Effect of precursor type on Optical, grain sizes and Structural Properties
of Zinc Oxide Nanoparticles using Cassia leaf extract as capping and
Reducing agent
SAMAILA H1, YERIMA J. B.2, EZIKIE S. C.2
1Department of Physics, Faculty of Physical Sciences, University of Maiduguri, P.M.B. 1069,
Maiduguri, Borno,
NIGERIA
2Department of Physics, Faculty of Physical Sciences, Modibbo Adama University, P.M.B. 2076,
Yola, Adamawa,
NIGERIA
Abstract: Because of its special qualities and uses in optoelectronic devices, zinc oxide nanoparticles
have drawn the attention of researchers in recent years. At ambient temperature, zinc oxide
nanoparticles have a very significant excitation binding energy of 60 meV and band gap energy of 3.37
eV. It is also environmentally benign, non-toxic, and transparent to the visible spectrum. Zinc acetate,
zinc chloride, and zinc sulphate precursors were used in the current study to create zinc oxide
nanoparticles utilizing a green technique. Cassia leaf extract was used as a precursor and capping agent.
Distilled (DW) water was utilized as the solvent, and 1M sodium hydroxide was added in drops to get
the pH to 11.6. The produced zinc oxide nanoparticles' morphology and structure were examined by the
use of X-ray diffraction (XRD), spectroscopy, and scanning electron microscopy.
Key-words: Precursor, Grain size, Nanoparticles, Cassia Plant, Capping agent, Reducing agent and Zinc
Oxide
Received: April 13, 2023. Revised: October 24, 2024. Accepted: November 18, 2024. Published: December 12, 2024.
1. Introduction
Since it was developed as a startling discovery
in the world of things on the nanoscale between
1 and 100 nm, nanotechnology is the most
dynamic field of present scientific success in
materials science (Gnanabangetha and Suresh,
2020). Due to its potential and the wide range of
applications that may be achieved when
handling many materials at the nanoscale,
nanotechnology has brought about a paradigm
shift in life as a result of recent advancements in
nanoscale materials (Demissie et al., 2020).
Thus, it is safe to say that in the current
technological era, nanotechnology has greatly
expanded and advanced many technologies
(Hajiashrafi et al., 2015).Nanoparticles have
unique properties, like a large surface area to
volume ratio, when compared to their bulk
counterparts, which makes them an excellent
choice for operation-oriented applications. The
main effect of size on nanoparticles is electron
confinement, as noted by Sierra, Harrera, and
Ojeda (2018), because the influence of
nanoparticle size and surface area became more
pronounced or stringent as the sizes reduced.
A variety of chemical techniques, such as
thermal evaporation, microwave method, sol-gel
processing, homogeneous precipitation,
organometallic synthesis, and green method,
have been employed to create nanoparticles.
With the exception of green, all of these
techniques have been shown to have the
potential to be harmful to both humans and the
environment because they involve the release of
hazardous byproducts into the environment, the
use of complex, challenging-to-operate
equipment, high temperatures and pressures,
high costs or financial implications, and, lastly,
the loss of medical applications for
nanoparticles due to the risk of poisoning from
absorbing toxic substances on their surface.
(Denmez, 2020). The synthesis of green
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nanoparticles has gained recognition as a
competitive substitute for conventional
techniques. According to Balogun et al. (2020),
green synthesis employing plant extract is easy
to implement and advantageous for the
environment because it does not involve high
pressure, heat, energy, or hazardous materials
during the synthesis processes (Ossai et al.,
2020). The primary characteristics of the
conventional techniques for synthesizing
nanoparticles (NPs), their spherical shape, and
their antibacterial activity, according to
Hajiashrafi et al. (2018), depended on
temperature and time. Tomato, onion, cabbage,
and carrot extracts are used by Degefa et al.
