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SYNTHESIS AND CHARACTERIZATION OF SELENIUM DOPED ZINC OXIDE

(ZNO-SE) NANOPARTICLES

Article  in  International Journal of Current Research · September 2018

DOI: 10.24941/ijcr.xxxx.09.2018

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INTERNATIONAL JOURNAL
OF CURRENT RESEARCH
International Journal of Current Research
Vol. 9, Issue, 09, pp.xxxxxxx, September, 2018

DOI: https://doi.org/10.24941/ijcr.xxxx.09.2018
ISSN: 0975-833X
RESEARCH ARTICLE

SYNTHESIS AND CHARACTERIZATION OF SELENIUM DOPED ZINC OXIDE (ZNO

(ZNO-SE)
NANOPARTICLES

1Musadag.M. Mustafa, 2Hasabo A. Mohamed Ahmed, 3Kamal.K.Taha and 2Ramadan. Mohammed

1Sudan Academy of Science, Africa City of Technology, Khartoum, Sudan

Sudan Academy of Science, Africa City of Technology, Khartoum, Sudan
2Textiles Department. College of Engineering and Technology of Industries, Sudan University of science
Textiles Department. College of Engineering and Technology of Industries, Sudan University of science and
Technology, Khartoum, Sudan
3Dept.. of Chemistry, College of Science, Al Imam Mohammad Ibn Saud Islamic University (IMSIU) Riyadh, KSA

ARTICLE INFO ABSTRACT

Article History: In this study ZnO nanoparticles were synthesized by using different procedures. In the first procedure
Received xxxxxxxxx, 2018 ZnO prepared by using sol-gel
sol gel method by precipitating ZnO from a reaction of Zinc nitrate
Received in revised form (Zn(NO3)2) and Sodium hydroxide (NaOH) different techniques are used sol sol-gel method with stirring
xxxxxxxx, 2018 and centrifugation to obtain ZnO nanoparticles. In the second
second procedure grinding of Zn(CH3COO)2
Accepted xxxxxxxx, 2018 and H2C2O4.2H2O in a mortar for 30 min is used, also by doping Selenium powder (5%) to the
Published online xxxxxxx, 2018 mixture and ZnO-doped
ZnO Selenium was obtained ZnO nanoparticles were characterized by X X-ray
(Rajendra et al., 2009) diffraction (XRD) where diameter ranged between 16 16-33 nm by using Scherrer
Key Words: equation. d-space
d space (d) was calculate theoretically by using Bragg’s law and practically by the formula.
Nanoparticles, Some lattice also
also were calculated and showed in the tables like: micro strain (ε), potential parameter
ZnO-Selenium doped, (μ), bond length (L), unit cell volume (V) and stress (σ).
XRD.

Copyright © 2018, Dr. Ahmed Nazar Dhannoon et al. This is an open access article distributed under the Creative Commons Attribution License, which permits
unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

Citation: Musadag.M. Mustafa,afa, Hasabo A. Mohamed Ahmed, Kamal.K.Taha and Ramadan. Mohammed. 20188. “Synthesis and characterization of
selenium doped zinc oxide (zno-se) nanoparticles”, International Journal of Current Research,
Research 10, (09), xxxxxxxxxx.

