Optical Materials 145 (2023) 114464

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Optical Materials
journal homepage: www.elsevier.com/locate/optmat

Research Article

Improvement in ammonia gas sensing properties of La doped MoO3 thin

films fabricated by nebulizer spray pyrolysis method
R. Jansi a, b, M.S. Revathy a, **, S. Vinoth c, Anuj Kumar d, R.S. Rimal Isaac e, N. Deepa f, Abdullah
M. Al-Enizi g, ***, Mohd Ubaidullah g, *, Bidhan Pandit h, Mohd Shahazad i, Manish Gupta j
a
Department of Physics, School of Advanced Sciences, Kalasalingam Academy of Research and Education, Krishnankoil-626126, Virudhunagar, Tamil Nadu, India
b
Multifunctional Materials Laboratory, International Research Centre, KalasalingamAcademy of Research and Education, Krishnankoil, 626126, Virudhunagar, Tamil
Nadu, India
c
Department of Electronics and Communication Engineering, ManakulaVinayagar Institute of Technology, Kalitheerthalkuppam, Puducherry, 605 107, India
d
Department of Chemistry, GLA University, Mathura, 281406, India
e
Department of Nanotechnology, Noorul Islam Centre for Higher Education, Kumaracoil, Kanyakumari District, 629180, Tamil Nadu, India
f
Department of Electronics and Instrumentation, SRM Institute of Science and Technology, Kattatankulathur, 603 203, Chennai, India
g
Department of Chemistry, College of Science, King Saud University, P.O. Box 2455, Riyadh, 11451, Saudi Arabia
h
Department of Materials Science and Engineering and Chemical Engineering, Universidad Carlos III de Madrid (UC3M), Avenida de la Universidad 30, 28911 Leganés,
Madrid, Spain
i
Department of Chemistry, Bhakt Darshan Government Post Graduate College, Jaiharikhal, 246193, District Pauri Garhwal, Uttarakhand, India
j
Division of Research and Development, Lovely Professional University, Phagwara, Punjab, 144411, India

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

Keywords: In the present work, different doping concentration (0, 1, 2, 3, 4 and 5 wt%) of Lanthanum (La) doped Mo­
La doped MoO3thin films lybdenum trioxide (MoO3) thin films were prepared using low cost Nebulizer spray pyrolysis (NSP)technique.
Nebulizer spray pyrolysis The crystalline, morphology, optical and gas sensing properties of thin films were investigated. The presence of
Gas response
monoclinic MoO3 structure was confirmed through the XRD investigation for all the samples with highest
Adsorption- desorption model
crystallite of 61 nm was observed for 2 wt% La doped MoO3 thin film. The surface morphology of the produced
thin films exhibits a reticulate nanofibrous mesh shape with increased particle size and porosity on addition of
2% La dopants in MoO3.The UV–Vis results showed the band gap values for the prepared thin films in the range
3.12–3.26 eV and the minimum bandgap was observed for the 2 wt% of La doped MoO3 thin film. Also the PL
results confirmed the presence of more oxygen vacancies for the 2 wt% of La doped MoO3 thin film. The NH3 gas
sensing study was conducted for the prepared films at room temperature, the 2 wt% of La doped MoO3thin film
exhibits a maximum sensor response of 900, faster response times (28 s and 2.9s) compared to other fabricated
devices. The results suggest that the 2% La doping in MoO3 could be an optimum doping concentration for the
preparation of commercial NH3 gas sensors.

1. Introduction agent in agricultural field, an anti-fungal agent, a curative agent in the

In current scenario, a device that monitors olfactory discrimination is
much required for detection, identification and quality evaluation of
gaseous mixtures not only in many industries but also essential for
environmental pollution control for early diagnosis of diseases [1].
Among various pungent odour gases, Ammonia (NH3) is a nitrogen
source for plant growth, a fertilizer (liquefied gas form), a preservative
leather industry, a coolant in vehicles, chemical, textile, and paper in­
dustries, and an anti-corrosion agent in the petroleum sector [2].
Conversely, its acute exposure implication is perilous. High dosage
creates a sun blocking function, smog and aerosols cause sudden tem­
perature drop [3], chronic health issues like headache, vomiting,
dyspnoea, pneumonedema, even death [4], impaired pulmonary func­
tion and Respiratory failures such as persistent bronchitis,

* Corresponding author.
** Corresponding author.
*** Corresponding author.
E-mail addresses: revz27vijay@gmail.com (M.S. Revathy), amenizi@ksu.edu.sa (A.M. Al-Enizi), mtayyab@ksu.edu.sa (M. Ubaidullah).

