Synthesis and Characterization of Nanoparticle Semiconductor

Materials (ZnO) by Hydrothermal Technique

ABBAS M. ALI AL-KIFAIE1, NARIMANN NEAMAH HUSSEIN2, TAGHREED N.JAMIL 2,

ALAA A. AKON2 AND ALI ABID ABOJASSIM1

1Department of physics, Faculty of Science, University of Kufa, Najaf, IRAQ

2Radiology Techniques Department, College of Medical Technology, The Islamic University, Najaf,

IRAQ

Abstract: - ZnO nanoparticles have been synthesized by the Hydrothermal technique of

[Zn(CH3COO)2 2H2O] solution by ethanol within NaOH. The samples have been characterized by an

X-ray diffraction study. Field emission Scanning electron microscopy reveals the nanostructure of the

particles produced. their crystal size ranges in the range of nm (74-94 nm) and changes to(53-59 nm)

under change of the time preparation.

Keywords: - Hydrothermal technique, nanoparticle, X-ray diffraction, Fesem, Semiconductor

Materials, crystal size. chemical synthesis.

Received: April 27, 2021. Revised: March 13, 2022. Accepted: April 15, 2022. Published: May 6, 2022.

1 Introduction

For a long time, nanomaterials abroad have been of

interest in research and development activities.

Nanomaterials are of interest for their optical,

electrical, and other properties. These properties

have the potential to have incredible effects on

electronics, medicine, space exploration, and other

fields [1]. Nanomaterials are characterized by a

group of materials (crystalline or amorphous) from

natural or inorganic materials with sizes in the

range of 1-100 nanometers. Nanomaterials are

categorized into nanostructures, nanoscale, and

nanoparticle materials [2]. For this to happen, the

melting temperature of gold nanoparticles is much

lower than 300 degrees than the melting

temperature of a gold nugget [3]. Nanomaterials are

the building materials for the twenty-first century

and its building blocks and the most important

pillars of technologies (nanotechnology,

biotechnology, information, and communication

technology), a standard for the progress and

civilization of nations and an indicator of their rise.