(2021) as stabilizing and reducing agents to
create ZnO NPs with a single-phase hexagonal
form with average particle sizes of 17 nm, 18
nm, 24 nm, and 15 nm using the same precursor,
According to Bandeira et al. (2018), the
amounts of the biological extract and zinc
precursors significantly affect the final
properties of the manufactured ZnO
nanoparticles. Wafula et al. (2020) produced
ZnO-NPs with a crystalline size of 20.91 nm by
bio-reduction of Zn2+ using TDLE in an
environmentally friendly manner. The
antibacterial capabilities of the particles appear
promising. Noorjahan et al. (2015) also use
neem leaf extract to make zinc oxide
nanoparticles. Their SEM research shows,
nanoflakes and spindle-shaped nanoparticles as
small as 50 nm have been formed. Owing to its
many environmentally beneficial qualities, it has
been studied as a potent catalyst for a range of
organic transformations. Taherian et al., (2018)
use Satureja plants to synthesize green
nanoparticles of zinc oxide. They chose Satureja
because it contains chemical compounds that are
responsible for antioxidant and regenerative
activities. They obtain crystalline nanoparticles
with spherical shapes. XRD confirmed the
average particle diameter to be 35.88 nm which
proved to be low-cost, simple, low-risk, and
environmentally friendly, capable of producing
nanoparticles of appropriate size, and should be
used instead of environmentally hazardous
chemical methods. In another separate study,
Vaishnav et al., (2017) produced ZnO
nanoparticles from Celosia argentea leaf extract.
The average size of the nanoparticles
synthesized was 25 nm. The antibacterial
activity of the particles against E.coli,
Salmonella, and Acetobacter bacteria were
comparatively good against Salmonella, but
moderate against E. coli and Acetobacter. Zinc
oxide nanoparticles were also found to have
anti-inflammatory and anti-cancer properties in
their study. Kaningini et al., (2020) used
Athrixiaphylicoides natural extract as a reducing
agent to synthesize ZnO nanoparticles.
According to XRD and UV-Vis analysis,
synthesized ZnO nanoparticles have a spherical
shape with an average crystallite size of 24 nm.
Thus, there was no single clear factor for
controlling the size of the nanoparticles, which
directly controls their electrical and optical
properties. This study will look at the effect of
types of precursors on the size, electrical
properties, and optical properties of Zinc Oxide
nanoparticles synthesized via the Green method
using three different precursors (Zinc Acetate,
Zinc Chloride, and Zinc Sulphate) using cassia
leaves as reducing and capping agent. This
study will look at the effect of precursor types
on the size, electrical properties, and optical
properties of Zinc Oxide nanoparticles
synthesized via the Green method using 4g/100
cm3 of four different precursors (Zinc Nitrate
hexahydrate Zn(NO3).6H2O, Zinc acetate
dehydrate Zn(C4H6O4).2H2O, Zinc Chloride
ZnCl2 and Zinc Sulphate heptahydrate
ZnSO4.7H2O using Jatropha leaves as reducing
and capping agent.
2. Materials and Methods
For the synthesis of nanoparticles from the
Cassia leaf, three Zinc precursors, Zinc acetate
dehydrate (219 g), Zinc
Chloride (126 g) and Zinc Sulphate
heptahydrate (291 g) and triple
distilled water were used. All important
International Journal on Applied Physics and Engineering
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Volume 3, 2024
materials are cleaned by using nitric acid and
additionally by deionized water, and then
dehydrated by keeping it in a hot air oven before
the preparation of nanoparticles. The leaves of
the cassia plant were gathered from Shaffa
Village in Hawul Borno state, Nigeria. All the
synthesis processes were carried out in
SHESTCO Chemistry Advanced Research Lab.