https://doi.org/10.1016/j.optmat.2023.114464
Received 20 March 2023; Received in revised form 24 September 2023; Accepted 2 October 2023
0925-3467/© 2023 Elsevier B.V. All rights reserved.
R. Jansi et al.
bronchiectasis, breathlessness, interstitial fibrosis, and poor gas ex­
change are examples of residual chronic lung illness [5]. Occupational
Safety and Health Administration (OSHA) had framed an allowable
exposure limit(PEL) for humans as 25 ppm for prolonged (8 h) and 35
ppm for shorter period (15 min) exposure [6], and concentration limit
for Immediate Danger to Life & Health (IDLH) is 300 ppm [7]. A Gas
sensor for human breath analysis is a potential alternative for detecting
the concentration level of exposure. Gas sensors strongly depend on the
size and morphology of the nanostructures. Ammonia (NH3) is a col­
ourless gas that is widely used in many parts of daily life. Ammonia is
largely utilized for the production of polymers, explosives, pesticides,
fabrics, pigments, and other chemicals, but it is also employed as a
refrigerant gas, fertilizers, and water purifier [8,9]. However, when
frequently utilized, not only affects living things but also harms the
environment. For instance, exposure to 500 ppm of NH3 can immedi­
ately irritate the nasal system, whereas exposure of NH3 at the con­
centration level around 1000 ppm might result in a pulmonary edema,
an accumulation of fluid inside the lungs, or even death [10–12]. As a
result, a higher performance gas sensor for detecting and monitoring
NH3 has become increasingly important in recent years [13], [14]. A gas
sensing device is the investigation for quick detection of toxic gases. Gas
sensing devices made from thin layers of nano material, there are widely
used to detect toxic gas and dangerous gas, especially nanomaterial that
have improved the gas sensing behaviour. Sensing parameters are
operating temperature, sensing limit, cost-effective manufacturing
technique, standardisation transferability and so on. These above pa­
rameters confirm that these gas detectors often can be used in gas
sensing applications [15]. Since metal oxide semiconducting thin layer
change their conductivity when they interact with gas molecules, they
are widely used for gas detection. Metal oxide gas sensors (MOS) also
offer easy manufacturing, low cost, and constant performance compared
to other types of gas sensing devices. Currently, metal oxide structured
materials were specifically designed as gas detection elements over
recent years [16]. Many literatures report the metal oxide (In2O3, SnO2,
and ZnO etc.) based gas detection materials. On the other hand, tran­
sition metal oxide V2O5, WO3 and MoO3 have become an hopeful
sensing materials to detect the gases [17]. Properties of MoO3 have been
studied widely and gained more attention because of its wide range of
applications, including catalysis, gas sensing, photo sensing, and
supercapacitor [18]. MOS are of two types, p-type (Co3O4,CuO and
Cr2O3) and n-type (Fe2O3, In2O3, SnO2, and MoO3) which are used as gas
sensors [19]. Among many n-type semiconducting gas sensors, MoO3 is
one of the best material as it offers a variety of advantages, including a
distinctive layered structure, variable band gap (2.8–3.6 eV), excellent
electron mobility, inexpensive cost-phase-controlled production, non­
toxicity, and outstanding electrochemical properties. As a result, interest
in this intriguing material is growing [20,21]. MoO3 exists in three
polymorphic phases. One is thermodynamically stable (α-MoO3), second
one is meta-stable (ß-MoO3) and the third is h-MoO3) [22]. Out of which,
meta-stable (ß-MoO3) structure exhibits excellent physio-chemical and
mechanical characteristics such as refractive index, energy gap, and
hardness [23]. MoO3 was also studied for its gas detection capabilities
for LPG, NH3, H2, and CO [16]. However, MoO3 suffer from numerous
short comings, including lower sensitivity & selectivity, higher opera­
tion temperatures, and lesser stability. Significant efforts have been
undertaken to overcome these drawbacks through doping process. The
structural and optical characteristics of nanostructures could be altered
by the process of doping with rare earth minerals. A wide band gap
semiconductor’s optical and luminescence characteristics could be
significantly changed by the addition of suitable Rare Earth (RE) ele­
ments. In semiconductors, noble metal additives like Pd, Pt, Au, Rh, Er,
Gd, Pr, and so on typically function as activators to improve their surface
