Environmental Research 197 (2021) 111115

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Environmental Research
journal homepage: www.elsevier.com/locate/envres

Synergetic effect of Sn doped ZnO nanoparticles synthesized via

ultrasonication technique and its photocatalytic and antibacterial activity
Steplinpaulselvin Selvinsimpson a, P. Gnanamozhi b, V. Pandiyan b, Mani Govindasamy c,
Mohamed A. Habila c, **, Najla AlMasoud d, Yong Chen a, *
a
School of Environmental Science and Engineering, Huazhong University of Science and Technology, Wuhan, China
b
PG and Research Department of Physics, Nehru Memorial College, Tiruchirappalli, 620017, Tamil Nadu, India
c
Advanced Materials Research Chair Chemistry Department, College of Science, King Saud University, Riyadh, 11451, Saudi Arabia
d
Department of Chemistry, College of Science, Princess Nourah Bint Abdulrahman University, Riyadh, 11671, Saudi Arabia

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

Keywords: The current work reports the photocatalytic and antibacterial performance of tin (Sn) doped zinc oxide (ZnO)
Ultrasonication nanoparticles synthesized via ultrasonic aided co-precipitation technique. The increase of Sn concentration
ZnO decreased the lattice parameter and increased the crystallite size without changing the ZnO structure. The
Tin
hexagonal shaped particles and sheets obtained for 3% and 5% Sn substituted ZnO, respectively. The increase of
Water treatment
Antibacterial activity
dopant concentration reduced the reflectance and optical band gap energy of Sn doped ZnO. The vibrational
band present at 1443 cm− 1 confirmed the successful bond formation of Sn–O–Zn. The 5% Sn doped ZnO
nanoparticles exhibited greater dye elimination rate of methylene blue compared to 3% Sn. The antibacterial
activity of Sn doped ZnO showed the higher zone of inhibition about 14 mm against different pathogens. The 5%
Sn doped ZnO photocatalyst improve the transfer rate of photo excite carrier and decrease the rate of recom­
bination which greatly influence on the photocatalytic and antibacterial performance.

1. Introduction ambient reaction conditions without any secondary pollution. Metal

oxide semiconductor has been extensively used in photocatalyst water
Release of wastewater from various industries includes textile, splitting, air purification, gas sensors and other applications. Among
leather, pharmaceuticals and personal care products which cause haz­ various metal oxide semiconductors, zinc oxide has been extensively
ardous pollution to the environment (Kumar et al., 2014; Zhu et al., used as photocatalyst and antibiotic due to wide band gap, stability,
2020). Wastewater from these industries directly mix into the water conductivity, nontoxic and abundancy. Moreover, it is easy to tune the
bodies without any prior process can cause various disorders. Because it band gap energy. Zinc oxide is used as antibiotic, preservative and also it
contains various organic dyes and bacteria which contaminate the water is used in drug delivery, packaging, purification of water and skin
bodies and creates severe issues to the living organisms. Combination of coating from the olden days because it serves as a charge trapping sites
organic dyes and bacteria could cause contamination contamination in to kill the bacteria and degrade the toxic dyes (Hirota et al., 2010;
the water bodies which results in the death of living organism in the Martha et al., 2014; Ohira et al., 2008; Wei et al., 2019). Several efforts
water environment especially aquatic flora, fauna and fish (Khin et al., have been widely practiced to increase the photocatalytic and antibac­
2012; Kuhn et al., 2019; Kumar et al., 2016; Lim et al., 2013; Sharma terial ability of ZnO in the visible light (Kannadasan et al., 2014;
et al., 2010). The use of contaminated water shows various health effects Khanchandani et al., 2012; Pascariu and Homocianu, 2019). To increase
such as respiratory, nervous and skin issues to the animals and human the photocatalytic and the antibacterial activity of the ZnO material, Sn
beings. So, it is an urgency for environmental remediation to eradicate is replaced in the Zn lattice through the electronegativity and ionic radii.
the dyes and bacteria with modern techniques. Photocatalyst is an Vasanthi et al. (2013) reported that doping Sn increases the antibacterial
efficient and cost-effective method to degrade the dyes completely in activity against E. coli. Siva et al. (2020) also reported that doping of Sn

