Synthesis and Characterization of SnO2 and T iO2

Nanoparticles For Sensor Application

Akansha Singh Ankitha T M Sahana
Department of ECE Department of ECE Department of ECE
Siddaganga Institute of Technology Siddaganga Institute of Technology Siddaganga Institute of Technology
Tumakuru, Karnataka, 572103, India Tumakuru, Karnataka, 572103, India Tumakuru, Karnataka, 572103, India
[email protected] [email protected] [email protected]

Sai Shree Bindu B T O Geetha Rani

Department of ECE Department of ECE
Siddaganga Institute of Technology Siddaganga Institute of Technology
Tumakuru, Karnataka, 572103, India Tumakuru, Karnataka, 572103, India
[email protected] [email protected]

Abstract—Air pollution is a serious problem caused by in- II. R ELATED W ORK

creased industrial activity, vehicle emissions, population growth,
and agricultural practices, all of which endanger human health. Author Nitu Singh et al. in the paper [1] has discussed the
Emissions emit hazardous compounds into the environment, development of T iO2 /SnO2 nanoparticles for gas sensing.
causing pollution and deterioration in air quality. It is critical to
develop gas sensors that are both efficient and selective. This Then exposure to ammonia boosted photoluminescence
project uses the combustion synthesis method to create and intensity without altering the peak position. This raises the
characterize T iO2 -SnO2 nanoparticles, which has advantages possibility of optical gas sensing. The interaction between
such as ease of implementation, efficiency, and environmental ammonia with nanoparticles resulted in speedier response
benefits. The nanoparticles have excellent gas-sensing properties times. Thus, T iO2 /SnO2 nanoparticles hold promise as
and are extensively characterized. Gas sensing devices are made
with optimized nanoparticle compositions, and their performance quick-responding optical sensors for detecting ammonia at
in detecting target gases like ammonia and carbon monoxide from ambient temperature.
vehicle exhaust is measured using an amperometric circuit.
E. Chinarro et al. in the paper [2] has explained the
I. I NTRODUCTION synthesized (1-x)T iO2 -xSnO2 ceramics with x ranging from
Nanoparticles of SnO2 and T iO2 play a vital role in 0.05 to 0.30 via combustion synthesis. After sintering at 1450
several applications due to their unique nucleation and growth °C, they produced a single T iO2 -SnO2 rutile phase. SEM
characteristics, which greatly influence size, shape, and crystal investigation indicated homogeneous microstructures with
structure. Their amazing surface-to-volume ratio, small size, decreasing grain sizes as the SnO2 level rose. Impedance
increased surface area, porosity, and superior mechanical qual- spectroscopy revealed several conduction methods, with
ities provide them a considerable advantage over bulk materi- x=0.05 and x=0.30 indicating electronic band conduction.
als, especially in catalytic applications and organic synthesis, At 700 °C, conductivity peaked at x=0.10, indicating that
where nanoparticles easily spread without aggregation. semiconducting T iO2 rutile was doped with SnO2 . The
SnO2 and T iO2 nanoparticles have numerous applications, work reveals the link between electrical properties and the
including photocatalysis, solar cells, photovoltaic cells, gas T iO2 -SnO2 phase diagram, which allows for the discovery
sensors, electrochemical sensors, drug delivery, hyperthermia, of a narrow spinodal decomposition effect.
biosensing, and nanomedicine.
Sol-gel, chemical vapor deposition, laser ablation, sono- In [3] Author F.A. Deorsola et al. has studied the gel
chemical, and hydrothermal processes are all used to synthe- combustion to create nano T iO2 and SnO2 powders with
size nanoparticles. The combustion approach ensures appropri- large surface areas (>100 m2 /g) and small diameters (50
ate crystal alignment and necessitates high temperatures and nm) for solid-state gas sensors. T iO2 sensors demonstrated
pressures, resulting in regulated nanoparticle formation. quick resistance shifts around the stoichiometric air-fuel
This project tries to synthesize the developed design of ratio, making them appropriate for monitoring vehicle oxygen
SnO2 and T iO2 nanoparticles for better gas sensing capa- levels. Pt-added sensors demonstrated increased sensitivity