properties, especially by providing surface adsorption sites and discrete
energy levels in order to promote the adsorption of the dissociative
oxygen at the surface even at low operating temperatures [24]. More­
over, RE oxides also possess intriguing catalytic characteristics, quick
2
Optical Materials 145 (2023) 114464
oxide ion mobility, and high surface basicity, all of which are predicted
to be significant in gas sensing. Lanthanum (La), one of the significant
RE elements, has drawn the greatest interest, since it would improve the
luminous behaviour, conductivity, and absorption properties of the host
material. To the best of the author knowledge, there were no reports on
the La-doped MoO3 thin films for NH3 gas sensing. Thus, in this study,
the authors focussed their attention towards studying the gas sensing
capabilities of larger ionic radii (La) doped with smaller ionic radii of
(Mo). Xin Li et al. [25] studied the gas sensing performance of Zr doped
MoO3 sample. High gas sensing performance is due to the 1D nano­
structure and Zr doping strategy. Zhuoqi Li et al. [26] observed the
enhancement in the sensing characteristic MoO3 nanobelts toward Tri­
methylamine gas due to the Ce site was acted as O2 absorbers and which
generate O− adsorption sites around Ce atoms. Shouli Bai et al. [27]
investigated the enhancement of the sensing properties Cd-doped MoO3
sample is due to the change of intrinsic defects of the samples. In
addition, MoO3 nanostructures were developed by using a variety of
techniques, including spin coating [4], hydrothermal evaporation [19],
chemical vapour deposition [28], sputtering [18], sol gel [29], spray
pyrolysis [30], and nebulized spray pyrolysis [31]. Spray pyrolysis is a
technique where the solution is sprayed and heated up to generate a thin
film. Whereas, nebulizer spray pyrolysis technique is a variation of spray
pyrolysis method, where a nebulizer was used to generate a tiny droplet
of the solution that are dispersed onto the substrate. This technique is
useful for depositing films with a more uniform thickness. Overall,
nebulizer spray pyrolysis is a more precise and controlled variation of
spray pyrolysis that can be better suited for thin film applications.
Semiconductor thin films prepared using nebulizer spray pyrolysis
technology (NSP), are cost effective and are suitable for mass produc­
tion. A major advantage of NSP is the low material consumption and
carrier gas flow that allow for pinhole-free smooth film deposition. In
the NSP method, optimization of several parameters can be done like
distance between the gun& the substrate, temperature, molarity, the
volume of the solution, pressure and substrate [31].
In this present work, (0, 1, 2, 3, 4and 5 wt %) La-doped MoO3 thin
films were prepared using NSP method. Further characterization was
done using XRD, FESEM, and EDX to clarify structural, morphological
and elemental analysis of the prepared films. Optical properties were
investigated using photoluminescence and UV–Vis spectrophotometer.
Homemade gas sensor set up was used to test the ammonia gas sensing
properties of the La doped MoO3 films.
2. Thin film coating procedure and characterization methods
2.1. Thin film coating
Nebulizer spray pyrolysis method was used to prepare a MoO3 and
La-doped MoO3 thin films. In this process 0.05 M (0.123 g) of ammo­
nium molybdatetetrahydrate((NH4)6Mo7O24.4H2O) (99.98%, Sigma-
Aldrich) and 1,2,3,4, 5 wt% of Lanthanum(III) nitrate hexahydrate (La
(NO3)3.6H2O), ((99.99%, Sigma-Aldrich) were added in the glass
container and mixed in 10 mL distilled (DI) water with continuous
stirring for 10 min. Initially, the glass slides were cleaned to remove
substrate impurities by usual cleaning techniques and then placed on a
hot plate kept inside a heating chamber at 450 ± 2 ◦ C. The prepared
solution was loaded into the nebulizer needle and continually sprayed
on the heated glass plate. The spraying pressure was kept constant at 1.5
kg cm− 2, the spacing between the glass substrate and the spray gun was
kept constant at 5 cm and the nozzle diameter is 5 mm. The spraying
nozzle was kept exactly above the substrate during the deposition pro­
cess, which includes a stepper motor system controlled by a micropro­
cessor was used to slowly move in the X and Y axes. After the La-doped
MoO3 film was deposited, the film temperature was reduced to normal
under open air conditions. The coated films were then placed in the
airtight container for further characterization.
R. Jansi et al. Optical Materials 145 (2023) 114464