Nanomaterials differ according to the source, as

they differ according to their proportions, such as

being organic or inorganic, natural or synthetic. All

known engineering materials such as metallic

elements and their alloys (metals and metal alloys),

semiconductors, oxides, and metals, as well as in

this century enhance performance in a unique and

unprecedented way [4]. Zinc oxide has gained great

interest in the scientific and medical communities,

due to its important use in many biomedical and

antibacterial applications, due to its chemical and

physical properties , such as a high electrochemical

correlation coefficient and high photochemical

stability. Zinc oxide is classified as a group II-VI

semiconductor between ionic and covalent

semiconductors, zinc oxide can be found in one-

dimensional, two-dimensional, and three-

dimensional structures and the structures are more

one-dimensional than others. ZnO shows wurtzite

(hexagonal symmetry) or (cubic symmetry) rock

salt structure, but ZnO crystals are more common

and stable with wurtzite ZnO is an excellent oxide

semiconductor with a wide direct bandgap of 3.37

eV and a large exciton binding energy of 60 meV at

room temperature [5]. Zinc oxide is one of the

most widely used semiconductors in various fields

such as flat displays, electroacoustic devices, and

photocatalysis. Zinc oxide is a wonderful material

with multiple properties suitable for high

technology such as light-emitting diodes,

photodetectors, chemical and biological sensors,

and energy collectors including solar cells,

nanogenerators, electromagnetics, etc. due to its

high chemical and thermal stability, electronic and

optoelectronic properties. Zinc oxide belongs to the

hexagonal crystal system. Zinc and oxygen join a

tetrahedron centered on a common zinc atom to

form an additional tetrahedron core, resulting in the

development of a wurtzite-type crystal lattice. ZnO

material has attracted more and more attention

during the past few years due to these applications

in various fields [6]. It includes properties such as a

WSEAS TRANSACTIONS on APPLIED and THEORETICAL MECHANICS

DOI: 10.37394/232011.2022.17.8

Abbas M. Ali Al-Kifaie,

Narimann Neamah Hussein, Taghreed N. Jamil,

Alaa A. Akon, Ali Abid Abojassim

E-ISSN: 2224-3429

Volume 17, 2022

strong oxidizing ability to degrade organic

compounds [7]. Then after that, a great abundance

of works that in a great picture, in the light of some

things that in ultraviolet light. Solar Energy

Efficiency, Household Materials Research on

Energy ZnO Photocatalysts. To date, various

shapes of ZnO powders include prismatic,

elliptical, pyramidal, dumbbell-like, flower-like,

nanowire, nanorod [9], nanotubes, nanoshells

[10]. They were prepared by different syntheses of

different preparation conditions [10]. To synthesize

ZnO semiconductors, Several wet chemical

methods are available for the synthesis of ZnO

nanomaterials such as spray pyrolysis,

hydrothermal, thermal solvents, sol-gel

Precipitation, and combined precipitation. The

hydrothermal method is widely used because it

avoids it. Toxic and expensive solvents for

preparing crystal oxide materials. To me

Preparation of oxide nanoparticles, usually three

methods are included, such as hydrolysis,

Oxidation, and thermal decomposition. All this is

done under hydrothermal conditions thermal water.

The method is a promising method for the synthesis

of high purity materials with control of

homogeneity. various methods have been used,

including the natural method, the physiotherapy

method and the ultrasound method, the direct

heating of the salt precursor, the organometallic

synthesis method, and the hydrothermal method

[10]. Because of its diverse properties, both

chemical and physical, zinc oxide is widely used in

many areas. It plays an important role in a very

wide range of applications, ranging from tires to

ceramics, from pharmaceuticals to agriculture, and

from paints to chemicals [10]. The mechanical

properties come on top of the properties that benefit

from the reduction in the size of the particles of the

material and the presence of large numbers of

atoms on the faces of its outer surface, where the

degree of hardness of metallic materials and their

alloys increases, and their resistance increases to

face the stresses and loads on them, and ceramic

materials are given a great deal of strength,

formability, and endurance. Stresses were not

available, and this means the synthesis of new

types of these materials [11]. This research aims to

study the structural properties and surface

properties and their effect on the rest of the

properties, including the mechanical properties, and

benefit from them in mechanical engineering.

2 Experiment Setup

The materials that were prepared during the winter

season have been prepared, were dissolved in 1.5 g

of [Zn(CH3COO)2 2H2O] in 25 ml of ethanol and

25ml of DDW for 15 min using a magnet. 1g

of NaOH was obtained at the same time. NaOH

solution was added dropwise to the aqueous

[Zn(CH3COO)2

2H2O] solution. Under stirring for 20 min at 25ºC

to produce a white gelatinous deposit. It was in an

autoclave and placed in an oven at 160°C for (5

and 6 h). A precipitate is formed at the bottom of

the autoclave and allowed to cool naturally to 25ºC.

The obtained precipitate was centrifuged and rinsed

with distilled water and ethanol three times to

remove the sodium salt, the product was dried at 60

°C for 45 min with a hot plate to obtain ZnOnano-

powder. Zn(CH3COO)2.2H2O + 2NaOH

Zn(OH)2 + 2CH3COONa + 2H2O

It was sealed in an autoclave and placed inside the

muffle furnace at a temperature of 160ºC

for 5 hours. A precipitate was formed at the bottom

of the autoclave and it was allowed to cool toroom

temperature naturally. The obtained precipitate was

centrifuged and thoroughly rinsed withdistilled wat

er and ethanol three times to

remove the residual sodium salt CH3COONa.

3 Results and Discussion

3.1. X-Ray

The XRD patterns of ZnO nanostructure film was

shown in figure (1),(2) and table (1). The XRD of

the synthesized zinc oxide shows broad peaks at

values of 31.9, 34.5, 36.3, 56.7, and 62.9 which are

typical for the zinc oxide structure. Notable line

broadening of the diffraction peaks is an indication

that the synthesized materials are in the nanometre

range. The average particle size has been

determined from the full width at half maximum

(FWHM) of the diffraction peaks . The average

particle size of zinc oxide nanoparticles is 9 nm.