bility. The synthesis methodologies, characterization methods, and selectivity for carbon monoxide, indicating a viable
gas sensing evaluation, result analysis, and practical applica- application for detecting ethanol breath. SnO2 sensors
tion implications will all be thoroughly described. responded linearly to varying ethanol concentrations. Overall,
gel combustion successfully generated nano metal oxide 2.5 to 17 nm in diameter. Surface area, porosity, acidity,
materials with the necessary gas-sensing properties. and phase composition all have a substantial impact on
photocatalytic and sorption capabilities. Crystalline T iO2
The author M. Radecka et al. in [4] has introduced the has more photocatalytic activity, whereas amorphous T iO2
study of nanocrystalline T iO2 /SnO2 composites for ammonia has better adsorption properties. The study emphasises the
detection, which were synthesised from commercially importance of precursor selection and synthesis conditions in
available metal oxide nanoparticles. The 50 mol% SnO2 /50 tailoring T iO2 nanomaterial performance.
mol% T iO2 composition demonstrated optimum N H3
sensing capabilities, with reversible changes in electrical Author Sandip M. Deshmukh et al. in the paper [9]
resistivity after ammonia exposure. Thermal stability was discusses the synthesis of T iO2 -SnO2 nanocomposites via
assessed using mass spectrometry and thermal analysis to urea-assisted thermal breakdown. Analytical approaches
guide gas sensor production settings. This emphasises the confirm that T iO2 and SnO2 can create heterojunctions
value of composite design and thermal stability in gas sensor efficiently. The optimised nanocomposite exhibits higher
development. photostability and photocatalytic activity than pure T iO2
and SnO2 , particularly when degrading methyl orange dye
A study in [5] by the author investigated using solution under UV light. The higher performance is attributed to
combustion synthesis (SCS) to produce T iO2 nanopowders greater separation of photogenerated charge carriers and
as photoelectrodes for dye-sensitized solar cells (DSSCs). increased light absorption enabled by the heterojunction. The
These powders, containing impurities of C and/or S, absorbed study’s simple synthesis process shows potential for creating
visible light and had reduced band gaps compared to pure efficient mixed-metal-oxide nanocomposite photocatalysts for
T iO2 and commercial Degussa P25 T iO2 . While some environmental remediation.
parameters, such as open-circuit voltage and fill factor,
remained consistent, others, like short-circuit current and In [10] author Jinbiao Jia et al. has introduced a combus-
efficiency, were influenced by factors. tion approach for generating high-performance SnO2 elec-
tron transport layers (ETLs) in perovskite solar cells (PSCs).
The author Nitu Singh et al. in [6] describes a new method The combustion-derived SnO2 ETL outperforms existing ap-
for producing titanium dioxide (T iO2 ) nanoparticles for proaches in terms of electron mobility, resulting in a 19.12%
application in photocatalysis. When titanium particles and power conversion efficiency (PCE). Adding Nd3+ ions to the
sodium perchlorate were ignited, researchers discovered that SnO2 layer further improves performance, resulting in a PCE
particle size affected the shape and structure of the T iO2 of 20.92% with little hysteresis. These benefits are attributable
created. Smaller titanium particles (10 m) produced irregular to increased electron extraction and transport capacity, as
rutile phase nanoparticles, while larger ones (25 m) produced well as reduced interfacial recombination, which is helped by
spherical anatase phase nanoparticles. Despite having a combustion synthesis and Nd3+ doping.
smaller surface area, the rutile-rich sample demonstrated
higher photocatalytic activity in methanol dehydrogenation
III. METHODOLOGY
and acetic acid oxidative breakdown than the anatase-rich
sample. This shows that T iO2 nanoparticle characteristics In this section, the synthesis, characterization, and fabrica-
can be tailored using combustion synthesis by altering the tion processes of SnO2 and T iO2 are discussed.
size of the titanium particles.