Sheda Abuja Nigeria
3. Preparation of Extraction from
Cassia Plant Leaves
The leaves of the Cassia plant (Figure 1) are
collected in the Hawul local Government area of
Borno state, Nigeria, and washed by using warm
water to eradicate dirt adverts. The leaves dried
in the air after three weeks since the season in
which the present research was conducted was
summer; after drying, the leaves were powdered
by using a metal mortar and wood pestle till
they ground very well. The extraction of Cassia
leaves was done by measuring 20 g of powder
of Cassia leaves which was put into 20
milliliters of distilled water at an adjusted
temperature of 60°C for 30min, and the pH
value of the solution was measured to be 5. The
solution was finally filtered and kept in a freezer
at 7°C for further work as enumerated in Figure
1
(a). Cassia Leaves
b) Cassia Leaves Powder
(c) Cassia Leaves solution
Figure 1: a) Cassia Plant b) Cassia leaves
Powder and C) Cassia Leaves Solution
where figure 1(a) show the cassia plant, 1(b)
show the cassia powder which was grounded
and ready for extraction and finally 1(c) is the
filtrate or extracted solution from the plan ready
for green synthesis of ZnO nanoparticles.
4. Synthesis of ZnO Nanoparticles
from Cassia Leaf Extraction
The precursor basis for the zinc ion used in this
study were Zinc acetate dehydrate, Zinc
Chloride and Zinc Sulphate heptahydrate, which
was taken from chemical shops from Abuja,
Nigeria. The Zinc salts (Zinc acetate dehydrate,
Zinc Chloride and Zinc Sulphate heptahydrate)
were dissolved in deionized water. For synthesis
of ZnO nanoparticles, Conical flask volume of
500 ml, 200 ml of the source of zinc (Zinc
Acetate) (50 g/dm3) was mixed with 20 ml of
the leaf extract of the Cassia leaf and PH of the
solution adjusted to 11.6 by addition of drops of
1 molar solution of sodium hydroxide then
stimulated on a magnetic stirrer heated at 70° C,
and the stirring was nonstop for 2 hours to
allowed formation of uniform solution. The
homogenous solution was allowed to overnight
then filtered and dry in hot air oven at the
temperature of 100-120°C for 60 min. It was
then calcined in furnace for two hours at
temperature of 550°C, the color of prepared
nanoparticles is yellowish and is crumpled in a
metallic mortar and pestle to get a green
prepared of ZnO nanoparticles.
International Journal on Applied Physics and Engineering
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Samaila H., Yerima J. B, Ezikie S. C.
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Volume 3, 2024
Figure 2: Steps in Synthesis of ZnO
Nanoparticles using Cassia Plant Extract
The Nanoparticles obtaied was label as CCC
(1), this procedure was repeated for the other
precursors (Zinc Chloride and Sulphate
heptahydrate) all at concetration of 50 g/dm3,
where CCC (2) is from Zinc Chloride and CCC
(3) is from Zinc Sulphate heptahydrate
4.1 Characterization of synthesized ZnO
Nanoparticles
(i) Optical Properties:
This characterization was carried out in
Chemistry Advanced Research Laboratory
SHESTCO Using UV-Vis. Spectrophotometer.
The Synthesized nanoparticles were ground into
fine powder. A very small mass of the powder
was suspended in solution of water and ethanol
in the ratio of 2:1 in a standard cuvette of length
1 cm. The second cuvette contains only the
solution without any suspension then absorption
of the nanoparticles was scanned within the
range of 190 nm to 1100 nm. The result was
displayed on a computer attached to the
spectrophotometer. Using Origin Lab Software
and CSV file of the raw data, the graphs of
wavelength versus absorption of light by the
nanoparticles were plotted. The wavelength at
which the highest absorption take place within
the 300 nm 450 nm range for ZnO nanoparticle
was measured by the help or Origin Lab
software. Therefore, .maximum absorption
wavelength λmax and the band gaps of the entire
three (3) nanoparticles were calculated using the
equation (1).
(ii). Structural Properties
The three Nanoparticles synthesized were sent
for XRD analysis at Kaduna Geological survey
center Kaduna State. The particles were scanned
within the range of 2Ɵ is (0 - 70 degree). From
the plot of intensity against the angle of
diffraction, the half width at half maximum
(HWHM) was calculated, and subsequently the
grain sizes of the particles. Even though, the
particles are not the same size, an average of the
particles sizes was calculated. Also from the
result of the XRD spectroscopy, the zinc sites
(miler indices) were automatically or directly
read from the machine output. The particles
sizes were obtained using calculation for the
101 peak using the Debye - Scherrer’s formula
(Talam et al. 2012)
where, λ is the x-ray wavelength (1.504 nm), θ
is the Bragg diffraction angle, and β is the full
width at half maximum.
