, the effect of
morphology on the optical properties has been studied in detail. The gas
sensing properties of both morphologies were tested at different oper­
ating temperatures for 100 ppm of NO2 gas and it was found that syn­
thesized nanostructures are ideal candidates for gas sensing.
2. Experimental
2.1. MoS2 nano-sheet fabrication using hydrothermal method
Fig. 1 illustrates the hydrothermal synthesis of MOS2. Here, MoS2
nanosheets and nanoflowers are synthesized by optimization of hydro­
thermal temperature and reaction time [27]. In the production of MoS2
nano-sheets, ammonium molybdate ((NH4)6Mo7O24⋅4H2O) and sulfur
(S) powder were used as molybdenum and sulfur sources, respectively.
At first, 30 mL distilled water was used to dissolve 1.2 g ammonium
molybdate and 0.435 g sulfur powder. Now, 12 mL hydrazine was
poured into the above solution with continual stirring. After that, the
solution was autoclaved for 12 h at 160 ◦ C in a 100 mL stainless Teflon-
Table 1
Comparison of the NO2 gas response for various MoS2 nanostructures reported in the literature:
Material Method Morphology NO2 Conc.
MoS2 Hydrothermal Hollow sphere 100 ppm
MoS2 Sputtering Nano worms 100 ppm
MoS2TiO2 hydrothermal method – 50 ppm
nanotube
MOS2 CVD Flakes 100 ppm
MoS2 Hydrothermal Flower 100 ppm
MoS2 Hydrothermal Sheet 100 ppm
2
Inorganic Chemistry Communications 159 (2024) 111833
lined autoclave. Thereafter, the black MoS2 product was separated and
treated numerous times with ethanol and distilled water. Finally, the
black-coloured product was dried for 6 h at 60 ◦ C.
2.2. MoS2 nano-flowers fabrication using hydrothermal method
((NH4)6Mo7O24⋅4H2O) Ammonium molybdate and (CH4N2S) thio­
urea were adopted as precursors to make MoS2 flower-like nano­
structure. To start, 0.70 g ammonium molybdate ((NH4)6Mo7O24⋅4H2O)
and 4.48 g thiourea were mixed in 70 mL distilled water and repeatedly
agitated till a clear solution was obtained.
The produced solution was then autoclaved for 20 h at 180 ◦ C and 40
bar pressure in a 100 mL Teflon autoclave and at the end of treatment,
MoS2 black precipitate was extracted. After that, the pH of the solution
was adjusted to 7 by washing the materials with ethanol and distilled
water many times. Finally, the precipitates were dried at 60 ◦ C for 8 h
before being used for further analysis.
2.3. Characterization
Various characterization methods were used to characterize the hy­
drothermally fabricated MoS2 nanomaterials. Structural analysis has
been done by using an X-ray Diffractometer (Rigaku D/MAX2500PC)
with Cu Kα (1.54 Å) radiation. The scanning rate used was 4◦ /min, and
the diffraction angle value (2θ) extends from 10 ◦ C to 90 ◦ C. The surface
properties of the synthesized MoS2 samples were examined using Field
Effect Scanning Electron Microscopy (FE-SEM) and Transmission elec­
tron microscope (TEM) techniques. The chemical composition of the
synthesized MoS2 samples were analyzed by X-ray photoelectron spec­
troscopy (XPS). The functional groups linked to the produced MoS2 were
investigated in the region 4000 cm− 1 ––400 cm− 1 by using a Perkin
Elmer FTIR spectrometer. The optical properties of samples were
examined by using a UV–Visible 2600i spectrophotometer.
3. Results and discussion
3.1. Structural analysis
X-ray Diffraction analysis has been performed to analyze the struc­
ture of MoS2, which is shown in Fig. 2(a and b) . For the sheet-like
nanostructures of as prepared MoS2, the prominent peaks are posi­
tioned at 14.01◦ , 32.54◦ , and 57.54◦ which were related to (0 0 2),
(1 0 0) and (1 1 0) planes respectively, indexed to the hexagonal structure
of MoS2 [28]. The interplanar atomic spacing of MoS2 Nanosheets can be
evaluated from the XRD pattern using the Bragg equation:
2dsinθ = nλ (1)
where, d denotes the inter-planar spacing, θ is the Bragg scattering
angle, n is the diffraction order and λ is the wavelength of incident X-ray.