The author F. A. Deorsola et al. in [7] describes utilising

gel combustion to create nanoscale titanium dioxide (T iO2 )
particles. Titanium tetraisopropoxide serves as a precursor
for the combustion of hydrogen peroxide. The resultant
nanoparticles are around 20 nm in size and have a poor
crystallinity. Various thermal treatments’ effects on structure
and size are investigated, and 300 °C is shown to be the best
for creating pure anatase T iO2 nanopowders with a large
surface area (115 m2 /g) and increased crystallinity. This
emphasises the significance of composite design and heat
stability in these procedures.

In [8] author Tetiana Dontsova et al. study investigates

how precursor type and sol-gel synthesis factors affect the Fig. 1. Block diagram of synthesis of SnO2 -T iO2 nanoparticles using
characteristics of T iO2 nanopowders. XRD and electron combustion method.
microscopy indicate nanocrystalline features measuring
A. Nanoparticle Synthesis electrical characterization and assessment of their sensing
Figure 1, outlines a process for evaluating nanoparticles performance towards target gases.
suitability for gas sensor applications. It begins with Three devices are fabricated using 1.01 g of nanoparticles.
synthesizing nanoparticles using the combustion method, Each device possessed an external diameter of 5.98 mm and
followed by a thorough characterization of their structure, an internal diameter of 5.2 mm. Ethanol served as the binding
optical properties, and electrical properties. The final step agent for the nanoparticles, and the devices were dried for
involves testing the nanoparticles sensitivity to specific gases one hour after assembly. To establish electrical connections,
and determining their effectiveness as gas sensors. two diametrically opposed holes were drilled into each
device. These holes were subsequently fitted with aluminum
The synthesis, fabrication of gas sensing devices, and char- or copper wires, with copper being the preferred choice.
acterization of nanoparticles are discussed in this section. The nanoparticle material (1.01 g total) was loaded into
the devices and thoroughly mixed to ensure a homogenous
B. Nanoparticles Synthesis composite. The fabricated device is exposed to ammonia gas
Titanium isopropoxide and Tin (II) oxalate are mixed as under controlled conditions as the gas interact with the sensor
the precursors, along with urea as the fuel, in the desired material, they induce changes in the electrical properties
stoichiometric as shown in equation 1. Here, x ranges from of the material. These changes are recorded as variations
0.05 to 0.50. in electrical resistance using an amperometric circuit. Fig.3
(1 − x)T iO2 − xSnO2 (1) presents an image of the final devices obtained using this
compact fabrication method.
Six distinct T iO2 -SnO2 nanoparticle compositions
were synthesized: (a) 95%T iO2 –5%SnO2 (500 °C), (b)
90%T iO2 –10%SnO2 (380 °C), (c) 70%T iO2 –30%SnO2
(280 °C), (d)95%T iO2 – 5%SnO2 (380 °C), (e) 70%T iO2 -
20%SnO2 -10%CuO (380 °C), (f) 50%T iO2 –50%SnO2 (500
°C) via the combustion method and calcined at 600 °C as
shown in Figure 3.2. A fixed amount of 5 g urea and 50 mL
water were employed as fuel and solvent, respectively, for all
syntheses. Notably, composition (e) used cupric nitrate as a
dopant to study its effects on nanoparticle characteristics. The
combustion reaction produced porous, yellow-white foam-like
substance. This as-prepared product was simply ground into Fig. 3. Fabricated nanodevice for ammonia gas sensing.
a fine, homogeneous powder before being calcined at 600 °C.

Fig. 4. Fabricated nanodevice for carbon monoxide gas sensing.

