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Green synthesis of ITO nanoparticles using

Carica papaya seed extract: impact of annealing
temperature on microstructural and electrical
properties of ITO thin films for sensor applications

S. Mala, H.K.E. Latha, A. Udayakumar & H.S. Lalithamba

To cite this article: S. Mala, H.K.E. Latha, A. Udayakumar & H.S. Lalithamba (2022) Green
synthesis of ITO nanoparticles using Carica�papaya seed extract: impact of annealing temperature
on microstructural and electrical properties of ITO thin films for sensor applications, Materials
Technology, 37:10, 1432-1438, DOI: 10.1080/10667857.2021.1954278

To link to this article: https://doi.org/10.1080/10667857.2021.1954278

Published online: 19 Jul 2021.

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MATERIALS TECHNOLOGY
2022, VOL. 37, NO. 10, 1432–1438
https://doi.org/10.1080/10667857.2021.1954278

Green synthesis of ITO nanoparticles using Carica papaya seed extract: impact
of annealing temperature on microstructural and electrical properties of ITO
thin films for sensor applications
S. Malaa, H.K.E. Lathaa, A. Udayakumarb and H.S. Lalithambac
a
Department of Electronics and Instrumentation Engineering, Siddaganga Institute of Technology, Tumakuru, India; bMaterials Science
Division, Council of Scientific and Industrial Research-National Aerospace Laboratories, Bangalore, India; cDepartment of Chemistry,
Siddaganga Institute of Technology, Tumakuru, India

ABSTRACT ARTICLE HISTORY

This paper reports the synthesis of indium tin oxide (ITO) nanoparticles and the effect of Received 4 March 2021
annealing temperature on the microstructural and electrical properties of ITO thin films. The Accepted 6 July 2021
synthesized ITO (90:10) nanoparticles are deposited at 29°C using E beam evaporation to form KEYWORDS
ITO thin films and annealed at 200, 400 and 500°C. The microstructural properties are investi­ Green synthesis; ITO thin
gated using XRD and AFM , and electrical properties such as temperature coefficient of films; crystallite size;
resistance (TCR) and gauge factor are investigated using four-probe and four-point beam resistivity; temperature
bending method, respectively. The investigations results reveal an increase in grain size, carrier coefficient of resistance;
concentration and gauge factor with an increase in the annealing temperature. The absolute gauge factor
value of TCR is constant at high temperatures for the film annealed at 500°C. The ITO thin film
annealed at 500°C shows improved morphological and electrical properties and can be used
for the development of sensors operating at high temperature.

Introduction Carica papaya seed extract as the fuel. The synthesized

Over the past few decades, researchers have focused
on the development of metal-oxide-based sensors.
Metal oxides such as indium tin oxide (ITO), zinc
oxide (ZnO), cadmium oxide (CdO), titanium
dioxide (TiO2), and antimony tin oxide (ATO) are
extensively used for sensor applications. Among
these metal oxides, ITO is considered as a highly
degenerative n-type semiconductor with low resis­
tivity (7 × 10−5 Ωcm), and wide band gap (3.2–
4.3 eV), and it exhibits good piezoresistive proper­
ties [1,2]. ITO nanoparticles can be synthesized
using techniques such as sol-gel route, green com­
bustion, or hydrothermal synthesis. The ITO films
can be deposited using physical vapour deposition
methods, such as DC or RF magnetron sputtering,
electron beam evaporation, and thermal evapora­
tion, or chemical methods, such as sol-gel method,
anodic oxidation, spray pyrolysis and chemical
vapour deposition (CVD) [3–9].
Recently, several studies have carried out the synth­
esis of ITO nanoparticles and deposition of ITO thin
films for liquid crystal displays, active and passive
electronic components, and optoelectronic device
applications using various precursors and deposition
techniques [10,11].
In the present work, ITO nanoparticles were green-
synthesized using tin and indium as precursors and
ITO nanoparticles were deposited on a glass substrate
to form an ITO thin film using e-beam evaporation.
The effect of annealing temperature on the micro­
structural and electrical properties of ITO thin films
was studied and qualitatively explained for application
in high-temperature sensors.
Experimentation
Synthesis of ITO nanoparticles using green
combustion method
ITO nanoparticles were synthesized by a green com­
bustion method using Carica papaya seed extract as
the fuel. For the green synthesis of ITO nanoparticles,
indium and tin were used as precursors, Carica papaya
seed extract as the fuel, and distilled water as the
medium for synthesis. Carica papaya seeds were
washed with de-ionized water and dried under sun­
light for 5 days. The dried seeds were grinded to obtain
15 g of powder. The sun-dried and powdered seeds
were mixed with 50 mL of distilled water, and the
solution was heated with constant stirring for 1 h at
80°C. The solution was allowed to cool at room tem­
perature and was filtered to obtain Carica papaya seed
extract. The seed extract was used for the synthesis of
ITO nanoparticles. To prepare the indium nitrate
solution, 10 g of indium (In) ingots was dissolved in