Fig. 1. Schematic diagram for gas sensing setup.

2.2. Characterization techniques

The structural information of the prepared (0, 1, 2, 3, 4 and 5wt %)

La-doped MoO3 films were obtained by X-ray diffraction (XRD) studies
using the (Bruker D8 Advance Eco XRD). The morphology of materials
was investigated using a field emission scanning electron microscopy
(Apreo). A Varian Carry Eclipse PL Spectrometer was used to acquire
ambient temperature Photoluminescence (PL) data. Ocean Optics HR
2000 optical fiber spectrophotometer was employed to assess the optical
characteristics. The thin film ammonia sensing properties were
measured using a Keithley (model 2450) Source Meter in air and target
NH3 gas environment at ambient temperature. Average film thickness
was measured using stylus profilometer and it is around 550 nm.

2.3. Ammonia sensing procedure& testing

The observed humidity inside the gas chamber is 65%. Gas sensing
study was conducted with uniform humidity value. The experimental set
up for gas sensing is shown in Fig. 1, the prepared MoO3 thin films were
inserted into the gas sensing chamber. Ammonia was injected into the
chamber through the appropriate metal tube with flow rate of 0.1 mL/s,
which was attached to a heating element and a thermocouple. Atmo­
spheric pressure was maintained inside the chamber. The ammonia so­
lution is then processed to release ammonia vapours by heating to
100 ◦ C temperature. The current value under open air and ammonia gas
were measured at room temperature. After reaching the saturation
current, the front door was opened to reach the outside air on the film
surface. The process was repeated for a number of different NH3
concentrations.
Following formula was used to calculate the concentration of NH3. Fig. 2. XRD pattern of (a) MoO3, (b) MoO3:La1% (c) MoO3:La2%, (d) MoO3:
La3%, (e) MoO3:La4% and (f) MoO3:La5% thin films.
δVRT
C(ppm) = × 10− 6
(1)
MPb Vb
3. Results and its discussions
Where, δ represents the concentration of test gas (g ml− 1), R denotes the
gas constant (8.415 J mol− 1 K− 1), Vindicates the injected test gas vol­ 3.1. Crystallite structure
ume (mL), T denotes the temperature of the sensor (K), Pb and Vb are the
chamber pressure & volume (litres), and M represents the molecular Crystal structures of as-prepared undoped MoO3 and La (1,2,3,4 and
weight of the test gas (g mol− 1) [32]. The current value was continually 5 wt %)doped MoO3 samples were studied through diffraction pattern
monitored with respect to time for various NH3 concentration ranges. shown in Fig. 2. From Fig. 2, all the prominent peaks are matched well
Finally, the relationship between the current in the air (Ia) and the with the monoclinic MoO3 (JCPDS No.47-1320).Three strongest peaks
current in the target gas NH3 (Ig) was used to determine the overall located at (001), (002) and (102)for MoO3 and La (1, 2, 3, 4 and 5 wt%)
sensor response to the gas. doped MoO3, shows high crystallinity [33–35].The intensity of the peak

3
R. Jansi et al. Optical Materials 145 (2023) 114464

Table 1
0.9 λ
Structural parameters and lattice constants variation of La doped MoO3 thin D= (2)
films. β Cos θ

La doping Crystallite Strain x Lattice constants (Å) Cell β Cot θ

Concentration size (nm) 10− 3 volume ε= (3)
a b c 4
(%) V(Å3)

0 56 5.52 3.935 3.660 7.312 101.65 The lattice parameters were calculated using the relations
1 59 5.22 3.938 3.661 7.267 101.16 ( 2 )
2 61 5.03 3.980 3.690 7.113 101.26
1 1 h k2 sin2 β l2 2hlcosβ
= + + − (4)
3 58 5.37 4.046 3.608 7.162 100.72 d2 sin2 β a2 b2 c2 ac
4 54 5.74 3.972 3.691 7.076 100.65
5 53 5.83 3.963 3.698 7.103 101.02 V = abcsinβ (5)

