Digest Journal of Nanomaterials and Biostructures Vol. 16, No. 1, January - March 2021, p.

41 - 49

SYNTHESIS OF TIN OXIDE NANOPARTICLES IN ORDER

TO STUDY ITS PROPERTIES

N. SHAHZADa, N. ALIb*, A. SHAHIDb, S. KHANb, H. ALROBEIc*

a
National University of Sciences and Technology (NUST), Pakistan
b
Department of Physics, GPG Jahanzeb College Saidu Sharif, Swat, Pakistan
c
Department of Mechanical Engineering, College of Engineering, Prince Sattam bin
Abdullaziz University, AlKharj, Saudi Arabia

Pure tin oxide nanoparticles ware synthesized via Co-precipitation method. The as-
synthesized nanoparticles were characterized by Fourier transform infrared spectroscopy
(FTIR), thermo-gravimetric analysis (TGA), X-ray diffraction (XRD) and diffuse
reflectance spectroscopy (DRS). X-ray diffraction shows that tetrahedral shaped
nanoparticles of crystallite size 47.35nm were prepared successfully. The crystallinity was
established due the reduction in distortion ratio and dislocation density. The value of strain
showed that the nanoparticles fabricated were of high stability. The direct and indirect
optical band gap of as-synthesized SnO2 nanoparticles were determined from the
reflectance spectra, which were 3eV and 2.65eV respectively.

(Received September 10, 2020; Accepted January 8, 2021)

Keywords: Tin Oxides, nanoparticles, XRD, DRS, Band gap

1. Introduction

Nanoscience is the study of matter’s properties at a nanoscale. It is based on the special

size dependent properties of solid state materials [1]. Nanoscience deals with objects of size
having the smallest dimension ranging from a few nanometers to less than 100 nanometers. In the
field of physics and electrical engineering nanoscience is most often related with quantum
behavior, the behavior of electrons and photons in nanoparticles [2]. The word “nanotechnology”
was the first time used by Norio Taniguchi and defines nanotechnology as ““Nano-technology”
mainly consists of the processing of separation, consolidation, and deformation of materials by one
atom or one molecule”[1]. Nanotechnology is the technology which works on level of nanometer
(nm), one billionth of a meter. In the nano region the elements change properties unpredictably. It
is generally related to mechanical engineering on a molecular scale, but it is a confusing term. It is
sometimes also related to today’s applied nanotechnology because of its numerous uses in
cosmetics or industrial coating [3]. The term nanomaterial stands for the nano sized structures in
which at least one of its phases has one or more dimensions, and they include nanometer sized
particles ranging from 1nm to 100nm [4]. The properties of nanomaterial change due to its size,
shape, and morphology. The structure of nanomaterials depends on the method of preparation,
nature of solvent, concentration, strength of reducing agent, and temperature [5]. The
nanomaterials are classified as zero dimensional (0-D), one dimensional (1-D), two dimensional
(2-D), and three dimensional (3-D).
Nanomaterials have wide ranging applications in many areas of studies. Some of them are
narrated below:
a. Nanomaterials are used for the elimination of dense metallic ions, and dyes from
waste water organic, and inorganic pollutants [6].
b. Nanomaterials are used in agriculture, and crop production [7].

*
Corresponding author: [email protected]
42

c. Nanomaterials are used to improve molecular diagnostics such as gene detection,