* Corresponding author.
** Corresponding author.
E-mail addresses: Mhabila@ksu.edu.sa (M.A. Habila), ychen@hust.edu.cn (Y. Chen).

https://doi.org/10.1016/j.envres.2021.111115
Received 13 January 2021; Received in revised form 2 March 2021; Accepted 29 March 2021
Available online 1 April 2021
0013-9351/© 2021 Elsevier Inc. All rights reserved.
S. Selvinsimpson et al. Environmental Research 197 (2021) 111115

supresses the carrier recombination. In the present work, Sn (3% and reliable results. The zone of inhibition of Sn doped ZnO nanoparticles
5%) doped ZnO nanoparticles were synthesized by ultrasonic aided was measured.
co-precipitation technique and observed the photocatalytic and anti­
bacterial efficacy. Ultrasonication method is advantageous which avoid 3. Results and discussion
the burst nucleation and controlled growth which directly related to
their size and prevent the agglomeration of nanoparticles (Eskandarloo 3.1. Impact of Sn concentration on the structural property of ZnO
et al., 2016). The ultrasonication process creates the acoustic cavitation nanoparticles
and collapse the bubbles through local heating and high pressure in
short time this leads to the enhancement in the photocatalytic and The powder XRD pattern of 3% and 5% Sn doped ZnO nanopowder is
antibacterial activity (Alfonso-Muniozguren et al., 2020; Gedanken, shown in the Fig. 1a. The inset of Fig. 1 (a) shows the XRD pattern of
2004). This study particularly gives a new insight into the ultrasonic bare ZnO nanoparticles. The presence 100, 002, 101, 102, 110, 103,
effect on the photocatalytic and antibacterial property of Sn doped ZnO 200, 112 and 201 planes correspond to the wurtzite hexagonal ZnO with
nanoparticles. The ultrasonication process initiates the physical changes space group of sP63mc. The diffraction pattern of Sn doped ZnO nano­
by rapid chemical reaction and improve the photocatalytic dye degra­ particles matches well with the standard JCPDS pattern of wurtzite
dation efficacy of aqueous dye pollutants (Shirsath et al., 2013). Zinat­ hexagonal ZnO (Ghayempour and Montazer, 2017). Both 3% and 5% Sn
loo-Ajabshir et al. (2018) reported that the photocatalytic efficacies doped ZnO nanoparticles exhibits similar crystal structure without
ultrasound assisted preparation processes exhibit higher compared to addition of any impure phase. The existence of Sn phase in the pattern
that of conventional methods towards methylene blue decomposition. concluded that the Sn ions uniformly dispersed in the wurtzite hexag­
onal crystal structure of ZnO by the cavitation result of the ultra­
2. Experimental procedure sonication process. The enhancement of 100, 002 and 101 peak intensity
is due to the enrichment of Sn ions at zinc sites which reduces the surface
2.1. Preparation of Sn doped ZnO nanoparticles energy and sonication process greatly improves the crystallinity of the
material (Mehraz et al., 2019). The shift in the angle confirm that the
Zinc acetate, sodium hydroxide and stannous chloride were obtained substitution of Sn slightly alters the lattice parameter, crystallite size,
from Merck, India and used for the synthesis without any further puri­ cell volume, and dislocation density of the ZnO nanoparticles.
fication. 1 M of Sn doped ZnO nanoparticles were synthesized by ul­ The crystallite size, cell parameter, dislocation density, and the cell
trasonic aided co-precipitation technique (Gnanamozhi et al., 2020; volume of the Sn doped ZnO nanoparticles were calculated (Suwanboon
Jamshidi et al., 2016). 0.97 M of zinc acetate, 0.03 M of stannous et al., 2011; Sivaraj and Vijayalakshmi, 2019) and it is given in the
chloride and sodium hydroxide were dissolved in 50 ml of distilled water Table S1. It reveals that the crystallite size of the ZnO nanoparticles
in a separated beaker and kept under magnetic stirring at 850 rpm. greater than before and dislocation density reduced with increasing of
Then, the tin precursor solution was added slowly into the zinc precursor Sn concertation. The variation in the crystallite size and cell parameter