(iii) Morphological Properties
The morphology of ZnO nanoparticles was
examined by means of scanning electron
microscopy (SEM) SU3500, Hitachi with
spectral imaging system Thermo Scientific NSS
(EDS) at Umaru Musa Yar’adua University
Katsina, the tape of detector (BSE-3D),
acceleration voltage (15.0 kV), working
distance (11.6 mm), pressure (in the case of
variable vacuum conditions, 40 Pa). The results
of the SEM reveal the structures of particles
while the EDS reveal the atomic and weight
percentages of the element present in the
nanoparticles.
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5. Result and discussion
5.1: Optical Characterization
Figure 3. UV-Vis spectra of nanoparticles
Figure. 3 is the spectral lines obtained from the
nanoparticles synthesis using 50 g/dm3 of three
different precursor and Cassia leaves as the
reducing and capping agent. The result clear
shows that, the different precursors have greatly
improved the behavior of the absorption spectra
of the particles Uv–Visible spectroscopy. For
the different precursors there was a defined
pattern of absorption with peak absorptions at
374 nm for CCC 1 and 372 nm and for both
CCC2 and 373 nm for CCC3 respectively. The
energy gap for the nanoparticles were found to
be 3.33, 3.33 eV and 3.34 eV for Zinc acetate
dehydrate, Zinc Chloride and Zinc Sulphate
heptahydrate precursors respectively.
3.1: Structural Characterization
Figure 4: XRD spectra of the nanoparticles
From the above XRD spectra, it can be seen
that, they seem to have similar pattern of spectra
but their height differs which make the grain
sizes different from each other, for sample
CCC1 with a concentration of 50g/dm3 of Zinc
Acetate, the particle size was calcurate using
Scherer’s equation below:
Where: k = Scherer’s constant (usually 0.9), λ =
Wavelength of X-Ray source, Cu Kα radiation
(1.5406), β = Full width at half-maximum
(FWHM) of the diffraction peak in radian
θ = Bragg’s diffraction angle and β obtained
from the XRD data was converted to radian unit
using the equation shown below:-
was found to be 24.22.87 nm similarly, CCC2
and CCC 3 with the same concentrations as
Zinc Acetate using Zinc Chloride and Zinc
Sulphate were found to have19.27 nm and 18.31
nm respectively. From the data obtain above it
is clear that the sizes of the nanoparticles
changes with types of precousor. This is not far
away from the work of Barzinjy and Azeez
(2020) where they biologically synthesized ZnO
NPs from Eucalyptus globulus leaf extract for
water pollution removal, solar cell fabrications
and medical/cosmetic applications with
spherical nanoparticles range from 27 to 35 nm
grain sizes.
According to Sahai and Goswami (2013) a
hexagonal system like ZnO, lattice constants
andcrystallographic axes
. In this case, the lattice constants
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were calculated for those XRD peaks
for which l = 0 and lattice constant c were also
calculated only for those XRD peaks for which
h = k = 0. Based on these conditions, the
equations below were used to calculate of
usinig data in table 1
The lattice constant a is given by Zak et al
(2011) as
The lattice constant a is given by by Zak et al
(2011) and Taha et al. (2015) as
The constant is displacement of each atom
with respect to next atom along the axis ‘c’ was
given by:
The Zn–O bond length L is given by Sahai
&Goswami as:
The dislocation density (δ), which defines the
length of dislocation line per unit volume of the
crystals were calculated by the equation below
as in Sahai &Goswami (2011) and Yadav &
Chauhan (2019) as
(a.)
(b.)
(c.)
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Figure 4: SEM images of the three
nanoparticles.