The inter-planer spacing corresponding to the (0 0 2) plane of the nano-
sheet is found to be 3.18 Å. While on the other hand in the case of nano-
flower MoS2, XRD peaks are observed at 13.90◦ , 32.39◦ , 35.75◦ , 43.16◦
and 57.26◦ attributes to various planes (0 0 2), (1 0 0) (1 0 2), (0 0 6) and
Op. Temp.(◦ C) %Response Response/Recovery time Ref.
150 40.3 79/225 sec [38]
150 32 56/80 sec [39]
150 14.2 – [40]
100 21.56 % 71/310 sec [41]
100 24.03 163/213sec This work
100 15.64 218/312 sec This work
P. Berwal et al. Inorganic Chemistry Communications 159 (2024) 111833

Fig. 1. Schematic representation of Hydrothermal synthesis of MoS2 nanoflower and nanosheet.

Fig. 2. XRD Pattern (a) MoS2 Nanosheet (b) MoS2 nanoflower.

(1 1 0) respectively, which confirms the hexagonal crystal structure. No background intensities of peaks show the amorphous behavior in MoS2
other peak was observed which shows the purity of samples [29]. The samples [30].
sharp peak at 13.9◦ , belongs to the (0 0 2) plane, has an inter-planner The FE-SEM was used to examine the surface characteristics of the
spacing of 3.20 Å and shows the layered MoS2 formation. The prepared nanostructures. Fig. 3 illustrates the FE-SEM measurements of

Fig. 3. FE-SEM images of synthesized Nano-sheets of MoS2 (a), (b) and MoS2 Nano-flower (c), (d).

3
P. Berwal et al.
both manufactured MoS2 nanostructures at various magnifications,
Fig. 3(a) and 3(b) depict the morphology of as prepared MoS2 with a
sheet-like structure at low and high magnifications respectively. The
flower-like morphologies of synthesized MoS2 are shown in Fig. 3(c) and
(d), with several petals growing in all directions and partly spherical or
spherical and also, contains nano-sheets [31] which agglomerated to
form nano-flower like structure. The sample was analyzed at various
magnifications to demonstrate the genuine flower-like structure of the
fabricated samples. The flower-like MoS2 nanostructure has a mean
diameter of 2.8 μm.
Further, the TEM analysis of synthesized samples of MoS2 was also
carried out to study morphological and topography properties. Fig. 4 (a,
c) shows the HR-TEM images of the MoS2 nanosheets. It can be seen that
the noticeable contrast between the sheet and few layers covered with
each other. In Fig. 4 (b, d), the MoS2 nanoflower [32] reveals the tightly
packed multi-layers and thin nanosheet layers connected together to
form flower like structure. In Fig. 4(c), the high resolutions HR-TEM
images show the few layered structures and the d-spacing is 0.287 nm
and ascribed to the (1 0 0) plane. the d-spacing of (1 0 0) plane is
consistent with the XRD indexed plane (1 0 0).
Fig. 4 (e and f) the SAED pattern of the MoS2 nanosheets and MoS2
nanoflower and showed that the MoS2 nanoflower is more crystalline
than nanosheet and the results are consistent with the XRD.
3.2. XPS analysis
The X-ray photoelectron spectroscopy (XPS) was used to analyze the
elemental and chemical state of MoS2. Fig. 5(a and d) show the survey
spectra of the MoS2 Nano sheet and Nano flower with peaks of Mo and S
which confirms that each sample has Mo and S. Moreover Fig. 5 (b and c)
reveals the two broad Mo 3d distinguished peaks observed at 228 (±1)
Fig. 4. TEM image of MoS2 (a,c) nanosheet at different magnification (b,d) nanoflower at different magnification. (e), (f), the SAED pattern of the MoS2 nanosheets
and MoS2 nanoflower.
4
Inorganic Chemistry Communications 159 (2024) 111833
eV and 231 (±1) eV, which have been indexed to Mo4+ 3d5/2 and Mo4+
3d3/2, respectively. In the Nano sheet, these deconvoluted peaks show
the existence of Mo4+ at 228.2 eV and 231.09 eV, while the Nano flower
structure indicates the presence of Mo4+ at 229.8 eV and 232.6 eV.
