Arabian Journal of Chemical and Environmental Research

Vol. 08 Issue 02 (2021) 355–371

Review: Synthesis of Zinc Sulfide Nanoparticles by Various Methods

R. P. Dewi1, A. Nurdiana2, L. Astuti3, R. Ragadita4, A. B. D. Nandiyanto5

1
Departemen Kimia, Fakultas Pendidikan Matematika dan Ilmu Pengetahuan Alam,
Universitas Pendidikan Indonesia, Jl. Dr. Setiabudi no. 229, Bandung 40154, Indonesia.
2
Departemen Kimia, Fakultas Pendidikan Matematika dan Ilmu Pengetahuan Alam,
Universitas Pendidikan Indonesia, Jl. Dr. Setiabudi no. 229, Bandung 40154, Indonesia.
3
Departemen Kimia, Fakultas Pendidikan Matematika dan Ilmu Pengetahuan Alam,
Universitas Pendidikan Indonesia, Jl. Dr. Setiabudi no. 229, Bandung 40154, Indonesia.
4
Departemen Kimia, Fakultas Pendidikan Matematika dan Ilmu Pengetahuan Alam,
Universitas Pendidikan Indonesia, Jl. Dr. Setiabudi no. 229, Bandung 40154, Indonesia.
5
Departemen Kimia, Fakultas Pendidikan Matematika dan Ilmu Pengetahuan Alam,
Universitas Pendidikan Indonesia, Jl. Dr. Setiabudi no. 229, Bandung 40154, Indonesia.

Received 18 July 2020, Revised 26 xxx 2020, Accepted 26 xxx 2020

Abstract

ZnS nanoparticles have prospects for use as diodes and sensors. These various uses caused the synthesis of ZnS
nanoparticles has been widely carried out. However, sphalerite resources will be depleted, thus requiring research
and development of renewable materials to meet the needs of zinc sulfide on an industrial scale. The purpose of
this study was to analyze various ZnS synthesis methods. In this study, various synthesis methods of ZnS from
various journals from 1982 to 2020 were discussed which include one-pot synthesis method, sol-gel, hydrothermal
process, coprecipitation, ultrasonic radiation, and microwave irradiation. These methods have their advantages
and disadvantages. The results of the study show that the wave irradiation method is more proper for the synthesis
of ZnS, especially on an industrial scale. This is because the precursors used are commercially available, the
reaction time is short, the operating temperature is low, and the products have high purity. Several raw materials
have prospects for the synthesis of ZnS including, Zn(CH3COOH)2.2H2O, CH4N2S, Na2S, ZnSO4.7H2O, and ZnO.
We hope this study can provide references to readers, industry, and researchers in the field of material
development regarding efficient and effective synthesis methods of ZnS on a large scale.

Keywords: coprecipitation, hydrothermal process, microwave irradiation, one-pot, sol-gel, sphalerite, ultrasonic
radiation, zinc sulfide (ZnS).
*Corresponding author. E-mail address: [email protected]
ISSN : 2458-6544 © 2021 ; www.mocedes.org. All rights reserved.
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1.! Introduction
Nanostructure materials have dimensions of about 1-100 nm. Nanostructures can be divided into 0
dimensions/uniform), 1 dimension/lengthwise, and 2 dimensions/planar [1]. Semiconductor
nanostructure materials recently attracted a lot of interest. Especially its application as optoelectronic
materials [2]. Semiconductor nanostructures have a variety of different properties due to the sharing of
3-dimensional electrons and holes in volume or the fact that the number of atoms on the surface is
proportional to that particles [3].
Zinc sulfide has a wide energy bandgap of 3.7 eV at 300 and it is one of the first semiconductors to be
discovered and widely used in various fields, for example in optical devices, sensors, and the
environment [4,5].
ZnS applications can be found in light-emitting diodes [6], electroluminescence [7], flat panel solar cells
[8], infrared windows, sensors [9], wastewater treatment [10], photocatalysis, and biological sensors
[11]. The use of ZnS in optical devices is supported by its properties that have a high index of refraction
and transmission in the visible light region [12].
Zinc sulfide has two common allotropes, namely, zinc blende (sphalerite) and wurtzite with a cubic
structure. The cube shape has high stability at low temperatures, but at 1296K it can form polymorphs
[13]. Under atomic conditions, these two allotropes have a coordination number of four forming a
tetrahedral structure [14].
Sphalerite is composed of zinc and sulfur atoms that are tetrahedral coordinated and stacked in an
ABCABC pattern with lattice parameters a = b = c = 5.41 Å. While wurtzite contains zinc and oxygen
atoms stacked in an ABABAB pattern with lattice parameters a = b = 3.82 and c = 6.26. As a result, the
electronic structures of the two allotropes are different. Wurtzite has a bandgap of 3.77 eV [15] while
sphalerite is 3.72 eV [16].
Hexagon wurtzite can metastasize thermodynamically and can change the hexagonal structure into a
cubic crystal structure spontaneously through reaction with organic substances [17].
ZnS was found to be more thermodynamically stable in the form of 'cubic sphalerite'. Pure sphalerite
has a clear crystal form. The higher impurities such as iron, the darker the color of the sphalerite crystals
[18].
ZnS nanoparticles have anomalous physical and chemical properties such as have higher surface and
volume ratio, quantum size effect, surface and volume effect, macroscopic quantum tunneling effect,
more optical absorption, thermal resistance, and low melting point. Table 1. presents the properties of
zinc sulfide [19].