in constant stirring, after that sodium hydroxide was added into the mainly influence in the optical and morphological property of the Sn
resultant tin doped zinc solution. The resultant white precipitate of tin doped ZnO nanoparticles. The increase in the crystallite size of the Sn
doped zinc oxide was kept in the sonication bath for 2 h. The sonication doped ZnO nanoparticles compared to other convention process mostly
process of the solution greatly improves the nucleation process and owed to the ultrasonication preparation process (Xue et al., 2015). This
homogeneity of the nanoparticles. The resultant powder was calcined result may reflect in the enhancement of photocatalytic and antibacte­
for 2 h at 300 ◦ C. Similar method was used to synthesize 5% Sn doped rial efficiency of the Sn doped ZnO nanoparticles.
ZnO nanoparticles. The as-synthesized powders were characterized by
XRD, FTIR, UV–Vis DRS, SEM and EDS. 3.2. Impact of Sn concentration on the vibrational property of ZnO
nanoparticles
2.2. Photocatalytic activity of Sn doped ZnO nanoparticles
The FTIR spectra of the different ZnO and Sn doped ZnO nano­
The photocatalytic dye degradation of methylene blue (MB) was particles synthesized by ultrasonic aided co-precipitation method were
studied using Sn doped ZnO nanoparticle (Sharifalhoseini et al., 2015). shown in the Fig. 1b. The spectra of 3% and 5% Sn doped ZnO nano­
Heber Scientific multi lamp photo reactor was used with UV lamp of 8 particles shows similar peaks with increase of Sn concentration, all the
Watt for the degradation MB. The photoreactor was made with double bands become sharper. It exhibits that the presence stretching and
walled borosilicate provided with water circulation to prevent heat. The bending mode of Sn substitute ZnO nanoparticles and some functional
lamp was fitted in between the double walled borosilicate. Dissimilar groups mainly due to the ultrasonic process. The broad band existing at
concentration of Sn doped ZnO photocatalysts were added into MB 400-600 cm− 1 belongs to the stretching vibration of Zn–O bond (Guo
aqueous solution. Then the Sn doped photocatalysts were stirred for 30 et al., 2020). The vibrational bands existing in the range of 850–1050
min to reach adsorption-desorption balance in the dark condition. The cm− 1 belongs to the metal oxide with more than one oxygen atom. The
photocatalysts were added into the methylene blue dye solution and small band present at 1040 cm− 1 and 1070 cm− 1 ascribed to the
kept the suspension at constant motion. The dye solution was collected stretching vibration of Sn–O and Zn–O. The band present at 1443 cm− 1
in the equal interval of time and immediately analysed by UV–vis corresponds to the vibrational band of dual metal Sn–Zn. The band
spectrophotometer to check the absorbance of MB. appeared at 1640 and 3443 cm− 1 belongs to stretching and bending
vibrational modes of the hydroxyl radical (Khan et al., 2019).
2.3. Antibacterial investigation of Sn doped ZnO nanoparticles
3.3. Impact of Sn concentration on the optical properties of ZnO
The antibacterial activity of Sn doped ZnO nanoparticles against nanoparticles
different pathogens were studied using agar well diffusion method
(Petkova et al., 2016). Microorganisms were cultured for 24 h at 37 ◦ C The optical properties of the 3% and 5% Sn doped ZnO nanoparticles
and added into saline solution to reach 106 colony forming units per were examined by UV–Vis diffused reflectance spectroscopy. Fig. 1c
milliliter (CFU/ml). Then the microorganism was streak on the surface displays the diffused reflectance spectra of the bare and Sn doped ZnO
of the Petri dish and made 6 mm well using crock borer. The Sn doped nanoparticles. It reveals that, both the samples have strong reflectance
solution was diluted, then added into the 6 mm well. After 24 h, the zone in the visible region and the reflectance decreases after increasing the Sn
inhibition was noted and the experiment was triplicated to get the concentration. Also, from the Fig. S1, the absorbance of the 5% Sn doped