There is a shift in the binding energy of Nano flower and Nano sheet
which may occur due to the change in morphology of both samples.
Nano flower enhances the electrical conductivity due to the enhanced
charge density or surface area, moreover, Nano sheet provides stability.
Further, the S2p spectrum (shown in Fig. 5c and 5e) possesses two strong
peaks of S 2p3/2 and S 2p1/2 at ~ 162.2 eV and ~ 163.36 eV, respec­
tively. Strong peaks positioned in the Mo spectra and S spectra of both
samples confirm the oxidation state of MoS2 and provide a confirmation
check towards the correct synthesis of both samples.
3.3. Optical properties
The FT-IR spectra of prepared nano-sheets and nano-flower are
shown in Fig. 6 (a) and 6 (b), respectively. The absorption peaks at
591.10 cm− 1, 1117 cm− 1, 1637 cm− 1 and 3441.18 cm− 1 are observed
for nano-sheet like MoS2 while in the case of flower-like nanostructure,
the peaks are obtained at 596.41 cm− 1, 907.40 cm− 1, 1038.09 cm− 1,
1630 cm− 1 and 3429.77 cm− 1respectively. The absorption peaks in the
range 500–600 cm− 1 and 900–950 cm− 1 are attributed to the molyb­
denum/sulfur bond and sulfur-sulfur bond, respectively [33]. The
Molybdenum-oxygen vibrations and stretching vibrations of the OH
group are responsible for the absorption band between 1100 cm− 1 and
1650 cm− 1. The presence of the hydroxyl (–OH) group is responsible for
the strong and broad found around 3500 cm− 1.
The UV–Visible spectra of MoS2 nano-sheet and Nano flower were
analyzed at room temperature in the wavelength range of 200–800 nm
as shown in Fig. 7(a and c). MoS2 exhibits strong absorbance in the UV
P. Berwal et al.
Fig. 5. XPS spectra of the MoS2 (a-c) nanosheets sample: a survey scan, Mo 3d and S 2p (d-f) nanoflower sample: a survey scan, Mo 3d and S 2p.
Fig. 6. FTIR spectra of (a) MoS2 Nano-sheets (b) MoS2 nanoflower.
region.
The nano sheet-like morphology shows strong absorption peaks at a
shorter wavelength of 324 nm and the Nano flower shows strong peaks
at 276 nm and 303 nm respectively. The energy bandgap of both the
MoS2 nanostructures are calculated by using the Tauc’s plot equation,
(αhv)n = A(hυ − Eg
Where, α denotes the absorbance coefficient, hυ represents incident
energy, Eg denotes band gap value, A denotes constant, n = 2 for direct
band gap. Since the MoS2 exhibits a direct transition at the nanoscale
and an indirect transition at the bulk level, so n = 2 was taken for both
synthesized samples [34,35]. The plots of (αhν) n versus hν for MoS2
samples are shown in Fig. 7 (b and d) . The value of optical band gap
Inorganic Chemistry Communications 159 (2024) 111833
energy (Eg) can be calculated by extrapolating the linear portion of the
plot of (αhν) n versus hν to (αhν) n = 0. The calculated direct band gap
value for the MoS2 Nano sheet is 1.63 eV and MoS2 Nano flower is 2.2
eV.
4. Gas sensing measurements
(2)
The gas sensing measurements were done using the pallet mode of
synthesized MoS2 powder. For this, firstly measure the sample having
weight 0.14 g and make the pallet of thickness 1 mm and diameter 13
mm by applying the pressure of 100 kg/cm3 using the Hydraulic press
machine. Then apply the silver paste to two ends of the pallet having a
separation of 2 mm for electrical contacts and dry the pallet at 80 ⁰C for 3
5
P. Berwal et al.
Fig. 7. (a) UV–Visible absorption spectra of MoS2 Nano sheet (b) Tauc plot of MoS2 Nano sheet (c) UV–visible absorption spectra of MoS2 Nano flower (d) Tauc plot
of MoS2 Nano flower.