Three completely packed devices as shown in Fig. 4 are

fabricated and holes are drilled on the surface for vehicle
Fig. 2. Block diagram of synthesis of SnO2 -T iO2 nanoparticles using exhaust (CO) exposure. Two holes are drilled diametrically
combustion method.
and fitted with aluminum or copper wires, preferably copper,
and a total of 1.01 g of nanoparticles is filled into the devices.
C. Device fabrication using the compact method The fabricated device is exposed to vehicle exhaust under
Fabricating a device is a crucial step in evaluating the controlled conditions as the gas interacts with the sensor
practical applicability of the synthesized nanoparticles for material, they induce changes in the electrical properties of the
gas sensing applications. It enables the integration of the material. These changes are recorded as variations in electrical
nanoparticles into a functional gas sensor setup, facilitating resistance using an amperometric circuit.
D. Characterization of nanoparticles as lattice parameter, crystalline structure, phase, and the crys-
A suite of characterization techniques is employed to talline size. Peak intensity in XRD indicates the position of
comprehensively analyze the synthesized materials. Scanning the atoms and the electron density inside the unit cell, the
electron microscopy (SEM) is used to study surface mor- peak positions indicate the translation symmetry form and size
phology, particle size distribution, and particle shape. X- of the particles. This technique is not suitable for amorphous
ray diffraction (XRD) investigation helps to understand the materials and small particles below 3 nm because the peaks
crystal structure, phase composition, and identification of any of XRD are too wide. The crystallite size of the synthesized
existing crystalline phases. Furthermore, energy-dispersive X- nanoparticles is estimated using the Scherrer formula as given
ray spectroscopy (EDX) combined with SEM offers elemen- by,
kλ
tal composition data, indicating the types and quantities of D= (2)
β cos(θ)
elements present in the sample. This information helps you
understand the material’s structure and qualities. Finally, UV- k is the particle shape factor = 0.89
visible (UV-Vis) spectroscopy can be used to investigate the λ is the X-ray wavelength = 0.15406
optical properties of the produced materials. β is the full-width at half maximum height (FWHM) in radians
θ is the diffraction angle
IV. C HARACTERIZATION T ECHNIQUES λ and β should be determined from the graphs.
In this section, the synthesized T iO2 -SnO2 nanoparticles In this project XRD is employed to determine the crystal
are characterized by the X-ray diffraction method (XRD), structure, phase composition, and chemical composition of
Scanning electron microscopy (SEM), Energy-dispersive X- materials. X-rays are directed at the sample, and the result-
ray spectroscopy, and UV-visible spectroscope and the results ing diffraction pattern provides information about the crystal
are observed for suitable gas sensing properties. lattice structure. This allows the identification of crystal phases
and the determination of their relative abundance.
A. Scanning electron microscopy (SEM)
D. UV-Vis spectroscopy
SEM stands for Scanning Electron Microscopy, which is
A UV spectroscope, or ultraviolet-visible (UV-Vis) spec-
a type of electron microscopy used to observe the surface
trophotometer, is a scientific instrument used to measure the
structure of a sample at high magnification. SEM works by
absorption of ultraviolet and visible light by a sample. It
scanning a focused electron beam over the sample surface,
operates by passing a beam of UV or visible light through
which interacts with the atoms in the sample and produces
a sample and measuring the intensity of light transmitted
signals that can be used to form an image of the sample sur-
through the sample as a function of wavelength. The amount of
face. It is mainly used for morphological study of nanoparticles
light absorbed by the sample at different wavelengths provides
and thin films. In this project, SEM is utilized to examine the
information about its chemical composition and concentration
surface morphology, shapes, and size distribution of particles.
of absorbing species. UV spectroscopy is widely used in
A focused electron beam scans the surface of the sample, gen-
various fields such as chemistry, biochemistry, and materials
erating high-resolution images. Secondary electrons emitted
science for quantitative and qualitative analysis of substances,
from the sample’s surface provide detailed information about
determining molecular structure, and studying reaction kinet-
the sample’s topography.
ics.
B. Energy-dispersive X-ray spectroscopy (EDS) UV-Vis spectroscopy is particularly useful for gas sensing.
Researchers can learn about the interaction between gas
Energy-dispersive X-ray spectroscopy (EDS or EDX) is an molecules and sensing materials by measuring changes in
analytical technique used for identifying the elemental com- the absorbance spectrum after being exposed to a gas. This
position of materials. It works by detecting the characteristic knowledge is useful in the design and development of gas
X-rays emitted by a sample when bombarded with high-energy sensors with specific sensitivities.
electrons or X-rays. EDS provides qualitative and quanti-
tative information about the elements present in a sample, V. R ESULT AND D ISCUSSION
their relative concentrations, and their distribution across the In this section, the results of the proposed method are
sample surface. This technique is widely used in fields such shown.
as materials science, metallurgy, geology, and forensics for
elemental analysis, phase identification, and microstructural A. X-ray diffraction
characterization. In this project EDX is utilized to reveal the X-ray diffraction (XRD) patterns for six distinct compo-
types and amounts of elements present. This helps in the sitions of SnO2 -T iO2 nanoparticles synthesized at varied
analysis of a material’s structure and properties. temperatures and compositions are shown in Figure 5.1.
In these XRD patterns, the x-axis represents the diffraction
C. X-ray diffraction (XRD) angle (2θ) in degrees, and the y-axis represents the intensity of
XRD is the most common characterization technique used the diffracted X-rays. The peaks in the patterns correspond to
to figure out morphology and crystallographic structure such the diffraction of X-rays from specific crystallographic planes
within the material, and their positions and intensities provide
information about the crystal structure and phases present in
the sample and crystalline size (D) is calculated by using the
Debye Scherrer formula given by the Eq. (5.1):
kλ
D= (3)
β cos(θ)
In this case, k and λ are constants with values of 0.89 and
0.1546 nm, respectively. β is the full-width at half maximum
height (FWHM) in radians and θ is the diffraction angle which
are determined using the XRD patterns of the compositions.

Fig. 7. XRD pattern of 70%T iO2 –30%SnO2 (280°C).

Fig. 5. XRD pattern of 95%T iO2 –5%SnO2 (500°C).

Fig. 8. XRD pattern of 95%T iO2 –5%SnO2 (380°C).