INTRODUCTION Nanotechnology is likely to have a profound impact on our

economy and society in the early 21st century, comparable to
Nanotechnology deals with using objects in the nanometer that of semiconductor technology, information technology, or
scale (10-9) size range to develop products with possible cellular and molecular biology. Science and technology
practical application. It is usually based on nanoscience research in nanotechnology promises breakthrough in areas
insights. “Nanotechnology is concerned with materials and such as materials and manufacturing, nanoelectronics,
systems whose structures and components exhibit novel nov and medicine and healthcare, energy, biotechnology, information
significantly improved physical, chemical, and biological technology, andd national security. It is widely felt that
properties, phenomena, and processes due to their nanoscale nanotechnology will be the next Industrial Revolution
size. The goal is to exploit these properties by gaining control (Bhushan, 2010) (Fang and Wu, 2013) 2013). Zinc Oxide (ZnO)
of structures and devices at atomic, molecular and supra nanostructure have been receiving remarkable attention
molecular levels and to learn to efficiently manufacture and because of their unique properties and vast application for
use these devices (Filipponi et al., ., 2010). Nanotechnology nano devices and nano systems (Wang et al., 2013,
literally means any technology on a nanoscale that has Ahsanulhaq et al.,., 2007, Reddy et al., 2007a, Reddy et al.,
applications in the real world (Bainbridge, 2004). 2007b, Law et al.,., 2005, Könenkamp et al., 2005, Kim and
Nanotechnology encompasses the production on and application Osterloh, 2005). Various approaches have been employed to
of physical, chemical, and biological systems at scales ranging grow verity of ZnO nanostructures (Ahsanulhaq et al., 2008,
from individual atoms or molecules to submicron dimensions, Umar et al., 2006b, Umar et al al., 2006a, Umar et al., 2005c,
as well as the integration of the resulting nanostructures into Umar et al., 2005b, Sekar et al al., 2005, Umar et al., 2005a,
larger systems. Umar and Hahn, 2006, Cheng and Samulski, 2004). ZnO nano
structures with flower-like
like morphology have been synthesized
*Corresponding author: Musadag.M. Mustafa by solution methods such as hydrothermal, and solvother
solvothermal
Sudan Academy of Science, Africa City of Technology, Khartoum, methods at relatively higher temperature of 160_200oC (Zhang
Sudan et al., 2004, Zhang et al.,., 2005a, Zhang et al., 2005b, Feng et
al., 2005). Zhang et al.. reported flower
flower-like ZnO nanostructure
using hydrothermal method at high temperature of 180oC beaker and it is kept on magnetic stirrer which helps in the
(Zhang et al., 2002). Recently Jiang et al. also reported proper mixing of both the solution at room temperature which
morphologically controlled ZnO flower-like structure by resulted in the formation of a white precipitation. The white
hydrothermal methods at 180oC (Jiang et al., 2007). However, product was centrifuged at 5000 rpm for 30 min and washed
hydrothermal and solvothermal methods required a rather three times with distilled water. Then it is filtered by
high-growth temperature, long reaction time, surfactants and Whatman’s filter paper. This filter paper was removed after
additives for tailoring the shape and size of ZnO filtration and kept for drying in hot oven at the temperature of
nanostructures. A wide variety of organic pollutants especially 60 - 80°C for 3 hours. The calcinations were carried out for the
pesticides are introduced into the water system from various obtained product at 400°C in the presence of atmosphere air
sources such as effluents, agricultural runoff and chemical for 4 hr (Dutta et al., 2012). The reaction between Zinc nitrate
spills (Cohen et al., 1986, Rahman et al., 2006). Their toxicity, and Sodium hydroxide for the synthesis of Zinc oxide
stability to natural decomposition and persistence in the nanoparticle can be represented as:
environment have been the cause of much concern to the Zn(NO3)2+2NaOH→ZnO +2NaNO3+H2O
societies and regulation authorities around the world (Qamar
and Muneer, 2009). The control of organic pollutants in water Synthesis of Selenium doped pristine ZnO NPs
is an important measure in environmental protection. Among
many processes proposed and /or being developed for the To synthesise the pristine ZnO NPs, 5.48g of Zinc acetate
destruction of the organic contaminants, biodegradation has dehydrate and 3.78 g of Oxalic acid were mixed and ground in