hrs. Then, gas sensing analysis was done for NO2 gas at various tem­
perature ranges (RT-150 ◦ C). To study the sensing properties, the pallet
was first placed inside the gas sensor setup and a change in the value of
current was noted down in the absence/presence of NO2 gas. The
Keithley 2450 source meter was used to record the change in current as a
time-dependent variable. By using the LABVIEW software measurement
panels and two mass flow controllers the required amount of gas was
injected inside the gas sensor set up. The total flow rate for nitrogen gas
and sensing gas was maintained constant which was 200 sccm. The gas
sensing properties of the synthesized materials were studied in terms of
percentage response, response time and recovery time. The percentage
response of the sensor was calculated with the formula [36,37] given
below:
] was 100 ◦ C as shown in Fig. 8 (a). The MoS2 flower-based sensor showed
[Ia − Ig
%R = × 100 (3)
Ia
.where Ia , denotes the value of the current of the sensor in the
presence of dry air and Ig denotes the value of current in the environ­
ment of the target gas. The time in which the sensor’s current becomes
90 % of the final current while the gas was adsorbed was termed the
response time and recovery time is the time at which the sensor is
required to return to the 90 % value of the initial baseline current in the
presence of dry air. Initially, the IV measurements were done having a
voltage range of − 1 to 1 V at every temperature and a constant voltage
value of 1 V, and sensing analysis of MoS2 based sensor were analyzed.
The gas sensing parameters of the prepared sensor based on MoS2
micro flower and sheet-like structure were analyzed for NO2 gas in
detail. For the purposes of gas sensor applications, the operating tem­
perature is an essential characteristic. So, the formed pallet-based sensor
of synthesized MoS2 was employed to find out the optimal working
6
Inorganic Chemistry Communications 159 (2024) 111833
temperature of the sample for NO2 gas with maximum response. The
response increases as the working temperature rises, reaches its
maximum value at 100 ◦ C, and then begins to decrease with an increase
in the temperature. The % response of sensor’s at various temp (RT-
150 ◦ C) is shown in supplementary information (Fig. S1). As the tem­
perature rises, the chemical reaction between gas molecules and the
surface of the MoS2 sensor increases. The MoS2 based sensor and NO2
transfer gas electrons more readily at higher temperatures. Furthermore,
if the response drops after the threshold temperature, it could be the
result of thermally generated electrical noise in the sensor or the
desorption of gas molecules from the sensing surface prior to the reac­
tion occurring.
The optimal temperature for the MoS2 flower and sheet-based sensor
a maximum % response of value 24.03, and sheet-based sensor showed
15.64 for 100 ppm NO2 gas at 100 ◦ C as shown in Fig. 8 (b). The IV
measurements of the MoS2 flower and MoS2 sheet-based sensor at
various temperatures are shown in Fig. 9 (a), (b). The sensor showed the
p-type behavior as the current started to increase as NO2 gas was
injected into the chamber. The detailed mechanism of gas sensing has
been mentioned in supplementary information. The response of the
MoS2 sensors exposed to 100 ppm NO2 gas mixed with dry synthetic air
at 100 ◦C in terms of actual current value is shown in Fig. 9 (c), (d).
These results indicate that the MoS2 gas sensor has a good response
towards NO2 gas. The response and recovery time were measured having
values of 163 sec and 213 sec for 100 ppm NO2 gas at 100 ◦ C for the
flower-based sensor and 218 s response time, and 312 s recovery time for
sheet-based sensor. The sensor was also tested for 3 cycles of repeat­
ability at 100 ◦ C for 100 ppm NO2 gas. Fig. 10(a) displays the repeat­
ability of the MF sample for three successive cycles to 100 ppm of NO2
P. Berwal et al. Inorganic Chemistry Communications 159 (2024) 111833

Fig. 8. (a) Operating temperature curve for MoS2 flower and sheet-based sensor (b) comparison of % response value for 100 ppm NO2 gas for MoS2 flower and sheet-
based sensor.

Fig. 9. (a) IV characteristics of MoS2 flower-based sensor at different temp. (RT-150 ◦ C) (b) IV curve of MOS2 nanosheet at various temp.(c) Response curve of
flower-based sensor at 100 ◦ C for 100 ppm NO2 gas in terms of current. (d) Response curve of sheet sensor at 100 ◦ C for 100 ppm NO2 gas in terms of current.

gas at 100 ⁰C.