β = 0.97 nm
D = 12.44043489 nm
Fig. 6 is the XRD plot of the composition
90%T iO2 –10%SnO2 , this pattern exhibits several well-
defined sharp peaks, suggesting a highly crystalline material
with a specific crystal structure.
θ = 77.24848
β = 0.94484 nm
D = 10.75963692 nm
Fig. 7 is the pattern of the composition
Fig. 6. XRD pattern of 90%T iO2 –10%SnO2 (380°C). 70%T iO2 –30%SnO2 , this pattern displays multiple intense
and sharp peaks, indicating the presence of multiple crystalline
The following observations are made from the XRD pat- phases or a complex crystal structure.
terns: θ = 81.469275
Fig. 5 is the XRD plot of the composition β = 0.97 nm
95%T iO2 –5%SnO2 (500°C) nanoparticles, this pattern D = 11.70835232 nm
shows a few broad peaks, indicating the presence of a Fig. 8 is the composition of 95%T iO2 –5%SnO2 (380°C),
crystalline phase with small crystalline size. Using the Debye the pattern shows a combination of sharp and broad peaks,
Scherrer formula as shown in Eq. (5.1) and substituting the suggesting a mixture of well-crystallized and less-ordered or
values of k, λ, θ, and β we obtain the crytalline size (D): smaller crystallite phases.
θ = 48.825 θ = 13.01249
β = 0.94484 nm SnO2 (JCPDS No. 77-0452). This suggests the co-
D = 9.319741121 nm existence of these crystalline phases in the synthesized
T iO2 –SnO2 nanoparticles. The calculated crystalline size of
the nanoparticles after calcination at 600 °C was determined
to be 11.31 nm. Interestingly, among all the investigated
compositions, the one containing 70%T iO2 –20%SnO2 -
10%CuO exhibited the most pronounced reflections
corresponding to the rutile phases of T iO2 and SnO2
as evidenced by the best agreement with both JCPDS
reference patterns. Compared to all other graphs sample
70% T iO2 –20%SnO2 -10%CuO has the best match with the
standard JCPDS No.21-1276, and JCPDS No. 77-0452. The
peaks of the graph closely match with the standard peaks of
T iO2 and SnO2 nanoparticles.

VI. UV V IS -S PECTROSCOPY
The UV-Vis spectrum depicts the properties of light absorp-
tion of nanoparticles utilized in gas-sensing applications. The
Fig. 9. XRD pattern of 70%T iO2 –20%SnO2 -10%CuO (380°C).
potential energy of the reactant molecules is represented by
the red line in the graphs (F (R).hv)2 vs photon energy, and
the potential energy of the product molecules is represented
by the black line. The point where the two curves cross is the
activation energy, which is the minimum amount of energy
required for the reaction to proceed.

Fig. 11 depicts a pronounced upsurge at an energy level of

3.3 eV. The portion of the curve below this value exhibits
a relatively featureless characteristic, signifying a minimal
value of the quantity being graphed. Conversely, the curve
demonstrates a marked escalation beyond 3.3 eV, implying a
substantial augmentation in the plotted quantity for energies
surpassing this threshold value.

Similar to Fig. 11, Fig. 12 manifests a pronounced upsurge

at an energy level of 2.7 eV. However, subsequent to this ini-
tial, sharp escalation, the curve exhibits a series of oscillations
Fig. 10. XRD pattern of 50%T iO2 –50%SnO2 (500°C).
or fluctuations. This observation suggests a considerably more
intricate behavior of the plotted quantity at energies exceeding
Fig. 9 is the composition of 70%T iO2 –20%SnO2 -
the threshold value.
10%CuO, the pattern exhibits a few broad peaks, similar to
Figure 5.1, indicating a less crystalline or more disordered In Fig. 13 the sharp edge occurs at a slightly higher energy
phase. of around 2.8 eV. Below this onset energy, the curve is
θ = 73.5 relatively flat, while above 2.8 eV, it rises steeply, indicating
β = 0.97 nm a significant increase in the plotted quantity. The shape of the
D = 12.15994112 nm curve above the onset energy is smoother compared to Figure
Fig. 10 is the composition of 50%T iO2 –50%SnO2 , this 5.8, without the oscillations or fluctuations.
pattern shows several sharp and intense peaks, indicating a
highly crystalline material with a specific crystal structure, Fig. 14 shows a sharp increase in the photoionization cross-
similar to Figure 5.2. section at around 2.2 eV, which likely corresponds to the
θ = 77.51 ionization energy or threshold energy required to remove an
β = 0.97 nm electron from the atom or molecule being studied.
D = 12.32971902 nm
Fig. 15 shows the sharp increase in the photoionization
X-ray diffraction (XRD) analysis revealed a close match cross-section occurs at a slightly lower energy of around 2.1
between the obtained peaks and the reference patterns eV, suggesting a different atomic or molecular species with a
for both rutile T iO2 (JCPDS No. 21-1276) and rutile lower ionization energy.
Fig. 11. UV-vis spectrum of 95%T iO2 –5%SnO2 (500°C). Fig. 13. UV-vis spectrum of 70%T iO2 –30%SnO2 (280°C).

Fig. 12. UV-vis spectrum of 90%T iO2 –10%SnO2 (380°C). Fig. 14. UV-vis spectrum of 95%T iO2 -5%SnO2 (380°C).