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S. Selvinsimpson et al. Environmental Research 197 (2021) 111115

Fig. 1. a) XRD pattern b) FTIR c) Diffused reflectance and d) EDS spectra of ZnO and Sn doped ZnO nanoparticles synthesized via ultrasonic aided co-
precipitation technique.

material shifted to the visible region. The shift in the optical absorbance 3.4. Impact of Sn concentration on the morphology of ZnO nanoparticles
edge from 400 to 412 nm leads to reduction in the band gap of 5% Sn
doped ZnO nanoparticles. Thus, ultrasonication has influenced on the The morphology of 3% and 5% Sn doped ZnO nanoparticles were
optical properties of the ZnO nanoparticles through the cavitation effect examined by SEM. The inset Fig. 2 shows the SEM image of ZnO
and the crystallite size of the particles without any phase change. nanoparticles. Fig. 2 displays the hexagonal shaped particle prepared via
The red shift after increasing the Sn concentration might be ultrasonic aided co-precipitation method. The Sn concentration and
accredited to the charge-transfer transitions between Sn electrons and ultrasonication method significantly influence on the nanomaterial
the ZnO conduction band, and the additional electron decreases the morphology and the size of ZnO nanoparticles. The 3% Sn doped sample
band gap through the electronic transition during the sonication reac­ reveals hexagonal shaped particles whereas 5% Sn doped ZnO nano­
tion. The band gap energy of the Sn doped ZnO nanoparticles were particles exhibits hexagonal sheet like particles. The difference in the
calculated using Kubelka–Munk equation (Siddiquey et al., 2012; morphology of the Sn doped sample mainly due the concentration of Sn
Vázquez-Cuchillo et al., 2013). Fig. S2 reveals the band gap energy and cavitation effect of the ultrasonication. The presence of hexagonal
spectra of Sn doped ZnO nanoparticles. It confirms that the increase of sheet like particle improve the photocatalytic activity by supressing the
Sn concentration reduces the band gap energy from 3.17 to 3.0 eV due to recombination rate. The ultrasonication process consisting of compres­
the presence of interstitially embedded Sn ions into Zn lattice. 3d-4s and sion and rare fraction cycles which creates the cavitation effect in the
4d-5s orbital electrons exchanges of the Sn doped ZnO decreases the reaction and it played main part in the morphological changes of Sn
electron density which reduces the band gap (Arpac et al., 2007). Fig. S3 doped ZnO nanoparticles morphology from rod to hexagonal thin sheets
displays the transmittance of 3% and 5% Sn doped ZnO nanoparticles, (Al-Hadeethi et al., 2017; Prakash et al., 2015). The formation of hex­
with the rise of Sn ratio transmittance decreases. The reduction in the agonal shaped ultra-thin sheet binds each other and form a network, this
transmittance mainly due to the homogeneity, and crystallinity of the network like sheets has high density which is beneficial to increase the
nanoparticles which improve the photocatalytic and antibacterial ac­ charge separation. Al-Hadeethi et al. (2017) also reported that the for­
tivity by their crystal defects (Prakash et al., 2015). mation network has high density and beneficial for the many applica­
The elemental analysis of 3% and 5% Sn doped ZnO nanoparticles tion. Moreover, this particle inhibits the bacterial growth by breaking
were examined by EDS. Fig. 1d displays the EDS spectra of bare and Sn the cell wall easily.
doped ZnO nanoparticles. The existence of Zn, Sn and O in the spectra
confirmed the effective addition Sn in the Zn lattice. Moreover, lesser
variation in the spectra clearly reveals the difference in the Sn concen­ 3.5. Impact of Sn concentration on the photocatalytic activity of ZnO
tration. This outcome shows good agreement with the XRD and SEM nanoparticles
results, respectively.
The photocatalyst is an effective approach for the treatment of
contaminated water to eliminate the organic dyes. Here, the photo­
catalytic degradation of MB using 3% and 5% Sn doped ZnO