Fig. 10(b) displays the repeatability of the MS (MOS2 sheet-based
sensor) sample for three successive cycles to 100 ppm of NO2 gas at
100 ⁰C. The comparison table 1 for NO2 sensing as reported in literature
with this work also listed below.
5. Conclusion
In this study, MoS2 morphologies have been effectively produced
using a simple and inexpensive hydrothermal method. The XRD
revealed the crystalline structures of produced nanostructures of MoS2.
The XRD results indicate the hexagonal like structure of the MoS2
samples. The FE-SEM confirmed the sheet and flower like morphology of
synthesized samples. The flower-like structure of MoS2 has a mean
diameter of 2.8 μm which is also in good agreement with TEM results.
The UV–visible spectra showed strong peaks in the UV region for both
samples and the calculated value of the band gap for the Nano sheet
structure is 1.63 eV and for Nano flower sample is 2.2 eV using Tauc’s
plot. The findings of the experiments reveal that reaction temperature
and duration were crucial factors in determining the final structures. By
altering the growing period, the morphology may be easily regulated.
The as-prepared nanostructures of MoS2 were used for application in the

7
P. Berwal et al.
Fig. 10. (a) Repeatability cycle of MoS2 flower-based sensor for 100 ppm at 100 ◦ C. (b) Repeatability cycle for MoS2 sheet-based sensor for 100 ppm at 100 ◦ C.
gas sensing field for NO2 gas sensing. Both nanostructures showed good
response for 100 ppm NO2 gas at 100 ◦ C having a 24.03 % response for
the MoS2 flower-based sensor and 15.64 % response for sheet like
morphology of MoS2 sensor. The sensor showed good response time,
recovery time and good repeatability. Both morphologies showed the p-
type behavior in gas sensing. The flower based MoS2 sensor exhibits
better response as compared to the nanosheet due to a more porous
structure and more active sites on the surface of the flower for better
adsorption of gas molecules.
CRediT authorship contribution statement
Priyanka Berwal: Conceptualization, Formal analysis, Writing –
review & editing. Suman Rani: Conceptualization, Formal analysis,
Writing – original draft. Smriti Sihag: Writing – review & editing. Paul
Singh: Investigation, Validation, Visualization. Rita Dahiya: Investi­
gation, Validation, Visualization. Ashwani Kumar: Formal analysis,
Investigation. Amit Sanger: Formal analysis, Investigation. Ajay
Kumar Mishra: Visualization, Writing – review & editing. Vinay
Kumar: Conceptualization, Methodology, Resources, Visualization,
Writing – review & editing.
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Data availability
The data that has been used is confidential.
Acknowledgement
We are grateful to the IIC, IIT, Roorkee, Uttarakhand, for providing
necessary ads for characterization tools. The first author, Priyanka
Berwal is thankful to University Grant Commission for providing
fellowship.
Appendix A. Supplementary data
Supplementary data to this article can be found online at https://doi.
org/10.1016/j.inoche.2023.111833.
8
Inorganic Chemistry Communications 159 (2024) 111833
References
[1] N. Chaudhary, M. Khanuja, S.S. Islam, Hydrothermal synthesis of MoS2 nanosheets
for multiple wavelength optical sensing applications, Sens. Actuators, A 277 (2018)
190–198, https://doi.org/10.1016/j.sna.2018.05.008.
[2] M. Farooq, T. Iqbal, M.S. Mansha, K.N. Riaz, G. Nabi, M.A. Sayed, S. Afsheen,
Synthesis and characterization of surfactant assisted MoS2 for degradation of
industrial pollutants, Opt. Mater. 133 (2022), 113033, https://doi.org/10.1016/j.
optmat.2022.113033.
[3] G. Eda, T. Fujita, H. Yamaguchi, D. Voiry, M. Chen, M. Chhowalla, Coherent atomic
and electronic heterostructures of single-layer MoS2, ACS Nano 6 (8) (2012)
7311–7317, https://doi.org/10.1021/nn302422x.
[4] S.J. Panchu, M.A. Adebisi, E. Manikandan, M.K. Moodley, Catalyst-free growth of
MoS2 nanorods synthesized by dual pulsed laser-assisted chemical vapor deposition
and their structural, optical and electrical properties, J. Electron. Mater. 49 (2020)
1957–1968, https://doi.org/10.1007/s11664-019-07817-z.