Where, miller indices were represented as h,k,l, the interplanar spacing

increases based on the doping as shown in spectrum of (b,c) [36].
denoted as d, lattice constants and cell volume are denoted by a, b, c and
Though ‘La’ is incorporated into the MoO3 crystal structure, it does not
V.
affect its crystal structure [29,37] and 2 wt% of La doped MoO3 possess
Table 1 summarizes, the crystallite size, strain, lattice constants and
high crystallinity due to its high crystalline size. This is because of the
cell volume for undoped MoO3 and La (1, 2, 3, 4 and 5 wt%) doped
larger ionic radius of La3+ ions (0.106 nm) compared to the Mo3+ ions
MoO3 films. The change in the crystallite size, strain & lattice constant
(0.069 nm). On further addition of La, the diffraction peaks of MoO3
values of the developed thin films might be due to the substitution of
crystal begin to decrease as shown in spectrum Fig. 2 (d),(e),(f) [27]. The
larger ionic radius La ions into the MoO3 matrix, leading to the creation
decrease in crystallinity with increment in La dopants might be because
of more nucleation centres. It was observed that the crystallite size in­
of the increased lattice distortion and strain. The results indicate that the
creases with substitution of La dopants and decreases with further
coated samples exhibit high levels of crystallinity and purity. From XRD,
incorporation of dopants. The incorporated La3+ ions in MoO3 might
the interaction between the dopant La into the matrix of MoO3 thin films
increases the mobility of grain boundaries or alter the interfacial ten­
would significantly improves the optical properties of the thin films.
sion/surface energy, which would speed up the grain growth, resulting
The crystallite size (D) and strain (ε) values of all the La doped MoO3
in larger grains [38]. The addition of La dopants in MoO3 decreases
thin film samples are estimated and reported using the following
strain value while improving crystallite size, with a 2% La doped MoO3
equations (2) and (3)

Fig. 3. FESEM images of (a) MoO3, (b) MoO3:La1% (c) MoO3:La2%, (d) MoO3:La 3% (e) MoO3:La4% and (f) MoO3:La5% thin films.

4
R. Jansi et al. Optical Materials 145 (2023) 114464

Table 3
Optical bandgap values La doped MoO3 thin films.
La doping Bandgap (eV)
Concentration (%)

0 3.26
1 3.19
2 3.12
3 3.15
4 3.18
5 3.23

[40]. Also, it could be noticed that the size of reticulated nano-fibrous

Fig. 4. EDX spectrum of 2 wt % La doped MoO3 thin film.
Table 2
Elemental % of La doped MoO3 thin films.
La doping Elements (at.%)
Concentration (%)
Mo
0 34.67
1 33.72
2 32.78
3 32.60
4 30.54
5 29.68
increases with the substitution of La3+ dopants and the maximum size
was observed for the 2% La in MoO3 thin film sample with increased
porosity. The increased diameter might be due to the result of
substituting larger ionc radius of La3+ dopants in MoO3, increasing the
grain size and grain boundaries. These might play a vital in increasing
the adsorption of gas molecules [8,33,41].As a result, the 2% La doped
MoO3 film could be a better gas sensing material. When La dopant
concentration is increased further, reticulated nano-fibrous diameter
decreases with decreased porosity, indicating that grain size and
boundaries may be reduced, which might impair the ability of MoO3
thin films to detect gases.
Fig. 4 shows the elemental analysis of 2 wt% La doped MoO3 thin
film obtained by EDX. The Mo, O, and La elements have been present in
the spectrum. Atomic percentage of the La doped MoO3 thin films is
given in Table 2. At room temperature, the presence of oxygen in the
O La film typically helps the gas detecting process when in contact with
65.33 – certain gas molecules. The additional peaks are observed due to the glass
65.21 1.07 substrate [13,42].
65.14 2.08
64.28 3.12
65.22 4.24 3.3. Optical studies
65.18 5.14

Optical spectra were recorded for La doped MoO3thin films in the

thin film providing the greatest crystallite size, which is projected to be
advantageous for application in gas sensors. Also, the larger ionic radius
of the dopant leads to crystal lattice expansion causing the increase in
lattice parameters. The decrease in structural parameters with higher
concentration of dopants could be because of the existence of exotic La3+
ions inhibiting the growth of MoO3 with the production of numerous
nucleation centres and increasing the lattice strain [39].
3.2. Morphological study
The morphology of the MoO3 and La (1, 2, 3, 4 and 5 wt%) doped
MoO3 thin films are shown in Fig. 3(a -f). From the figure, it is observed
that, the prepared thin films has a reticulate nanofibrous mesh shape
wavelength ranging from 300 to 900 nm. In the visible region, both
undoped and La doped MoO3 thin films displayed better transparency.
The undoped MoO3 thin film was found to have a highest transparency
in the visible region and the transparency of La doped MoO3 thin films
starts to decrease as shown in Fig. 5a. Transmittance value decreases
with the increase of La dopants in MoO3 thin film due to the augmented
scattering of the incoming light due to increased defects such as oxygen
vacancies, increased crystallite size & thickness, improved density of
grain boundaries and enhanced reactivity among the La, Mo & O ions.
Sanalkumar et al. [38], used magnetron sputtering technique in devel­
oping Tb doped MoO3 thin films, resulted in a similar drop in trans­
mittance value due to the higher thickness value compared to pristine
sample.
The energy gap values were estimated using the Tauc’s relation

Fig. 5. A Transmittance spectrum and b’ (αhν)2vs photon energy (hν) curves (a) MoO3, (b) MoO3:La1% (c) MoO3:La2%, (d) MoO3:La 3%, (e) MoO3:La4% and (f)
MoO3:La5% thin films.