In Fig. 16, a notable surge in the photoionization cross-

section becomes evident at approximately 2.1 eV, suggesting Table 1 comprehensively details the bandgap energies for
a correspondingly elevated ionization energy for the depicted each of the six synthesized material compositions. A dimin-
atom or molecule. This sharp rise signifies the energy threshold ished bandgap signifies a lessened energy barrier that must be
required to liberate an electron from the species under study, overcome for electron excitation to occur within the material.
implying a more robust binding force within its atomic or As a direct consequence of this, these materials possess the
molecular structure. capability to absorb photons of lower energy or exhibit a
propensity for more facile interaction with gas molecules. In
layman’s terms, a narrower bandgap translates to a requirement
TABLE I of less energy to induce excitation, a phenomenon that can
C OMPOSITION AND BANDGAP OF T iO2 -SnO2 NANOPARTICLES . often be achieved by visible light or even thermal energy.
Sl.No. Composition Bandgap
When a gas molecule comes into contact with the surface of
1. 95% T iO2 - 5% SnO2 3.3 eV the nanoparticle, it has the potential to either donate or accept
2. 90% T iO2 - 10% SnO2 2.7 eV electrons, thereby inducing a measurable alteration in the
3. 70% T iO2 - 30% SnO2 2.8 eV material’s conductivity. Crucially, this change in conductivity
4. 95% T iO2 - 5% SnO2 2.2 eV
5. 70% T iO2 - 20% SnO2 - 10% 2.1 eV offers a measurable response that can be effectively utilized
CuO to signal the presence of the target gas. As corroborated by
6. 50% T iO2 - 50% SnO2 2.1 eV the data in Table 5.1, the latter three compositions, designated
as 4, 5, and 6, exhibit the minimal bandgap values, rendering
them especially well-suited for applications in gas sensing.
Fig. 17. SEM images of synthesised SnO2 and T iO2 nanoparticles.

Fig. 15. UV-vis spectrum of 70%T iO2 -20%SnO2 -10% CuO (380°C).

Fig. 18. EDX image of 95%T iO2 –5%SnO2 (500 °C).

levels. These peaks correspond to the characteristic electronic

transitions of the elements present within the sample. The
Fig. 16. UV-vis spectrum of 50%T iO2 -50%SnO2 (500°C). intensity of each peak, quantified by its height, is directly
proportional to the concentration of the corresponding element.
By meticulously analyzing the peak positions, we can confi-
VII. SEM-EDX DATA dently identify the elements present in the sample, which in
this case include titanium (Ti), tin (Sn), and oxygen (O).
The morphology of the synthesized nanoparticles using a
high-resolution SEM image is shown in Figure 5.13, offering This elemental composition strongly suggests the presence
a magnified view (>x1000) of the nanoparticle assembly. The of titanium dioxide (T iO2 ) and tin dioxide (SnO2 ) com-
grayscale image captures the morphology of the nanoparticles. pounds within the sample.
The field of view, denoted as 20 µm and 10 µm suggests the
nanoparticles are smaller than 20 µm and 10 µm in size. A. IV analysis
Following the device fabrication process, Fig. 21 illustrates
Additionally, the 95%T iO2 -5%SnO2 sample has a tetrag- the gas sensing setup employed for characterization. This
onal grain, whereas the 70%T iO2 -20%SnO2 -10%CuO and setup utilizes Keithley Standard Series 2400 Source Measure
50%T iO2 -50%SnO2 samples have more circular grain struc- Unit (SMU) instruments, which boast high-precision voltage
tures. Furthermore, tetragonal nanoparticles show better for and current sourcing/loading capabilities alongside accurate
gas-sensing capabilities than spherical ones. This is because measurement functions across all four quadrants of the I-V
the flat faces of tetragonal particles create a higher surface area plane. In essence, each SMU instrument functions as a highly
compared to the smooth sphere. More surface area allows for stable DC power source and a dependable 6½-digit multimeter.
more interaction between the gas and the sensing material, The gas sensing mechanism itself leverages an
leading to potentially better sensitivity. amperometric circuit configuration, specifically designed
The X-ray spectra presented in Figures 5.14, 5.15, and to detect target gases such as ammonia (N H3 ), and carbon
5.16 exhibit a series of distinct peaks at varying energy monoxide (CO) present in vehicle exhaust. Fig. 22 depicts
Fig. 19. EDX image of 70%T iO2 –20%SnO2 -10%CuO (380 °C). Fig. 21. Keithley meter for gas sensing.

Fig. 22. I-V analysis of nanodevices for (a) 95%T iO2 –5%SnO2 (500°C), (b)
70%T iO2 –20%SnO2 -10%CuO, (c) 50%T iO2 –50%SnO2 compositions.

Fig. 20. EDX image of 50%T iO2 –50%SnO2 (500 °C).

the complete detection system, which incorporates pairs of

electrodes with a constant 5V bias voltage applied across
them.
In Fig. 23, 24, and 25, the graphs depict the current-time
response of SnO2 -T iO2 nanoparticles with different gases
exposed to determine the sensitivity of these nanoparticles to Fig. 23. I-V characterization of the fabricated devices 95%T iO2 -5%SnO2
different gases. for no gas.