sensitivity, and practicality [8].
d. They are used to improve the properties of transistors [9].
e. Some nanomaterials such as solid lipid nanoparticles are used for skin hydration,
and also have the ability to block UV-Rays [10].
f. Nano catalysts are used in the chemical, and pharmaceutical industries for
enhancing the efficiency of energy in connection with green technology with the production of
very less amount of chemical waste production.
g. Mesoporous silica shell nanospheres are widely used in hydrogenation catalysis,
and magnetic acid catalysis[11]. They are also used for the enhancement of chemical reactions,
and separation processes, and for simplification of the processes.
h. Metallic nanoparticles, quantum dots, and Nano bubbles have also been widely
used in catalysis [12].
i. Consolidated nanocomposites, and nanostructures are used for making very high
strength material with tough structure, tough pliable cements, and interestingly new magnets[13].
j. Nanostructured electrodes can enhance the efficiency, and capability of Li-ion
batteries[14].
k. Nanotubes can be used as electro chemical actuators because of its super
capacitance [15].
Amongst various nanomaterials being researched and used world over, Tin nanoparticles
are also gaining attention of different research studies owing to its wide ranging applications in
different fields. The research on Tin nanoparticles is extending with passage of time and with the
rapidly changing advancements in different fields including, construction industry. Tin
nanoparticles have a very broad and wide research area. The main reason is that Tin nanoparticles
may be easily modified by changing their chemical properties.
Out of the many advantages of Tin nanoparticles, one key advantage is that their
properties vary from the majority of the properties of the same composition. Tin nanoparticles may
be coated onto other metals for corrosion prevention. Tin nanomaterials are widely used for many
purposes, such as, enhancing the activities of super capacitors by providing high energy density to
the capacitor [16], enhancing the gas sensing ability due to high sensitivity, response, and low-
priced [17], enhancing the electrochemical properties of other materials such as improving the
storage capacity of a battery [18], enhancement of photocatalytic activities of the materials owing
to their good optical transparency, good intrinsic vacancies, and high density [19], acting as charge
transport layer to increase the charge transformation, and for reducing hysteresis [20], cosmetics
materials for protecting skin from UV-rays, and other rays effecting the skin [21].
Tin oxide (SnO2) nanoparticles have been prepared by many methods by many researchers
in recent years. These researchers use different types of precursors, and reagents for their work.
Tin oxides prepared by these methods have many applications in different fields.
Zhu and co-authors (2000) used sonochemical method for synthesizing SnO2
nanoparticles. They used SnCl4 aqueous solution, and azodicarbonamide under ambient air in their
work, and obtained Tin oxide nanoparticles of the size 3 to 5nm. The particles were spherical in
shape, and had band gap of 4.05ev which is greater than the value of band gap (3.7ev) of SnO 2
bulk material. The prepared Tin oxide was used as in lithium ion batteries as reversible insertion
electrode for enhancing the performance of battery, and increasing battery life [22].
Song and Kang (2000) used homogenous precipitation method for the preparation of SnO2
powders. They used tin chloride pentahydrate, and urea in their work. The particles prepared were
in powder form, and had large surface area. The particles prepared had size ranging from 3 to 5nm.
Because of the large surface area of the SnO2 powders prepared by this method, it was used in gas
sensors materials, and for enhancing the sensing properties of devices [23].
Qui and co-authors (2004) prepared tin nanoparticles using polyol process by
sonochemical method. They used tin chloride and ethylene glycol for their work. The particles
prepared were rod shaped having size in range of 50 to 100nm, and length in range of 1 to 3µm.
the prepared Tin oxide nanoparticles were used in lithium ion batteries as electrode material and
for enhancing the performance of batteries [24].
 43