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Table 1. Properties of Zinc Sulfide. This table is adopted from references [19].
Molecular Weight 97.46 g/mol
Zinc-12
group
Sulfur-16
Crystal structure Cube
Density 4.079 g/cm3
Melting point 1185°C
Boiling point 1850°C
Dielectric constant 8.9
Band Gap 3.54 ev
Electron mobility 180 cm2/Vs
formation energy 477 kJ/mol
Thermal expansion 6.36 µm/m°C
coefficient
Heat capacity 0.472 J/g°C

This article aims to present information about the source of the material and the synthesis method of
zinc sulfide nanoparticles, which is equipped with information about the advantages and disadvantages
of each synthesis method. The synthesis methods of ZnS nanoparticles presented include the one-pot
method, sol-gel formation, hydrothermal processes [4], coprecipitation [20], ultrasonic radiation [21],
and microwave radiation [22]. Information about the ZnO synthesis method is summarized in Table 2.

2.! Synthesis of ZnS Nanoparticles

The synthesis of ZnS nanoparticles consists of two methods, namely the physical method and the
chemical method. The chemical method includes thermal decomposition methods, micro-emulsions, sol-
gels, and others. These methods require high reaction temperatures, lots of organic solvents, high
operating and equipment costs, and complex process controls. Even in many cases, the particles
produced by this method have not good particle size and easily clump [38].
The synthesis of ZnS nanoparticles also can be done by a dopping method. ZnS nanoparticles doped
with optical luminescence centers can create many new physics and applications. Some materials apply
to luminescence devices, phosphors, optical sensor light emitters, and others [39]. Zinc sources from
sphalerite can use as salts such as zinc acetate and zinc chloride, which reacted with thiourea to obtain
ZnS nanoparticles [40].

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Table 2. Materials, Methods, Advantages, and Disadvantages of Synthesis of ZnS.

Materials Method Advantages Disanvantages Reference

Zn(MA)2 One-Pot •! Precursors are non- •! The experimental [23, 24,
toxic, inexpensive, and setup is tricky. 25]
readily available. •! If the temperature
•! The morphological is too high,
structure and structural damage
electrochemical can occur and
properties of the product reduce the safety of
can be controlled by the preparation
preparative parameters process.
such as temperature,
solution pH, and
precursor concentration.
Zn(CH3COO)2· Sol-Gel The product has high purity •! Preparations of [26,27,24]
2H2O in terms of physical large quantities of
properties, morphology, precursors are
and chemical properties. difficult to prepare
without cracking.
•! The reaction time
is too long due to
slow drying to
avoid cracking.
•! Conditions must
be controlled well.
Zn(CH3COO)2, Hydrotherma •! Easy and high yielded •! The reaction time [17, 28,
CH4N2S, Na2S, l products. is long so it 29, 30, 31]
oleic acid, •! The product crystal has consumes a lot of
Eu(CH3COO)3 high purity, good energy.
6H2O. dispersion, and high •! This method
stability. requires an
•! The precursor is non- expensive
toxic and inexpensive. stainless-steel
•! Environmentally autoclave and
friendly. Teflon.
•! The method can be •! Reactions are
carried out in various difficult to study
combinations of because they are
aqueous and solvent closed systems.
mixture-based systems.