In Fig. 25, the graph shows time-resolved signals of SnO2

and T iO2 nanoparticles when exposed to vehicle exhaust
(CO). The nanoparticles display a sharp, rapid rise in signal,
indicating strong and quick interaction with CO molecules.
The time-resolved analysis provides insights into the nanopar-
ticles gas-sensing potential, crucial for effective detection
and monitoring applications requiring rapid and distinctive
responses.
In summary, the above I-V graphs for the composition
of 95%T iO2 –5%SnO2 at (500°C), Fig. 24 illustrating the
current-time response to ammonia gas exposure, stands out as Fig. 24. I-V characterization of the fabricated devices 95%T iO2 -5%SnO2
it directly showcases the nanoparticles sensitivity and potential for ammonia gas.
for gas sensing applications, offering valuable insights for
signal indicative of rapid optical response, likely influenced by
factors like charge carrier generation. Time-resolved analysis
offers insights into nanoparticle behaviors, crucial for under-
standing their applications in optoelectronics, photocatalysis,
or sensing. In Fig. 27, Fig. 28, and Fig. 29 the graphs show

Fig. 25. I-V characterization of the fabricated devices 95%T iO2 -5%SnO2
for carbon monoxide.

sensor performance evaluation and material sensitivity to target

analytes. A comparison of the change in current of 95%T iO2 -
5%SnO2 for various gases is presented in Fig. 26. The graph
indicates that the nanoparticles are more sensitive to ammonia Fig. 28. I-V characterization of the fabricated devices 70%T iO2 -20%SnO2 -
10%CuO for ammonia gas.
gas.
tracking how SnO2 -T iO2 nanoparticles react to ammonia
gas and vehicle exhaust over time. The blue line jumps up
quickly, showing a fast response to ammonia gas as compared
to vehicle exhaust.

Fig. 29. I-V characterization of the fabricated devices 70%T iO2 -20%SnO2 -
10%CuO for carbon monoxide.

Fig. 26. Change in current for 95%T iO2 -5%SnO2 composition device.

In Fig. 26, the graph compares time-resolved optical

signals of SnO2 -T iO2 nanoparticles, revealing an abrupt
spike in signal indicative of rapid optical response, likely
influenced by factors like charge carrier generation. Time-
resolved analysis offers insights into nanoparticle behaviors,
crucial for understanding their applications in optoelectronics,
photocatalysis, or sensing.

Fig. 30. Change in current for 70%T iO2 -20%SnO2 -10%CuO composition
device.

In summary, Fig. 28 for the composition of

Fig. 27. I-V characterization of the fabricated devices 70%T iO2 -20%SnO2 - 70%T iO2 –20%SnO2 -10%CuO at 380°C, provides the
10%CuO for no gas. most comprehensive comparison as it directly contrasts the
responses of SnO2 -T iO2 nanoparticles to ammonia gas
In Fig. 26, the graph compares time-resolved optical signals exposure. It effectively communicates the differences in
of SnO2 -T iO2 nanoparticles, revealing an abrupt spike in response rates and sensitivities, contributing to a clearer
understanding of the nanoparticles’ behavior in gas sensing
applications.

Fig. 31. I-V characterization of fabricated nanodevice 50%T iO2 -50%SnO2 Fig. 34. Change in current for 50%T iO2 –50%SnO2 composition device.
for no gas.

In Fig. 30, the graph shows the current response of two

composition offers the most succinct and informative compar-
sets of SnO2 -T iO2 nanoparticles to gas exposure over time.
ison regarding the current response exhibited by two distinct
Differences in peak current and response shape imply varied
sets of 50%T iO2 –50%SnO2 nanoparticles upon exposure to
sensitivity and characteristics between the nanoparticle sets.
various gases over time. Figure 5.30 depicts the variation in
These distinctions likely stem from differences in composition
current observed for the 50%T iO2 –50%SnO2 nanoparticles
or structure. Overall, the graph effectively compares the gas-
in response to different gases.
sensing capabilities of the two nanoparticle systems.
C ONCLUSION
Tin oxalate, titanium isopropoxide, and urea precursors
were utilized in a straightforward combustion synthesis
method to create nanocrystalline (1-x)T iO2 -xSnO2 powders
(x = 0.05-0.3) with extremely uniform 5–10 nm particle
sizes. After sintering, a rutile T iO2 -SnO2 solid solution
was produced, with the composition including 10 mol%
SnO2 showing, as a result of spinodal breakdown processes,
a composite-like microstructure of insulating T iO2 and
Fig. 32. I-V characterization of fabricated nanodevice 50%T iO2 -50%SnO2
for ammonia gas.
a Sn-rich conducting phase. Maximal conductivity was
found using impedance analysis at 10 mol% SnO2 in the
vicinity of the phase boundary. The phase diagram was
correlated with the various hopping (T iO2 -rich) and band
conduction (SnO2 -rich) mechanisms that operate in different
compositional regimes. Therefore, in this technologically
significant system, combustion synthesis offered a simple
path to nanostructured T iO2 -SnO2 ceramics with tunable
electrical behaviour controlled by the miscibility gap.