Chiu and Yeh (2007) used hydrothermal method for the preparation of SnO2 nanoparticles.
They used tin chloride 2-propanol, and distilled water as solvent for their work. The prepared
nanoparticles were tetragonal shaped having size of 3nm. The band gap of the particles was 3.6eV,
and were used as sensing materials [25].
Bagheri-Mohgheghi and co-authors (2008) prepared SnO2 nanoparticles using sol gel
method. They used hydro-alcoholic solution, ethylene glycol as polymerizing agent, and tin
chloride, and citric acid as complexing agent. The particles prepared were tetragonal shaped of
size ranging from 5 to 25nm with a greater band gap from 4.05 to 4.11eV. The prepared
nanoparticles were used for the agglomeration of particles [26].
Liu and co-authors (2009) used gel combustion method for the preparation of SnO2
nanoparticles. They used Tin Chloride, and polyacrylamide gel in their work. SnO2 nanoparticles
prepared were sphere shaped, and had size in range of 8.1 to 27.9nm. The nanoparticles obtained
by this process were used for the detection purposes of gases [27].
Krishnakumar and co-authors (2009) used microwave technique for the synthesis of SnO2
nanoparticles. They used tin hydroxyl solution with hydrazine hydrate in a precursor solution for
obtaining Tin Oxide nanoparticles. The prepared SnO2 nanoparticles were having spherical shape,
and size in range of 10 to 11nm [3].
Xu and co-authors (2010) also used the homogenous precipitation method for the
preparation of SnO2 nanoparticles. They used tin chloride, urea (carbamide), and aluminum oxide
rod for their work. Tetragonal shaped SnO2 nanosheets of size 10nm were prepared. The particles
prepared indicated enhancement in high performance of sensing devices [28].
Gondal and co-authors (2010) prepared tin oxide nanoparticles using highly powerful laser
beams. They used tin metal as target material placed in distilled water, and highly powerful laser
in their work. The tin oxide nanoparticles prepared were tetragonal shaped of size 3nm, and a band
gap of 4.4eV [29].
Parthibavarman and co-authors (2011) prepared SnO2 nanoparticles using microwave
irradiation method. They used tin chloride and NH3.H2O in their work. The prepared SnO2
nanoparticles were spherical shaped with size in range of 20 to 25nm with a band gap of 3.7eV.
The acquired nanoparticles were used for highly susceptible environmental controlling and in
electronic devices for controlling humidity[30] .
Patil and co-authors (2012) also used hydrothermal method for the synthesis of SnO2
nanoparticles. They used hydrazine hydrate as a mediator for this process. The obtained SnO 2
nanoparticles were of tetragonal shape. The obtained particles were having size 22.4nm, and a
band gap of 3.6ev. SnO2 prepared by this method can be used as gas detectors in many gas
detecting devices [31].
Honghao and co-authors (2013) prepared SnO2 nanopowder through gas phase detonation
reaction. They used stannic chloride as precursor, and mixture of hydrogen, and oxygen gas. The
SnO2 nanopowders prepared were having size of 1 to 10nm, and have spherical morphology.
Further details were not discussed as gas phase reaction was not announced by this method.
Although, prepared SnO2 nanopowders were having high sensitivity [32].
Naje and co-authors (2013) used chemical precipitation method for the preparation of
SnO2 nanoparticles. They used tin chloride and ammonia solution in their work. The prepared
SnO2 nanoparticles were in powder form having tetragonal shape, and size was 8 to 10nm with a
band gap of 4.3eV higher than that of the band gap of bulk SnO2 [33].
Nayef and Hadi (2014) used laser ablation technique for the synthesis of SnO2
nanoparticles. They used tin, and methanol for this process. The prepared particles were spherical
shaped, and their size varied according to different experimental conditions. The band gap of the
particles was greater than that of bulk SnO2, and was observed at different laser concentration in
range of 4.16 to 4.26eV [34].
Srivastava and Mukhopadhyay (2014) used biological method for the synthesis of SnO2
nanoparticles. They used Erwinia herbicola (Gram-negative bacteria), and tin chloride for their
work. The SnO2 nanoparticles prepared were tetragonal shaped having size in range of 15 to 40nm.
The prepared SnO2 nanoparticles showed good photocatalytic behavior, and were used for the
photodegradation of many organic dyes [35].
44

Elango and co-authors (2015) used green synthesis for the preparation of SnO2
nanoparticles by green synthesis technique. They used plant’s (Persia Americana) seed extract, and
stannous chloride as precursor for their work. The SnO2 nanoparticles they obtained were
tetragonal shaped with size in range of 4nm, which were used for the degradation of dyes [36].
Bhagwat and co-authors (2015) also used sol-gel method for preparing SnO2 nanoparticles.
They used tin chloride, ethylene glycol, and liquid ammonia as precursors, and double distilled
water as solvent. The prepared particles were having size in range of 350 to 800nm, and a band
gap of 3.78ev [37].
Azade Esmaeili-Bafghi-Karimabad and co-authors (2015) prepared SnO2 nanoparticles
using simple chemical reaction method. They used tin chloride, and dimethylamine as capping
agent. The particles prepared were tetragonal shaped having size 40nm with a greater band gap of
3.82eV. These prepared particles were used for enhancing the thermal stability and reducing the
flammability of materials [38].
Nagirnyak and co-authors (2016) prepared SnO2 nanoparticles by using chemical
deposition method. They used tin chloride, and ammonium oxalate as precursors, and prepared
two samples of SnO2 nanoparticles of size in range of 40 to 200nm, and hexagonal shape. The
band gap was 3.69eV for one sample, and 3.78eV for other. The prepared materials were used as
sensing materials, and for enhancing the properties of gas sensors [39].
Kurniawan and Rahmi (2017) prepared SnO2 nanoparticles using electrochemical method
(electrolysis) at a large potential. They used tin bare as electrodes (both anode, and cathode), and
hydrochloric acid (HCl) as the electrolytic solution. The particles produced by this method showed
tetragonal shape, and size in range of 25 to 150nm [40].
Oliveira and co-authors (2018) prepared SnO2 nanoparticles using solvothermal method
using indium chloride tetrahydrate, and tin chloride pentahydrate as precursors, and ethylene
glycol as solvent. Spherical shaped particles of size in range of 3.4 to 8.2nm with a band gap of 3
to 3.4ev were obtained [41].
Kim and co-authors (2018) used the liquid phase plasma method for the preparation of
SnO2 nanoparticles. They used tin chloride as a precursor, cetyl trimethyl ammonium bromide, and
water as solvent. The SnO2 nanoparticles were of spherical shape with size in range of 5 to 10nm.
These particles were used for enhancing the storing capability, and life time of lithium ion
batteries [42].
Diaz and co-authors (2018) prepared SnO2 nanoparticles by using two step solid state
synthesis method. SnCl2.Chitson at different ratio of 1:1, 1:5, and 1:10 with dichloromethane
(CH2Cl2) as solvent were used for this process. Rod like nanostructures of SnO 2 of size 2.2 ±
0.2nm using precursors at 1:5. They used the SnO2 prepared by this method in optoelectronic
devices, and solid state sensor devices for enhancing the mechanical properties of these materials,
and upgrading their performance [43].