CONTACT H.K.E. Latha lathahke@gmail.com Department of Electronics and Instrumentation Engineering, Siddaganga Institute of Technology, B.
H. Road, Tumakuru, India
© 2021 Informa UK Limited, trading as Taylor & Francis Group

50 mL of nitric acid (HNO3), and 50 mL of distilled
water was added slowly with constant stirring and
refluxed for 3 h. The indium nitrate (InN3O9) solution
thus obtained was placed on a magnetic stirrer for
18 h. To prepare the tin nitrate (N4O12Sn) solution,
1.2 g of tin (Sn) was dissolved in 5 mL of HNO3 and
45 mL of distilled water, and the resulting solution was
stirred using a magnetic stirrer for 21 h. ITO nano­
particles of 90:10 composition were prepared by mix­
ing 9 mL of indium nitrate solution, 1 mL of tin nitrate
solution, and 15 mL of fuel extract in silica crucibles
and heated at 600°C for 18 h in a muffle furnace. The
ITO layer formed on the sides of silica crucibles was
scratched using a spatula, and the powder obtained
was subjected to calcination at 650°C for 3 h to obtain
ITO 90:10 nanoparticles.
Preparation of ITO thin films using E- beam
evaporation
The ITO thin films were deposited on a glass substrate
using an e-beam evaporation system (M/s Hind High
Vacuum Co. (P) Ltd., Model BC-300) with an electron
beam gun (EBG-PS-5 K). The green-synthesized ITO
(90:10) nanoparticles were placed in four molybde­
num crucibles for evaporation. The target (ITO nano­
particles) was water-cooled during the evaporation
process. Prior to the deposition, the nanoparticles
were preheated at 5 mA for 5 min with the glass
substrate being covered by a shield or shutter. The as-
deposited ITO thin films were annealed at 200°C,
400°C and 500°C in vacuum for 1 h. The optimized
Table 1. Optimized evaporation deposition parameters.
Sl.No. Deposition parameter/condition ITO thin film
1 Base pressure 2 × 10−5 mbar
2 Working pressure 2 × 10−3mbar
3 Target substrate distance 13 cm
4 E beam gun voltage 5 KV
5 Evaporation current 20 mA
6 Time of deposition 45 mins
7 Thickness 100 nm
Figure 1. XRD patterns of ITO thin films (a) as-deposited and annealed at (b) 200°C, (c) 400°C, (d) 500°C.
MATERIALS TECHNOLOGY 1433
evaporation parameters of the ITO thin film on the
glass substrate are tabulated in Table 1.
The microstructural and electrical properties of the
as-deposited and annealed ITO thin films were inves­
tigated using various characterization methods. The
crystal orientation of the ITO thin films was examined
by XRD (Model: Rigaku, Monochromatized CuKα
radiation operated at 40 kV, 20 mA). The morphology
and surface roughness of the ITO thin films were
studied using an F-80 type AFM. The sheet resistance
of ITO thin films was measured using the four-probe
method (in-situ) in the temperature range of 29–
500°C. The thickness of ITO thin films was measured
using a stylus profilometer (Dektak-XT). The gauge
factor (GF) of the ITO thin films was measured using
a 4-point beam bending method at room temperature.
The carrier concentration and mobility were deter­
mined using Hall effect measurements (Agilent
B1500A Semiconductor device analyser) by applying
a magnetic field strength of ±2.5 T.
Results and discussions
The XRD patterns of the as-deposited ITO thin
films and those annealed at different temperatures
are shown in Figure 1. The ITO thin films exhibit
a polycrystalline structure. The XRD peaks indexed
at 30.47° (222), 35° (400), 38.37° (411), 44.36° (431)
and 50.89° (440) are the diffraction peaks of the
ITO thin films corresponding to the cubic bixbyite
structure of In2O3(JC-PDS 06–0416) [12,13]. The
ITO thin films undergo a structural reorientation
as the annealing temperature increases.
Furthermore, the main peak intensity decreases
and the preferential plane changes to (222)
[14,15]. The absence of SnO2 peaks in the XRD
patterns indicates that Sn4+ ions are completely
incorporated into the In2O3 lattice. The crystallite
size (D222), strain, and dislocation density were
estimated using Scherrer’s formula [6,16–18], and
1434 S. MALA ET AL.