Raha and Ahmaruzzaman (2022), from the
finding of their research work, zinc oxide
nanoparticles were synthesis from local
materials from the environment which has many
applications in the environment, among which
includes transparent electronics, ultraviolet
(UV) light emitters, piezoelectric devices,
chemical sensors, opto-electronics, solar cells
and spin electronics. Nomura et al., 2003 and
Nakada et al., 2004, agree with the finding of
this work due to nontoxic, nature of ZnO, they
can be extensive use as an excellent
photocatalyst for the degradation of a great
many emerging organic pollutants. Due to the
antibacterial and good antifungal activity, ZnO,
the particles synthesis in this research work can
be used in production of various raw materials
used in medicine such as disinfectant agents and
for dermatological applications. On the other
hand, ZnO NPs because they absorb UVA and
UVB radiations and can be used in sun
protective creams just as reported some time
ago by El-Diasty et al., 2013.
In the military sector where Water-repellent and
self-cleaning fibers come handy in the military
world where laundering is difficult and
inconvenient with regard to both time and scope
Zinc Oxide when incorporated into the fabric
can preventing undesirable stains (Zhang and
Yang 2009). ZnO NPs ca be use as vehicles for
gene delivery, importing doxorubicin (DOX)
into cancer cells and efficient gene targeting to
the recipient tissues such as tumor cells
(Raghupathi et al. 2011; Yuan et al., 2010;
Zhang and Liu, 2010; Taylor and Webster,
2011; Asharani et al., 2008) last but not the
least, ZnO NPs can increase the growth and
yield of food crops they induced considerable
stimulation of seed germination, seedling vigor,
and stem and root growth food crop like maize
as observed in this research and peanuts as
reported in Prasad et al., 2012
6. Conclusion
The synthesis of Zinc Oxide nanoparticles was
done using green method to investigate the
effect of the precursor types on the sizes of the
particles. So in the present paper the production
ZnO nanoparticles were carried out by green
synthesis. Cassia leaves extract was used as
capping agent while the precursors used were
Zinc Acetate salt (Zn(NO3)2.2H2O) (219 g
molar mass), Zinc Chloride (126 g) and
Zinc Sulphate heptahydrate (291
g) and triple distilled water were used with
constant concentration of 50g/dm3. The
biological syntheses of zinc nanoparticles using
leaf extract of Cassia provide an environmental
friendly, simple and efficient route for synthesis
of nanoparticles. The use of plant extract avoids
usage of harmful and toxic reducing and
stabilizing agents. The characterization of ZnO
nanoparticles were carried out using different
techniques like XRD, SEM and UV-Vis etc.
From the results above it is clear that, size of the
nanoparticles are affected by then types of the
precursor because with Zinc Acetate the average
size of the nanoparticle is 24.22 nm, with Zinc
Chloride the particles sizes was 17.27 .87nm
and finally with Zinc Sulphate heptahydrate, the
particles sizes was 18.31 nm respectively.
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Chemistry, 1(1), 18
International Journal on Applied Physics and Engineering
DOI: 10.37394/232030.2024.3.11
Samaila H., Yerima J. B, Ezikie S. C.
E-ISSN: 2945-0489
85
Volume 3, 2024
Contribution of Individual Authors to the
Creation of a Scientific Article (Ghostwriting
Policy)
The authors equally contributed in the present
research, at all stages from the formulation of the
problem to the final findings and solution.
Sources of Funding for Research Presented in a
Scientific Article or Scientific Article Itself
No funding was received for conducting this study.
Conflict of Interest
The authors have no conflicts of interest to declare
that are relevant to the content of this article.
Creative Commons Attribution License 4.0
(Attribution 4.0 International, CC BY 4.0)
This article is published under the terms of the
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https://creativecommons.org/licenses/by/4.0/deed.en
_US
International Journal on Applied Physics and Engineering
DOI: 10.37394/232030.2024.3.11
Samaila H., Yerima J. B, Ezikie S. C.
E-ISSN: 2945-0489
86
Volume 3, 2024