2. Materials and methods

All analytical grade reagents were used. The solutions were prepared in distilled water
(E.C. 2.8µS/cm) which was obtained from the distillation apparatus (Model WSB/4, Hamilton
Laboratory Glass Ltd.). Tin chloride dihydrate (SnO2.2H2O) (Merck) was used as a precursor.
Ethanol (Merck) was used as a solvent.

2.1. Synthesis of tin nanoparticles

Co-precipitation method was used for Tin oxide nanoparticles synthesis. Two solutions
were mixed forming a precipitate, which was then washed, annealed to obtain the desired product.
Two approaches using ethanol as solvent, and using ethanol and water as solvent, were adopted
using the same method, to prepare two samples of SnO2 nanoparticles. Detailed procedure is as
under:
a. 1.12825g of tin chloride, and 50ml ethanol were taken in a beaker, and mixed with
the help of a magnetic stirrer for about 10 to 15minutes to obtain a complete soluble, and
transparent solution.
 45

b. 0.4g of sodium hydroxide was dissolved in 100ml of deionized water with the
help of a magnetic stirrer, and sodium hydroxide solution was obtained (0.1M solution)
c. The sodium hydroxide solution was dropwise added to the prepared tin chloride
solution at constant stirring as precipitating agent, and controlling pH of the solution. With the
addition of sodium hydroxide solution, precipitate was formed in the solution, and the pH value
reached 8 with the addition of 109ml of sodium hydroxide solution
d. As the pH of the solution was maintained, further stirring was stopped, and the
precipitate was allowed to settle down by keeping the solution still for 12hrs
e. After 12hrs the precipitate got concentrated at the bottom, and the ethanol above
the precipitate was decanted.
f. Ethanol was added to the precipitate for washing, and then again kept for 12hrs to
settle down. After 12hrs the ethanol was again removed. This process was repeated three times,
and at last a pure precipitate was obtained.
g. The precipitation was dried on heating at 90°C for 12 hours.
h. After heating, a solid matter was obtained which was grinded into powder and
annealed at 800°C for 3 hours.
i. After annealing we obtained our desired product which was further investigated
by different characterization techniques.

3. Results and discussions

3.1. FTIR
In the FTIR spectroscopy graph the band from the 3394 to 3409 cm-1shows the streching
vibration of O-H bond .This band is due to the OH groups and the adsorbed water bound at the
SnO2 surface. The band at 1620 to 1630 cm-1 matched to the bending vibration of water molecules,
caught in the SnO2 sample. The peak at 521cm-1 matching with the stretching vibrations of the
terminal Sn-OH and at the peak 660 to 600cm-1 region shows the stretching modes of the Sn-O-Sn.
Due to increase in temperature the peak is also broadened (Fig. 1).

Fig. 1. FTIR analysis of SnO2 nanoparticles.

3.2. TGA (thermogravemetric analysis)

The TGA analysis was carried out and it was observed that at 50 to 120 degrees increase
in weight occurred because of oxidation of Sn+2, because of this oxidation the temperature of the
furnace increased and the TGA curve was distorted. The constant weight condition was reached
near 300 C° after which the weight goes on decreasing slowly as the temperature increased. At
425° to 600° the weight loss further increased because of evaporation of OH- and water molecules
and above 600° the weight loss suddenly increased as shown in the figure.
46

Fig. 2. TGA OF SnO2.