Table 2. Average crystallite size, strain and dislocation density for the ITO peak (222).
Strain
Sl. Annealing FWHM(β) Average crystallite size Є Dislocation density d222
No. temperature (oC) (deg) D (nm) (10−3) δ (1016 lines/m2) Lattice parameter (Å) (nm)
1. As-deposited 1.36 6.33 4.17 1.32 10.12 0.292
2. 200 1.56 5.51 6.58 3.29 10.27 0.296
3. 400 1.07 8.04 4.04 1.24 10.07 0.291
4. 500 0.97 8.88 2.66 0.62 10.02 0.290

an increase in crystallite size was observed in the
film annealed at 400°C and 500°C (Table 2).
The ITO thin film annealed at 200°C shows
a decrease in crystallite size and increase in strain
and dislocation density compared with that of the
as-deposited ITO thin film (Table 2) due to impro­
per crystallization. The increase in the I222 peak for
the films annealed at 400°C and 500°C results in
the improvement of crystallite size due to the com­
plete incorporation of Sn4+ into In3+ sites [19,20].
As the annealing temperature increases (400°C and
500°C), the interplanar spacing along the (d222)
direction gradually decreases (Table 2), and it has
a higher value than that of the In2O3 powder
(0.292 nm up to 200°C) [21,22]. This is due to
the extensive structural defects in crystallized films
annealed below 200°C. The average lattice para­
meter of the (222) crystal orientation was 10.12 Å,
and the result was in good agreement with the
literature [6,20].

Figure 2. EDX spectrum of the as-deposited ITO thin film.

Figure 3. 3D AFM images of ITO thin films (a) as-deposited and annealed at (b) 200°C, (c) 400°C, (d) 500°C.

Surface morphological studies
The elemental composition of the ITO thin film was
analysed using energy-dispersive X-ray spectroscopy
(EDX) on the surface of the as-deposited ITO thin
film, and the elements were confirmed through a low
excitation EDX. Figure 2 shows the EDX spectrum of
the as-deposited ITO thin film.
The 3D AFM images of the as-deposited ITO thin
film and the films annealed at 200°C, 400°C and 500°C
are shown in Figure 3. The root mean square (RMS)
roughness of the ITO thin films increases from
0.923 nm (as-deposited) to 2.313 nm (annealed at
400°C) due to random and irregular growth of grains
[20,23–25]. A decrease in RMS roughness (1.872 nm)
is observed in the film annealed at 500°C, which is due
to the increase in crystallite size and decrease in strain
and dislocation density [26,27]. The ITO thin film
annealed at 500°C exhibits a stimulated grain growth
and smooth surface compared with that of the film
annealed at 200°C and 400°C. It was observed that the
optimized sputtering and annealing process used in
this work ensured good roughness and surface quality.
Electrical properties
Electrical properties such as the carrier concentration
and mobility of the ITO thin films were evaluated
using Hall measurements at 27°C. The changes in
mobility and carrier concentration of the ITO thin
films at various annealing temperatures are illustrated
in Figure 4. The carrier concentration increases with
an increase in annealing temperature due to the lib­
eration of electrons by the substitution of Sn4+ ions
with In3+ ions in In2O3 and liberation of two electrons
by oxygen vacancies in the reduced state In2O3
[28,29]. The mobility of the ITO thin film annealed
at 200°C decreased due to increase in grain boundary,
dislocation density and improper crystallization. The
mobility of the ITO thin films improved when the
Figure 4. Variation in Hall mobility (µ) and carrier concentration (n) as a function of annealing temperature for ITO thin films.
MATERIALS TECHNOLOGY 1435
films were annealed at 400°C and 500°C, due to the
proper reordering of grains, decrease in strain and
dislocation density (Table 2). Generally, the carrier
concentration and mobility affect the resistivity of
thin films. The resistivity values of the as-deposited
film and the film annealed at 500°C were 2.4 × 10−3
Ωcm and 1.3 × 10−3 Ωcm, respectively. Therefore,
a high annealing temperature resulted in low-
resistivity films due to an increase in carrier concen­
tration and mobility [14,29,30].
The GF of the ITO thin films was characterized to
determine the applicability of the material in sensor
applications. The GF or strain factor of a strain gauge
is the ratio of the relative change in electrical resis­
tance, R, of the thin films to the mechanical strain, ε.
A four-point bending system was designed and devel­
oped to measure the GF [31], as shown in Figure 5.
Before measuring the GF of the ITO thin films, the
four-point bending setup was calibrated using a metal
foil strain gauge (NiCr) that had a GF of 2. The ITO
thin films deposited on the glass substrates and
annealed at different temperatures were placed
between the rolling pins of the setup. Slotted weights
were placed on the upper slab of the setup for uniform
loading. When a load is applied, the sensing material
(ITO thin films) is under tension, and the strain (Ɛ) is
calculated using the following relation:
4tj@tj
ε¼ (1)
d2
where t is the thickness of the glass substrate in mm, ∂t
is the deflection in microns (µm), d is the distance
between outer rollers in mm. The change in the resis­
tance of the ITO thin films under strain was measured
using a Keithley 6 12 digital multimeter. The GF is
calculated using the following relation [4,32,33]:
ΔR=R
GF ¼ (2)
ε
1436 S. MALA ET AL.
Figure 5. The four-point bending beam setup.
where R is the resistance of the ITO material, ΔR is the
change in the resistance of the strained ITO material,
and Ɛ is the strain of the ITO thin films calculated
under uniform loading.
The effect of strain on the change in resistance of
the ITO thin films annealed at 200°C, 400°C and
500°C is shown in Figure 6. The result exhibited
a linear variation in the relative change in the resis­
tance with strain. The GFs of the ITO thin films
annealed at 200°C, 400°C and 500°C were 7.25, 8.20
and 8.37, respectively. These results indicate that the
GF significantly increased at a temperature above
400°C due to the recrystallization and decrease in the
Figure 6. Effect of strain on ITO thin films annealed at (a) 200°C, (b) 400°C, (c) 500°C.
strain and dislocation density in the ITO thin film. The
ITO thin film annealed at 200°C exhibits a low gauge
factor due to structural defects.
The ITO thin films annealed at 400°C and 500°C
exhibited improved the microstructural properties,
carrier concentration, and GF. Additionally, the TCR
is an important parameter that is evaluated to check
the applicability of ITO thin films for sensor applica­
tions. The TCR is calculated for the annealed ITO thin
films using the following equation
RT Rref
TCR ¼ � 10 6
ppm=� C (3)
Rref ðT Tref Þ
where RT is the resistance at operating temperature in
Ω, Rref is the reference resistance at room temperature
in Ω, T is the operating temperature in °C, Tref is the
reference temperature or room temperature in °C. The
TCR variations in the ITO thin films annealed at
400°C and 500°C with temperature (Figure 7) are
negative due to the presence of incomplete atomic
bonding at grain boundaries, which are capable of
trapping the free carriers. The traps become electri­
cally charged due to the free carriers, and an energy
barrier is created, which restricts the motion of car­
riers from one grain to another. This reduces the
number of carriers available for conduction
[4,32,34,35]. The average TCRs of the ITO films
annealed at 400°C and 500°C are −336 ppm/°C and
−414 ppm/°C, respectively. The absolute value of TCR
varies linearly from 29°C to 200°C (Figure 7). The
TCR remains quasi-constant above 200°C and is
found to be 400 ppm/°C for the ITO thin film