[5] M. Farooq, T. Iqbal, K.N. Riaz, A.M. Ali, A.A. El-Rehim, Simple synthesis of Ni-
doped MoS2 nanoparticles and their application as efficient photocatalyst:
experiment and COMSOL simulation, Chem. Pap. 76 (12) (2022) 7493–7506,
https://doi.org/10.1007/s11696-022-02422-7.
[6] H. Wu, L. Qin, G. Dong, M. Hua, S. Yang, J. Zhang, An investigation on the
lubrication mechanism of MoS2 nano sheet in point contact: The manner of particle
entering the contact area, Tribol. Int. 107 (2017) 48–55, https://doi.org/10.1016/
j.triboint.2016.11.009.
[7] J. He, J. Sun, J. Choi, C. Wang, D. Su, Synthesis of N-doped carbon quantum dots as
lubricant additive to enhance the tribological behavior of MoS2 nanofluid, Friction
11 (3) (2023) 441–459, https://doi.org/10.1007/s40544-022-0619-4.
[8] S. Kumar, V. Kumar, R. Devi, A.K. Sisodia, A. Jatrana, R.B. Singh, A.K. Mishra,
Sustainable and scalable approach for enhancing the electrochemical performance
of molybdenum disulfide (MoS2), Adv. Mater. Sci. Eng. (2022) 1–7, https://doi.
org/10.1155/2022/1288623.
[9] M. Gusain, A. Dubey, M. Das, S.K. Singh, Facial surfactant-free hydrothermal
synthesis of MoS2 microflower and its effect in electrochemical properties, Journal
of Solid-State Chemistry 274 (2019) 58–63, https://doi.org/10.1016/j.
jssc.2019.03.010.
[10] G. Ye, Y. Gong, J. Lin, B. Li, Y. He, S.T. Pantelides, P.M. Ajayan, Defects engineered
monolayer MoS2 for improved hydrogen evolution reaction, Nano Lett. 16 (2)
(2016) 1097–1103, https://doi.org/10.1021/acs.nanolett.5b04331.
[11] P. Berwal, S. Sihag, S. Rani, A. Kumar, A. Jatrana, P. Singh, V. Kumar, Hybrid metal
oxide nanocomposites for gas-sensing applications: A review, Ind. Eng. Chem. Res.
62 (37) (2023) 14835–14852, https://doi.org/10.1021/acs.iecr.3c02288.
[12] P. Berwal, P. Singh, S. Rani, S. Sihag, S. Kumar, A. Jatrana, V. Kumar, Fabrication
of two-dimensional MOS2 thin film using chemical vapor deposition (CVD) for gas
sensing application, in: International Conference on Nanotechnology:
Opportunities and Challenges, Springer Nature Singapore, Singapore, 2022,
pp. 403–408.
[13] S.V.P. Vattikuti, J. Shim, Synthesis, characterization and photocatalytic
performance of chemically exfoliated MoS2, in: IOP Conference Series: Materials
Science and Engineering 317, 2018, p. 012025.
[14] M.S. Mansha, T. Iqbal, Theoretical and experimental study of graphene modified
metal vanadate for its application as efficient photocatalyst, Opt. Quant. Electron.
54 (11) (2022) 706, https://doi.org/10.1007/s11082-022-04114-8.
[15] S.S. Sinha, L. Yadgarov, S.B. Aliev, Y. Feldman, I. Pinkas, P. Chithaiah, R. Tenne,
MoS2 and WS2 nanotubes: Synthesis, structural elucidation, and optical
characterization, J. Phys. Chem. C 125 (11) (2021) 6324–6340, https://doi.org/
10.1021/acs.jpcc.0c10784.
P. Berwal et al.
[16] Q. Jiang, S. Wang, X. Li, Z. Han, C. Zhao, T. Di, S. Liu, Z. Cheng, Controllable
growth of MoS2 nanosheets on TiO2 burst nanotubes and their photocatalytic
activity, RSC Adv. 10 (67) (2020) 40904–40915, https://doi.org/10.1039/
D0RA08421B.