5
R. Jansi et al. Optical Materials 145 (2023) 114464

Where, hν indicates the photon energy, A represents the constant, α

denotes the absorption co-efficient, Eg indicates the optical energy gap
[30,43,44]. Tauc plots of Fig. 5b, shows the band gaps of 1,2,3,4 and 5
wt% La doped MoO3 thin films and the measured values are shown in
Table 3.The substitution of the La3+ ions, with greater ionic radius, re­
sults in the formation of defect sites and charge imbalances, which
broaden the valence band to decrease bandgap of the material [38]. In
addition, the increase in the concentration of the carriers leads to the
bandgap narrowing which is related to the increased film defects. The
minimum band gap of 3.12 eV is observed for 2 wt% La doped MoO3
[45]. When the percentage of dopants further increases, it results in an
increase in band gap for 3, 4 and 5% doping of La with MoO3.This in­
crease in band gap might be due to the decrease in crystallite size which
is similar to the other reported works [46,47]. In accordance with the
Burstein-Moss effect, as the carrier concentration increases, the lower
energy levels in the conduction band was filled with electrons, which
leads to a red shift in the Fermi level when doped with La up to 2%.
Further, increase in the La dopant concentration (i.e 3, 4 and 5% of La)
leads to blue shift in Fermi level which results in the increase in bandgap
[48,49]. Thus in our work, the variation in bandgap was attributed to
the structural effects induced by the introduction of La atoms in MoO3.
Fig. 6. Photoluminescence spectra of (a) MoO3, (b) MoO3:La1% (c) MoO3:
La2%, (d) MoO3:La 3%, (e) MoO3:La4% and (f) MoO3:La5% thin films.
3.4. Photoluminescence study

which is given below. Optical Characteristics of La doped MoO3 thin films such as, surface
(αhν)2 = A(hν − Eg) (6) states and oxygen vacancies can be estimated via photoluminescence
(PL) measurements. Fig. 6 showsthe PL spectra excited using 350 nm

Fig. 7. Time-dependent gas response (Current vs time) of (a) MoO3, (b) MoO3:La1% (c) MoO3:La2%, (d) MoO3:La 3%, (e) MoO3:La4% and (f) MoO3:La5% thin films.

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R. Jansi et al. Optical Materials 145 (2023) 114464

Table 4
Response and rise/decay time of La doped MoO3 thin films.
La doping Sensor Rise time (s) Decay time (s)
Concentration (%) Response

0 188 31 3.2
1 405 30 3.2
2 900 28 2.9
3 640 29 3.0
4 171 30 3.1
5 115 31 3.1

Table 5
Comparison of ammonia sensing performances of current work with earlier re­
ported works.
Material Operating Concentration Rise Decay Reference
temperature (ppm) Time Time
(s) (s)

MoO3 RT 500 210 240 [8]