All the diffraction peaks of the samples can be

indexed to the hexagonal phase of ZnO (JCPDS 36-

1451), and no other crystalline phases were

detected, CrystalSize was calculated from the

Scherer formula

D=K λ/ βcos𝜃 (1)

when D: is the grain size, λ: is the wavelength

of Cu K (1.5406 Å), 𝛽: full width at half.

XRD was investigated for the crystalline purity

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DOI: 10.37394/232011.2022.17.8

Abbas M. Ali Al-Kifaie,

Narimann Neamah Hussein, Taghreed N. Jamil,

Alaa A. Akon, Ali Abid Abojassim

E-ISSN: 2224-3429

Volume 17, 2022

of ZnO with a Bruker Xray diffractometer

(Model AXS D8 Advance using Cu Wavelength1.5406 nm).

Fig. 1: X-ray diffraction spectrum of ZnO

Nanomaterial In 160ºc and 5h.

Fig. 2: X-ray diffraction spectrum of ZnO

nanomaterial in 160ºc and 6h.

Table 1. X-ray diffraction variables of ZnO

nanomaterial.

3.2 Field Emission Scanning Electron

Microscope

The Fesem scanning of the prepared Zinc Oxide

particles as shown in Figures (3) and(4) showed

that they have a nano-rods shape and the particles

are lumpy, regular in shape, with an average size of

particles nm (94 nm) and their crystal size ranges in

the range of nm (74-94 nm) and change to(53-59

nm) under change of the time Preparation. The

morphological features were recorded by

FESEM(Hitachi S4700) with an accelerating

Voltage of ~50kV and elemental composition was

obtained using an energydispersive Xray

spectrometer (FEI Philips XL).

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DOI: 10.37394/232011.2022.17.8

Abbas M. Ali Al-Kifaie,

Narimann Neamah Hussein, Taghreed N. Jamil,

Alaa A. Akon, Ali Abid Abojassim

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(a)

(b)

Fig. 3: Shows the FESEM of the ZnO nanomaterial in 160ºc and 5h in (a) 2 μm, (b) 200 nm

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DOI: 10.37394/232011.2022.17.8

Abbas M. Ali Al-Kifaie,

Narimann Neamah Hussein, Taghreed N. Jamil,

Alaa A. Akon, Ali Abid Abojassim

E-ISSN: 2224-3429

Volume 17, 2022

(a)

Fig. 4: Shows the FESEM of the ZnO nanomaterial in 160ºc and 6h in (a) 2 μm, (b) 200 nm.

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DOI: 10.37394/232011.2022.17.8

Abbas M. Ali Al-Kifaie,

Narimann Neamah Hussein, Taghreed N. Jamil,

Alaa A. Akon, Ali Abid Abojassim

E-ISSN: 2224-3429

Volume 17, 2022

4 Conclusions

ZnO nanostructure thin films have been

successfully synthesized on FTO substrate by

hydrothermal method. It is fast, clean, with an

extended period of stability, and cheap. It is a

better method to provide metallic oxide. The

structural and morphological, the shape is

nano-rods and the particles are lumpy, regular

in shape, with an average size of particles nm

(94 nm) and(59 nm) their crystal size ranges in

the range of nm (74-94 nm) and change to(53-

59 nm) under change of the time preparation.

According to the XRD characterization, the

average particle size of zinc oxide prepared

using Scherrer's equation. The average particle

size of zinc oxide nanoparticles is 9nm

Acknowledgments:

First of all, praise is thanks to Allah, the almighty

God, the most gracious and the most merciful, who

provided me with the capability to complete this

research work. would like to express my gratitude

and appreciation for the staff in the Radiology

Techniques Department, College of Medical

Technology, The Islamic University.

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WSEAS TRANSACTIONS on APPLIED and THEORETICAL MECHANICS

DOI: 10.37394/232011.2022.17.8

Abbas M. Ali Al-Kifaie,

Narimann Neamah Hussein, Taghreed N. Jamil,

Alaa A. Akon, Ali Abid Abojassim

E-ISSN: 2224-3429

Volume 17, 2022