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S. Selvinsimpson et al. Environmental Research 197 (2021) 111115

Fig. 2. Morphology of bare and Sn doped ZnO nanopowders synthesized using ultrasonic aided co-precipitation technique.

nanoparticles were investigated. The photocatalytic ability of the metal

oxide semiconductors generally depends on the electronic structure,
bandgap and morphology of the catalyst. Figs. 3 and 4 UV absorbance
spectra of MB degraded dye solution at dissimilar interval of time using
3% and 5% Sn doped ZnO nanoparticles. It shows that the MB dye
degraded completely within 1 h using 5% Sn doped ZnO nanoparticles
whereas 3% Sn doped samples shows 90% of degradation in 1 h.
The hierarchical structures, crystalline phase and surface area in­
fluence on the photocatalytic efficiency. The formation of the sheet in
the ultrasonication process has higher surface area which might adsorb
substantial quantities of hydroxyl groups, which produce the efficient
oxidant through the hydroxy radical. This oxidant yield huge amount of
heat and degrade the organics effluents. This dissimilarity in the pho­
tocatalytic efficacy of the nanoparticles generally owed to the Sn con­
centration. In addition, Sn concertation play major part in the band gap
energy, electronic structure, and the morphology of the nanoparticle (Do
et al., 2017; Ganesh et al., 2017). Moreover, 5% Sn doped sample re­
duces the ZnO band gap energy from 3.17 to 3.1 eV which significantly
enhance the photocatalytic performance by hindering the electron hole
recombination. The existence of hexagonal sheet like particle influence
in the dye degradation performance via trapping the electron hole on the
surface of the sheet. ROS such as h+, O−2 and OH‾ are accountable for Fig. 4. Photocatalytic activity of 5% Sn doped ZnO nanoparticles.
the elimination of methylene blue dye. In 5% Sn photocatalyst, the ul­
trasonic process creates more empty space (cavitation) and bubble dis­ photocatalytic dye degradation of the Sn doped ZnO is shown in the
sociates to form more OH• radical compared to the normal process under following equation and the Comparative study on the photocatalytic dye
visible light (Alfonso-Muniozguren et al., 2020). In this case 5% Sn degradation efficiency of MB against different nanomaterials are given
doped ZnO photo catalyst improve the transfer rate of photo excite in Table S2 (Mosleh et al., 2018; Khorasanizadeh et al., 2019).
carrier and decrease the rate of recombination. The mechanism of the
SnZnO + hν → SnZnO (e‾CB + h+VB)
——————————————————— (1)

Organic molecules (MB) + h+VB → Oxidation products

——————————————————— (2)

e− CB + O2 → O2• ——————————————————— (3)

O2• + H+ → HO2• ——————————————————— (4)

.
Radicals ( OH• or HO•2) + Pollutant → Degradation products
——————————————————— (5)

3.6. Antibacterial activity of 5% Sn doped ZnO nanoparticles

Bacteria has become resistant against antibiotics [Qin et al., 2020].

In recent times, treat those bacteria with metal ion doped metal oxide
semiconductor is developing area in the research field. Moreover, the
use of nanosized metal ion doped metal oxide play a major part in the
bacterial treatment. In this study, 5% Sn doped ZnO nanoparticles is
used to study the antibacterial activity against different pathogens.
Fig. 3. Photocatalytic activity of 3% Sn doped ZnO nanoparticle. Fig. 5 displays that the zone of inhibition with the standard deviation of

4
S. Selvinsimpson et al. Environmental Research 197 (2021) 111115

Princess Nourah bint Abdulrahman University through the fast-track

Research funding Program. V. Pandiyan is highly thankful to DST, Sci­
ence & Engineering Research Board (SERB through major research
project grant F. No. EMR/2017/003583).

Appendix A. Supplementary data

Supplementary data to this article can be found online at https://doi.

org/10.1016/j.envres.2021.111115.

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