R EFERENCES
Fig. 33. I-V characterization of fabricated nanodevice 50%T iO2 -50%SnO2
for carbon monoxide. [1] Nitu Singh, Vinita Pandey, Neha Singh, M. M. Malik1, Fozia Z. Haque,
“Application of T iO2 /SnO2 nanoparticles in photoluminescence based
In summary, Fig. 26, Fig. 30, and Fig. 34 present the fast ammonia gas sensing”, Journal of optics, vol. 46, pp. 199–203, 2017.
[2] E. Chinarro a, B. Moreno b, J.R. Jurado a, ”Combustion synthesis and
current-time response of 95%T iO2 –5%SnO2 nanoparticles EIS characterization of T iO2 –SnO2 system”, Journal of the European
to ammonia gas and vehicle gas exposure, emphasizing their Ceramic Society, vol. 27, pp. 3601–3604, 2007.
sensitivity for gas sensing applications. From graphs of re- [3] F.A. Deorsola, P. Mossino, I. Amato, B. DeBenedetti, A. Bonavita, G.
Micali, and G. Neri, ”Gas Sensing Properties of T iO2 and SnO2
sponses of SnO2 -T iO2 nanoparticles to ammonia and vehicle Nanopowders Obtained through Gel Combustion”, Advances in Science
gas exposure, highlighting distinct behaviors and aiding in and Technology, ISSN: 1662-0356, vol. 45, pp. 1828-1833, 2018.
understanding gas sensing and offer a concise comparison of [4] M. Radecka, A. Kusior, A. Lacz, A. Trenczek-Zajac, B. Lyson-Sypien,
K. Zakrzewska, ”Nanocrystalline T iO2 /SnO2 composites for gas sen-
T iO2 –SnO2 nanoparticles’ current response to gas exposure, sors”, Journal of Thermal Analysis and Calorimetry, vol. 108, pp.
attributing differences to composition or structure variances. 1079–1084, 2012.
Overall, these figures provide valuable insights into the gas- [5] Shyan-Lung Chung and Ching-Mei Wang, ”Solution Combustion Syn-
thesis of T iO2 and Its Use for Fabrication of Photoelectrode for Dye-
sensing capabilities of SnO2 -T iO2 nanoparticles across dif- sensitized Solar Cell”, Journal of Materials Science and Technology, vol.
ferent compositions. In conclusion, the 50%T iO2 –50%SnO2 28, pp. 713–722, 2012.
[6] Nitu Singh, Vinita Pandey, Neha Singh, M. M. Malik1, Fozia Z.
Haque,“Combustion synthesis of T iO2 nanoparticles as photocatalyst”,
Powder Technology, vol. 176, pp. 93–98, 2007.
[7] F. A. Deorsola, D. Vallauri, ”Synthesis of T iO2 nanoparticles through
the Gel Combustion process”, Journal of Materials Science, vol. 43, pp.
3274–3278, 2008.
[8] Tetiana Dontsova, Anastasiya Kutuzova1, Ahmad Hosseini-
Bandegharaei, ”Characterization and properties of Titanium(IV)
oxide, synthesised by different Routes”, Chemistry and Chemical
Technology, vol. 15, pp. 465–474, 2021.
[9] Sandip M. Deshmukh, Santosh S. Patil, Santosh B. Babar, Sultan
Alshehri, Mohammed M. Ghoneim, Asiya M. Tamboli, Nguyen Hoang
Lam, Nguyen Tam Nguyen Truong, Chang Duk Kim Mohaseen S.
Tamboli, Sanjay M. Khetre, Sambhaji R. Bamane, ”T iO2 –SnO2
Nanocomposites for Photocatalytic Environmental Remediation under
UV-Light”, Metals, vol. 12, pp. 733, 2022.
[10] Jinbiao Jia, Jia Dong, Jihuai Wu, Haoming Wei, Bingqiang Cao, ”Com-
bustion Procedure Deposited SnO2 Electron Transport Layers for High
Efficient Perovskite Solar Cells”, Journal of Alloys and Compounds, vol.
844, pp. 156032, 2020.