3.3. XRD
The XRD pattern of SnO2 nanoparticles synthesized by co-precipitation method is given
below. All of the peaks were matched with diffraction data of the tetragonal structure of tin oxide
(JCPDS 01-077-0447 ). Position of the main peak is 2θ= 26.68 and the width of the peak is 0.933
nm.
The average crystallite size (D) of the nanoparticles was estimated using the Debye
Scherrer formula as follows:

D=
(i)

where, λ, β, θ are the X-ray wavelength of radiation used. The averge crystallite size (D)
determined from SnO2 different plane by the Scherrer formula is about 47.35 nm and tetrahedral in
shaped.
The average dislocaton density of SnO2 particles is determined to be 7.28×1014/m2 by the
equation.

Dislocation density = 1/ D2 (ii)

The average strain was determined to be 0.206 by the equation.

Strain = β/4 tan θ (iii)

Fig. 3. XRD analysis of SnO2.

 47

Table 1. The detailed analysis of SnO2 by XRD.

No. 2θB θB 2Ɵ1 2Ɵ2 Interplanar Miller

Spacing d Indices
(A°) (hkl)
1 26.6883 13.3441° 26.314° 27.247° 0.4665 3.3409 30.5 (110)
2 33.9608 16.9804° 33.541° 34.473° 0.466 2.6397 31.1 (101)
3 38.0033 19.0016° 37.737° 38.436° 0.3495 2.6677 41.9 (200)
4 42.6432 21.3216° 42.516° 42.749° 0.1165 2.1207 127.7 (111)
5 51.8903 25.9451° 51.374° 52.540° 0.583 1.7621 26.4 (210)
6 54.8388 27.4194° 54.521° 55.104° 0.2915 1.6741 53.3 (211)
7 57.9546 28.9773° 57.668° 58.367° 0.3495 1.5913 45.3 (220)
8 61.9659 30.9829° 61.631° 62.564° 0.4665 1.4976 34.6 (002)
9 64.8092 32.4046° 64.312° 65.244° 0.466 1.4386 35.2 (310)
10 66.1391 33.0695° 65.827° 66.526° 0.3495 1.4116 47.3 (112)

Average particle size = 47.35nm

Structure = Tetrahedral

JCPDS Card # = 01-077-0447

Average strain = 0.206

Dislocation density = 1 / D2

Average Dislocation density= 7.28×1014/m

3.4. Optical properties

The optical properties were studied by using diffuse reflectance spectroscopy (DRS). The
reflectance spectra of the pure SnO2 nanoparticles are as shown in the figure 4. From the spectra,
it is observed that he quantum confinement effect increases with increase of reflectance. The
decrease in reflectance near the 300nm is due to the optical transition happening in the optical
bandgap. The synthesized SnO2 showed no reflection up to 290nm and washighly reflective above
the region of 320 nm.
The optical bandgap was determined by kubelka-munk relation as shown below, which is
commonly used to study diffuse reflectance spectroscopy.

F (R) = =

(iv)

where F(R) is the kubelka-munk function which relates to the absorbance, R is the reflectance, k is
the absorbance co-efficient and S is the scattering co-efficient. The optical transition in
semiconductors are of two types, the direct and indirect transitions. Therefore direct and indirect
bandgap determined by this relation as shown the figure 5 are 3eV and 2.65eV respectively.
48

Fig. 4. Reflectance spectra of SnO2.

Fig. 5. Bandgap of SnO2 from reflectance spectra.

4. Conclusions

SnO2 nanoparticles have been effectively prepared by Co-precipitation method using tin
chloride (SnCl) and sodium hydroxide (NaOH) at 800°C. The Fourier transform spectroscopy
(FTIR) illustrates that chlorine impurity was entirely removed by washing process. The TGA
analysis showed that sudden mass change occurred at 630°C, showing the breakdown of tin oxide.
The structural and optical properties were examined by X-Ray diffraction (XRD) and diffuse
reflectance spectrum (DRS). X-Ray diffraction (XRD) analysis showed that samples were well
crystalline and tetrahedral in shape having average crystallite size of 47.35nm. The direct and
indirect band gap was found to be 3eV and 2.65eV respectively.

Acknowledgment

This project was supported by the Deanship of Scientific Research at Prince

Sattam bin Abdul Aziz University under the research project no. 2020/1/17063. The
authors are also thankful to NUST Research Directorate for financial support.

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