[17] Q. Zhang, Y. Song, B. Chen, X. Hu, W. Peng, Y. Li, X. Fan, One-step hydrothermal
synthesis of hierarchically structured MoS2 nanorods via reaction intermediates as
self-templates for chemo selective hydrogenation, Chem. Eng. J. 454 (2023),
140330, https://doi.org/10.1016/j.cej.2022.140330.
[18] Y.R. Liu, X. Li, G.Q. Han, B. Dong, W.H. Hu, X. Shang, C.G. Liu, Template-assisted
synthesis of highly dispersed MoS2 nanosheets with enhanced activity for
hydrogen evolution reaction, Int. J. Hydrogen Energy 42 (4) (2017) 2054–2060,
https://doi.org/10.1016/j.ijhydene.2016.09.052.
[19] Y. Zhao, Y. Liu, H. Liu, H. Kang, K. Cao, Q. Wang, L. Jiao, Improved
dehydrogenation performance of LiBH4 by 3D hierarchical flower-like MoS2
spheres additives, Journal of Power Sources 300 (2015) 358–364, https://doi.org/
10.1016/j.jpowsour.2015.09.088.
[20] N. Qureshi, K. Harpale, M. Shinde, K. Vutova, M. More, T. Kim, D. Amalnerkar,
Hierarchical MoS2-based onion-flower-like nanostructures with and without
seedpods via hydrothermal route exhibiting low turn-on field emission, J. Electron.
Mater. 48 (2019) 1590–1598, https://doi.org/10.1007/s11664-018-06908-7.
[21] S. Han, K. Liu, L. Hu, F. Teng, P. Yu, Y. Zhu, Superior adsorption and regenerable
dye adsorbent based on flower-like molybdenum disulfide nanostructure, Sci. Rep.
7 (1) (2017) 43599, https://doi.org/10.1038/srep43599.
[22] Sihag, S., Dahiya, R., Rani, S., Kumar, A., & Kumar, V. (2022). Investigation of
structural and optical characteristics of CuO nanoparticles calcinated at various
temperatures https://doi.org/10.56042/ijct.v2925.61511.
[23] K. Wang, J. Wang, J. Fan, M. Lotya, A. O’Neill, D. Fox, W.J. Blau, Ultrafast
saturable absorption of two-dimensional MoS2 nanosheets, ACS Nano 7 (10) (2013)
9260–9267, https://doi.org/10.1021/nn403886t.
[24] S. Hu, J. Li, S. Wang, Y. Liang, H. Kang, Y. Zhang, Z. Chen, Y. Sui, G. Yu, S. Peng,
Z. Jin, X. Liu, Detecting the repair of sulfur vacancies in CVD-grown MoS2 domains
via hydrogen etching, J. Electron. Mater. 49 (2020) 2547–2555, https://doi.org/
10.1007/s11664-020-07957-7.
[25] M. Farooq, T. Iqbal, Facile hydrothermal synthesis of Cd doped MoS2
nanomaterials for degradation of organic pollutants: Correlation between
experimental and COMSOL simulation, J. Inorg. Organomet. Polym Mater. 32 (11)
(2022) 4422–4433, https://doi.org/10.1007/s10904-022-02428-4.
[26] M.S. Mansha, T. Iqbal, M. Farooq, K.N. Riaz, S. Afsheen, M.S. Sultan, A. Masood,
Facile hydrothermal synthesis of BiVO4 nanomaterials for degradation of industrial
waste, Heliyon 9 (5) (2023), https://doi.org/10.1016/j.heliyon.2023.e15978.
[27] L. Luo, M. Shi, S. Zhao, W. Tan, X. Lin, H. Wang, F. Jiang, Hydrothermal synthesis
of MoS2 with controllable morphologies and its adsorption properties for bisphenol
A, J. Saudi Chem. Soc. 23 (6) (2019) 762–773, https://doi.org/10.1016/j.
jscs.2019.01.005.
[28] L. Yang, X. Cui, J. Zhang, K. Wang, M. Shen, S. Zeng, S.A. Dayeh, L. Feng, B. Xiang,
Lattice strain effects on the optical properties of MoS2 nanosheets, Sci. Rep. 4 (1)
(2014) 5649, https://doi.org/10.1038/srep05649.