MoO3:Pr RT 250 54 12 [24]
MoO3:Co RT 250 52 13 [33]
MoO3:Si RT 400 50 60 [58]
Fig. 8. Sensor response with error of La doped MoO3thin films. MoO3 RT 1 229 73 [54]
α- MoO3 RT 100 37 17 [59]
and an emission wavelength of La doped MoO3, measured between 350 MoO3 RT 500 15 300 [60]
Thin
and 600 nm at room-temperature. From this figure, six emission signals
films
395, 415, 437, 452, 478, and 522 nm were observed. The UV emission 2-D h- RT 5 69 129 [57]
peak around 395 nm was attributed to the near-band edge emission MoO3
(NBE) caused due to the free-exciton recombination in the prepared thin MoO3:La RT 250 28 2.9 This work
films. The visible light emission around (415 nm (Violet), 437 nm (Blue),
452 & 478 nm (Bluish green), and 522 nm (Green)) could be attributed
facilitates more adsorption sites. Moreover, defects due to oxygen va­
to the deep level emissions caused by the dopant ions in host MoO3. The
cancies also play a vital role in improving the sensing response during
peaks are caused by deep level emission from several Mo5+ d-d transi­
their interaction with NH3. The variation in current was high for 2% of
tions, which symbolises the intra-band radioactive recombination. The
La doped MoO3 film might be due to the presence of more adsorp­
emission peaks around 437 nm are produced due to recombination of e−
tion/reactive sites because of the porous morphology. Additionally, our
and h+ in MoO3 crystals due to the hexa-coordinated [MoO6]5+ dz2 − dyz
PL data confirmed, 2% of La doped MoO3 film was found to have a
transitions. The [MoO5]5+ penta-coordinated dyz − dxz transition might
moderately higher level of oxygen-related defect, suggesting that more
be the cause for the rise in the near band edge emission at 480 nm [30,
oxygen adsorption could take place in the film. Thus, La dopants in
50]. Moreover, the green emission peak around 522 nm can be directly
MoO3 might release additional electrons into the conduction band of
attributed to a recombination of e− and h+ due to ionized oxygen va­
MoO3 and interact with chemisorbed oxygen species more often,
cancies [51]. The maximum intensity was reported for the 2% La doped
increasing the electrical responsiveness of ammonia gas [52].
MoO3 thin film with a slight red shift in the emission peaks compared to
The gas response of the films was determined using the equation
other thin films, due to increased crystallite size and presence of addi­
tional oxygen vacancies in MoO3 thin films. The decrement in the S=
Ig
(7)
emission peaks at higher concentrations (i.e 3, 4 & 5 wt%) might be due Ia
to the quantum confinement caused by the decrease in crystallite size of
the samples confirmed by our XRD results. The sample with the Where S is gas response, Ia is current in air(atmosphere) and Ig is current
maximum intensity was 2 wt% La doped MoO3, which may offer better in the presence of NH3 [32], [53]. Fig. 8, shows the variation of the gas
responsiveness towards the analyte gas. sensing response with error of La doping concentration in MoO3 films. It
can be seen that 2% La doped MoO3 shows maximum gas sensing
response of about 900 than the other films.
3.5. Gas sensing studies
3.5.1. Rise and decay time
MOS, exhibit varied electrical properties based on the adsorption of Raise time and decay time are the critical properties in determining
certain gas molecules. Usually, crystalline size, surface roughness, con­ the quality of gas sensors. The ts is the time taken by the current to attain
centration of dopants, surface defects and porosity of the surface affect 90% when exposed to target gas, and the tr is the time taken by the
the MOS sensing response [32].In this work, different volatile organic current to decay 90% to its original value when the target gas was cutoff.
compounds (VOCs) have tried to analyse the sensing performance of the Fig. 7, displays current vs time for (1, 2, 3, 4 and 5)wt.% La doped MoO3
sample such as methanol, toluene, isopropanol, acetone, ethanol, and with NH3 gas. The raise time and decay time are tabulated in Table 4,
ammonia (NH3) with the concentration of 50 ppm, in which ammonia The shortest raise time and decay time are 28 s and 2.9s respectively for
gas produced high response compare with other compounds. NH3 gas 250 ppm NH3 for the 2% La doped MoO3 film in comparison with the
was carried out with 5 different concentrations of 50, 100, 150, 200 and other film. At higher concentrations, the chemisorbed air oxygen on the
250 ppm at room temperature (Fig. 7). In terms of rise and decay time, MoO3 surface desorbs more quickly, reducing the decay time. The re­
the sensing capability of undoped MoO3 and MoO3 doped with La was sults show that, the La doped MoO3 thin film present extremely high
investigated for various NH3 concentrations. Undoped and La doped responses, comparatively low working temperature, and low detection
MoO3 films exhibit a dramatically increase in electrical current when limit than others. To date, there were no reports available on La doped
NH3 concentration was increased. Generally, doping of ions facilitate MoO3 thin film sensors at ambient temperature prepared using NSP
lattice defects in host, this result in the extrinsic electronic state which