received the greatest attention. However, many organic a mortar at room temperature for 30 min. the smell of acetic
chemical, especially those that are toxic or refractory, are not acid ceased indicating the completion of the reaction to form
amenable to microbial degradation. Recently considerable hydrated ZnC2O4. The thermogravimetric analysis of the
attention has been focused on the use of a semiconductor as a synthesized ZnC2O4 revealed mass loss at about 400°C
means to oxidize toxic organic chemicals (Blake, 2001, sample(4) in Table (1), suggesting formation of ZnO NPs and
Herrmann, 1999, Litter, 1999, Vidal et al., 1999, Alfano et al., agreed well with the reported literature (Shyni et al., 2016).
2000, Fujishima et al., 2000, Macounova et al., 2001, Topalov Consequently, the ZnO NPs were prepared by heating the
et al., 2001, Li et al., 2001). synthesized hydrated ZnC2O4 in a quartz crucible at 450°C for
30 min in a temperature controlled muffle furnace. Similarly
Synthesis of noble metal nanoparticles for applications such as batches of Se doped ZnO NPs (10%) were synthesized by
catalysis, electronics, textiles, environmental protection, and mechanochemical method after adding required amount of
biotechnology is an area of constant interest. Recently, an selenium metal powder with the Zinc acetate and oxalic acid
awareness of general sanitation, contact disease transmission, precursors. The synthesized NPs were washed with ethanol
and personal protection has led to the development of and kept overnight for drying at 60oC.sample (5) see Table (1).
antimicrobial textiles. The development of antimicrobial using
Zinc Oxide nanoparticles has been investigated in various Preparation of Selenium Doped Zinc Oxide Nanocomposite
works. The ZnO nanoparticles were prepared by wet chemical
method in this work (Rajendra et al., 2010, Rajendra, 2009 The synthesis of ZnO-Se has been carried out using Mory
#552, Basheer et al.) autoclaves provided with the Teflon. The condition selected
for the synthesis of ZnO – Se particles are T = 150°C
Objectives temperature. ZnO nanoparticles prepared by the sol gel method
were taken and around O.2 g of this ZnO is weighed and taken
 Synthesis of Zinc Oxide (ZnO) nanoparticles by in the Teflon liners. Around 0.2 g Selenium is weighed and
bottom-up process and then Selenium Doped. taken in the same Teflon lines. Then exactly measure 15 ml of
 Characterization of the synthesized Zinc Oxide Ethanol and it is poured into the seam Teflon liners. Stir the
nanoparticles using XRD. content for 10 minutes. Then these Teflon liners are placed in a
 Propose further use of Zinc Oxide in redox reaction Moray autoclave. Then the autoclaves were placed in the oven
provided with a temperature controller, the temperature of the
MATERIALS AND METHODS oven was raised up to a predetermined temperature for a
desired period (5 hours). After 5 hours the autoclave is cooled
Zinc nitrate (Zn(NO3)2,6H2O)2.(H2O)2, Oxalic acid dehydrate, to the room temperature. The contents of the liners are
Selenium (Se) metal powder (99.9%), Sodium hydroxide thoroughly washed in ethanol repeatedly and later drive in an
(NaOH), Zinc acetate and Ethanol. All precursors used in this oven at 60oc for 3 hours. These dried ZnO–Se nanoparticles
study were of analytical grade and the solvents were of were characterized by XRD. (Shyni et al., 2016).
laboratory grade, which were used without further purification.
RESULTS AND DISCUSSION
Synthesis of ZnO Nanoparticles by Sol-gel Method
Typical XRD patterns of ZnO nanoparticles which are shown
ZnO nanoparticles were synthesized by sol-gel method using in Fig(1). The different peaks at angles 2ϴ of 32.08°, 34.70°,
Zinc nitrate and NAOH as precursors. In this work, the 36.60°, 48.00°, 56.80°, 36.00°, 66.70°, 68.20° and 69.40°
aqueous solution (0.2M) of Zinc |nitrate (Zn(NO3)2.6H2O) of correspond to the respective reflections from the (100), (002),
NaOH were prepared with deionized water. The Zinc nitrate (101), (102), (110), (103), (200), (112) and (201) crystal planes
weighed around 2.9749g and it is transferred into a beaker and of the hexagonal Wurtzite Zinc Oxide structure (JCPDS 36-
exactly 1.22 g of NaOH pellets were taken another beaker 1451) can be seen at the spectrum of ZnO. The XRD for the
measure 50 ml of deionized water and pour in to respected different experiments are shown in Table(1).
beakers. The NaOH solution is taken in the beaker and slowly
added into the Zinc nitrate solution which is taken in another
 Table 1. The XRD for the different experiments