Figure 7. TCR of ITO thin films annealed at 400°C and 500°C as a function of temperature.
annealed at 500°C. The result shows that the ITO thin
film annealed at 500°C has a constant and low value of
TCR at temperatures from 200°C to 500°C). Hence,
this film can be used as a sensing material for the
development of high-temperature (>200°C) sensors.
Conclusion
ITO (90:10) nanoparticles were successfully synthe­
sized by green combustion using indium and tin as
precursors and Carica papaya seed extract as the fuel.
The synthesized ITO nanoparticles were evaporated
using e-beam evaporation, and the as-deposited films
were annealed at 200°C, 400°C and 500°C in vacuum.
The effect of annealing temperature on the micro­
structural and electrical properties of the ITO thin
films was analysed. XRD and AFM studies revealed
an increase in the crystallite size and grain size with an
increase in annealing temperature. The RMS rough­
ness of the thin film was found to be 1.872 nm for the
film annealed at 500°C. An increase in carrier concen­
tration and mobility was observed with an increase in
annealing temperature. ITO thin films annealed at
500°C exhibited a GF of 8.37 and an average TCR of
−414 ppm/°C. The ITO thin film annealed at 500°C
exhibited an improved microstructure, GF, and TCR,
and it is a suitable sensing material for the develop­
ment of high-temperature sensors.
Acknowledgements
The authors thank Director and Principal of Siddaganga
Institute of Technology, Tumakuru, Karnataka for the
research facilities. One of the authors is thankful to the
vision group of science and Technology (VGST), Govt. of
Karnataka for providing funds under CISEE programme
(GRD No. 645) for carrying out the research work.
Disclosure statement
No potential conflict of interest was reported by the authors.
MATERIALS TECHNOLOGY 1437
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