7
R. Jansi et al.
Fig. 9. Gas sensing mechanism of the prepared La doped MoO3 thin film sensors.
method. Gas sensing performances to NH3 between this study and those
published in literature shown in Table 5.
3.5.2. NH3 sensing mechanism
In order to understand sensing mechanism of MOS sensor,
adsorption-desorption process was often employed [49,54,55]. One of
the primaries which causes for change in electrical property of sensors is
contribution of oxygen. Under oxygen atmospheric conditions, at the
grain boundaries, potential barrier widens because of O−2 , O− , O2−
(ionized atmospheric oxygen), a depletion layer is formed by trapping
electrons from the surface of MOS, resulting in a drop in overall con­
ductivity. When NH3 gas is supplied, interestingly a reverse phenome­
non occurs (i.e.) as the interaction between adsorbed oxygen species and
electron increases, height of the barrier is reduced and thereby con­
ductivity is increased. This observance was in accordance with previous
report [44–47]. Fig. 9, depicts the schematic diagram of sensing
mechanism.
The reaction in mechanism of gas sensors is represented in the
following equations
2MoO3 + 2e− →2(MoO3 )O−2 (8)
2NH3 (adsorbed) + 4(MoO3 )O−2 −
→ 4MoO3 + N2 + 6H2 O + 3e (to MoO3 )
(9)
The raise in the current value in relation to the NH3 gas occurs while
the electrons are liberated from the negatively charged adsorbed oxygen
sites. Table 5 compares the measured gas sensing responses and other
characteristics to previous reports to demonstrate the importance and
necessity of the current endeavour. The 2% La doped MoO3 film exhibits
higher sensor response and a quicker rise time than previously published
values for metal oxide sensors at ambient temperature and at various
operation temperatures [56,57]. From the aforementioned results, the
fabricated La doped MoO3 thin film sensor might perform effectively to
identify NH3 gas leakage in a variety of situations based on a thorough
evaluation of the existing work. The gas sensing performance was
measured after three months period and limited drift in the sensor
response was observed for all the samples which confirm the stability of
the sample. It asserts that the varied atmospheric conditions doesnot
have an impact on the interaction of NH3 gas molecules with La doped
MoO3. Our La doped MoO3 based samples showed increased respon­
siveness and stability to NH3 vapour when employed at room temper­
ature. This demonstrates that the best-performing 2% La doped MoO3
thin film sensor would be better suited for use in commercial sensor
devices for environmental and air quality surveillance, early detection of
fire & explosion, agriculture, automobile emissions, and water quality
monitoring.
8
Optical Materials 145 (2023) 114464
4. Conclusion
Pristine MoO3 and La doped MoO3 thin films were coated using the
nebulizer assisted spray pyrolysis method and the fabricated samples
were studied for the ammonia gas sensing performance for the first time.
MoO3 and La doped MoO3 thin films exhibited monoclinic structure and
confirmed by XRD analysis. At room temperature, the synthesized
samples exhibited six significant conspicuous PL emission peaks posi­
tioned at 395, 415, 437, 452, 478, and 522 nm, which correspond to the
different defect levels. The La doped MoO3 thin film optical measure­
ments revealed a decrease in transmittance, smaller bandgap of 3.12 eV,
increased lattice defect and surface defects leading to the generation of
more oxygen vacancies as well. The rise and the decay time is 28 s and
2.9s respectively for the 2% La-doped MoO3 film at 250 ppm NH3. Thus,
the study revealed that the La doping improved the physical and sensing
characteristics of the MoO3 film with improved reaction times, sensor
response, durability and stability for fast and continuous NH3 detection
in commercial use as gas sensors better suited for various industrial,
environmental and household applications.
CRediT authorship contribution statement
R. Jansi: Writing – original draft, Writing – review & editing,
Conceptualization. M.S. Revathy: Writing – original draft, Writing –
review & editing, Conceptualization. S. Vinoth: Conceptualization,
Formal analysis. Anuj Kumar: Conceptualization, Formal analysis. R.S.
Rimal Isaac: Conceptualization, Formal analysis. N. Deepa: Concep­
tualization, Formal analysis. Abdullah M. Al-Enizi: Conceptualization,
Methodology, Formal analysis. Mohd Ubaidullah: Conceptualization,
Methodology, Formal analysis. Bidhan Pandit: Formal analysis, Su­
pervision. Mohd Shahazad: Formal analysis, Supervision. Manish
Gupta: Formal analysis, Supervision.
Declaration of competing interest
We declare that, there is no conflict of interest.
Data availability
The raw/processed data required to reproduce these findings cannot
be shared at this time as the data also forms part of an ongoing study.
Acknowledgement
The authors extend their appreciation to the Deputyship for Research
and Innovation, Ministry of Education in Saudi Arabia for funding this
research work through the project no. (IFKSUOR3–025–3).
R. Jansi et al. Optical Materials 145 (2023) 114464

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