[29] G. Tontini, G.D.L. Semione, C. Bernardi, R. Binder, J.D.B. de Mello, V. Drago,
Synthesis of nanostructured flower-like MoS2 and its friction properties as additive
Inorganic Chemistry Communications 159 (2024) 111833
in lubricating oils, Industrial Lubrication and Tribology 68 (6) (2016) 658–664,
https://doi.org/10.1108/ILT-12-2015-0194.
[30] N. Kumar, P. Siroha, H. Shankar, D. Singh, Y. Sharma, R. Kumar, J. Gangwar, Nano
Express 3 (3) (2022), 035001, https://doi.org/10.1088/2632-959X/ac7cfe.
[31] S. Santhosh, M. Sathish, S. Iyer, S. Kalluri, A.A. Madhavan, One-pot synthesis of
MoS2 nanoflowers for thermal energy storage applications, Materials Letters 302
(2021), 130343, https://doi.org/10.1016/j.matlet.2021.130343.
[32] H. Ganesha, S. Veeresh, Y.S. Nagaraju, M. Vandana, M. Basappa, H. Vijeth,
H. Devendrappa, 2-Dimensional layered molybdenum disulfide nanosheets and
CTAB-assisted molybdenum disulfide nanoflower for high performance
supercapacitor application, Nanoscale Advances 4 (2022) 521–531, https://doi.
org/10.1039/D1NA00664A.
[33] S. Mishra, P.K. Maurya, A.K. Mishra, 2H–MoS2 nanoflowers based high energy
density solid state supercapacitor, Mater. Chem. Phys. 255 (2020), 123551,
https://doi.org/10.1016/j.matchemphys.2020.123551.
[34] M. Ntakadzeni, W.W. Anku, N. Kumar, P.P. Govender, L. Reddy, PEGylated MoS2
nanosheets: A dual functional photocatalyst for photodegradation of organic dyes
and photoreduction of chromium from aqueous solution, Bulletin of Chemical
Reaction Engineering & Catalysis. 14 (1) (2019) 142–152, https://doi.org/10.9767/
bcrec.14.1.2258.142-152.
[35] C.P. Veeramalai, F. Li, Y. Liu, Z. Xu, T. Guo, T.W. Kim, Enhanced field emission
properties of molybdenum disulphide few layer nanosheets synthesized by
hydrothermal method, Appl. Surf. Sci. 389 (2016) 1017–1022, https://doi.org/
10.1016/j.apsusc.2016.08.031.
[36] S. Sihag, R. Dahiya, S. Rani, P. Berwal, A. Jatrana, A. Kumar, V. Kumar, The
development of CuO-ZnO based heterojunction for detection of NO2 gas at room
temperature, Appl. Phys. A 129 (10) (2023) 717, https://doi.org/10.1007/s00339-
023-06982-7.
[37] V. Kumar, A. Kumar, S. Priyanka, A. Jatrana, Two-dimensional (2D) nanostructures
for hazardous gas sensing applications, in: Handbook of Green and Sustainable
Nanotechnology: Fundamentals, Developments and Applications, Springer
International Publishing, Cham, 2023, pp. 2033–2053, https://doi.org/10.1007/
978.
[38] Y. Li, Z. Song, Y. Li, S. Chen, S. Li, Y. Li, H. Wang, Z. Wang, Hierarchical hollow
MoS2 microspheres as materials for conductometric NO2 gas sensors, Sens.
Actuators B Chem 282 (2019) 259–267, https://doi.org/10.1016/j.
snb.2018.11.069.
[39] A. Kumar, R. Chandra, V.K. Malik, MoS2 nanoworm thin films for NO2 gas sensing
application, Thin Solid Films (print) 725 (2021), https://doi.org/10.1016/j.
tsf.2021.138625.
[40] P.X. Zhao, Y. Tang, J. Mao, Y.X. Chen, H. Song, J.W. Wang, X.M. Zhang, One-
dimensional MoS2-decorated TiO2 nanotube gas sensors for efficient alcohol
sensing, J. Alloy. Compd. 674 (2016) 252–258, https://doi.org/10.1016/j.
jallcom.2016.03.029.
[41] R. Kumar, N. Goel, M. Kumar, UV-activated MoS2 based fast and reversible NO2
sensor at room temperature, ACS Sensors 2 (11) (2017) 1744–1752, https://doi.
org/10.1021/acssensors.7b00731.