Planes (hkl ) 1 2 3 4 5
2ϴ°
100 32.08 32.00 32.10 31.94 31.96
002 34.70 34.60 34.60 34.62 34.60
101 36.60 36.50 36.52 36.44 36.42
102 48.00 47.80 47.70 47.76 47.82
110 56.80 56.80 56.80 56.86 56.80
103 63.00 36.00 63.00 64.08 63.08
200 66.70 66.70 66.60 66.68 66.64
112 68.20 68.20 68.24 68.18 68.18
204 69.40 69.30 69.34 69.22 69.18

Table 2. The lattice constant value for the different samples

Sample 2ϴ° β (FWHM) D (nm) a c c/a

1 36.6 0.2526 33.125 3.2191 5.1662 1.6049
2 36.4849 0.5366 15.588 3.2172 5.1807 1.6103
3 36.4849 0.5366 15.588 3.2175 5.1807 1.6015
4 36.4840 0.2782 30.067 3.2328 5.1807 1.6025
5 36.4092 0.3535 23.657 3.2309 5.1807 1.6035

Table 3. The lattice constant value for the different samples

Sample ε Strain  (nm) 2- d (Bragg) (A°) d (formula) (A°) Reduction %

-3
1 3.331x10 9.1136x10-4 2.4532 2.4529 0.5
2 7.101x10-3 4.1154x10-3 2.4597 2.4537 0.4993
3 7.101x10-3 4.1154x10-3 2.4584 2.4537 0.4995
4 3.679x10-3 1.1061x10-3 2.4636 2.4626 0.4999
5 4.689x10-3 1.8005x10-3 2.4650 2.4616 0.4997

Table 4. The lattice constant value for the different samples

Sample L(A°) μ V (A°)3 σ (Gpa)

1 1.9602 0.3794 46.362 -1.7857
2 1.9612 0.3785 46.437 -1.1368
3 1.9612 0.3786 46.445 -1.1368
4 1.9676 0.3798 46.888 -1.1368
5 1.9669 0.3796 46.833 -1.1368

The lattice parameters are obtained using the formulae (Zak The lattice parameter obtained in this work highly related to
and Abd, 2011). those previously reported (Saleem et al., 2012). The d-spacing
was calculated by both methods using the Bragg’s law:

= and =
√ = as well as the formula:

The crystal sizes (D) of the ZnO nanoparticles were calculated

using Scherrer equation (Patterson, 1939) = +
( )

= that relates it to the lattice constants. The values obtained were

almost similar Table (3). The dhkl for the different samples
calculated by theoretical methods
where λ is the wavelength of the incident X-ray (1.5406 Aᵒ) for
Cu Kα, k is a constant equal to 0.90 (Damonte et al., 2004), The micro-strain is given by the formula, = and
βhkl is the peak width at half-maximum intensity, and θ is the
dislocation density ( ), that indicate the amount of defects is
peak position. The (101) plane (the strongest) was selected to
defined as the length of dislocation line per unit volume of
calculate the crystal size as can be seen in Table (2). The
lattice parameters are shown in table (2), the lattice parameter crystal, is calculated via relation = = (Barrett and
a and c have determined for all samples. The values for the Massalski, 1980). The Zn ‫ـــــ‬O bond length L is given by
lattice parameters a and c are identical to those reported
(Damonte et al., 2004), for ZnO nanoparticles prepared by (Seetawan et al., 2011), = + − here μ is the
standard methods. T measure of an atom displacement to the neighboring one along
the "c" axis. The value of μ is calculated by the equation,
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