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Table 2. (continued) Materials, Methods, Advantages, and Disadvantages of Synthesis of ZnS.

ZnSO4.7H2O Coprecipitation •! Affordable cost. •! The time to make [20, 32,

and CH4N2S. •! Simple working the product is fairly 33, 34, 35]
method. long.
•! Produce high quantities
of products.
•! The method can be used
for large-scale
production.
ZnO and Na2S Ultrasonic •! It does not take much The radiation source [28, 36,
Radiation time because of the only relies on 21]
large temperature and ultrasonic radiation.
pressure and extreme
cooling.
•! High reaction yield.
•! Enhance organic
transformation.
Zn(CH3COOH) Microwave •! Precursors are •! The control method [22, 37,
2.2H2O and Irradiation commercially available. on the size and 12]
CH3CSNH2. •! Short reaction time. morphology of the
•! Low operating results is less
temperature. accurate.
•! The method was carried
out under ambient
atmospheric conditions.
•! The resulting product
has high purity.

2.1 One-Pot
This process uses one reaction. The purpose of this process focused on ZnS materials. The reactions
used in this process are reactions with easy steps, a fast process, and high product yields [41].
Preparation of ZnS use chemical reagents such as ZnCl2 and ZnSO4 with a sulfur source from Na2S [42].
Sources of sulfur contain thiosulfate because thiosulfate hydrolyzed to S2 [43]. It also contains organic
solvents such as methanol, ethanol, ethylene glycol, and a small amount of acid or base to catalyze. In
this method, it is necessary to control physical properties such as surface area, pore size, and pore
volume. So organic stabilizers are uses [44]. Although the one-pot synthesis process has been using
successfully to prepare ZnS particles with high product purity, this process is still limited to the use of
high temperatures. So, organic stabilizers and solvent media can remove by the calcination process [45].
The S2- ion will bind to Zn2+ then become ZnS in the form of a precipitate. [42]

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S2O32- + H2O ! SO42- + H2S (1)

H2S + Zn2+ ! ZnS + 2H+ (2)
In general, the reaction used is shown in Figure 1. The product of this process is shown in Figure 2.

Figure 1.!The chemical reaction of the One-Pot process for the formation of ZnS. Figure was adopted
from Ummartyotin and Infahsaeng [46].

Figure 1. ZnS nanoparticles. The results of the One-Pot method with various characterizations. The
figure was adopted from Li, et al. [47].

2.2 Sol-Gel
The sol-gel formation is a method that produces solid materials from nanoparticles. This method
involves the conversion of monomers into colloidal solutions. The reagents used are metal-based
alkoxides. In the formation of sol-gel, there are different categories, namely sol and gel [48]. The factors
that influence this method are gel formation reaction time, solvent and pH conditions, chemical reagents,
and temperature during calcination [49]. This process requires a stabilizer to protect the particles from
particle enlargement. The thing to note in this method is to use a clean surface [3].
The size and shape of ZnS are controlled by adjusting the molecular weight of the stabilizer. For
example, polyvinylpyrrolidone, polyethylene glycol, and polyacrylic acid with various molecular weight
sizes from 500-100,000 are used as stabilizers. So that different sizes of ZnS are produced [46].

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Figure 3. Schematic of the Sol-Gel process for the formation of ZnS. Figure adopted from
Ummartyotin and Infahsaeng [46].

The results of ZnS nanoparticles are shown in Figure 4.

Figure 4a. Transmission of electrons in the form of a micrograph. Figure adopted from Bhattacharjee,
et al. [51].
Figure 4b. ZnS film. Sol-gel method results. Figure adopted from Bhattacharjee, et al. [51].

2.3!Hydrothermal Process
There are methods of preparation ZnS, namely the oil phase method and the water phase method. The
hydrothermal method belongs to the water phase method, which is environmentally friendly because it
uses water as a solvent and inorganic salts as reaction precursors. Therefore, the operation is simple, the
reagent is non-toxic and inexpensive. This method is widely used, and the crystals obtained have high

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purity and good dispersion. The advantages of this method are its high stability and fast process requiring
only a low thermal supply [30].
The hydrothermal technique is one of the effective methods for the preparation of ZnS particles. This
technique involves the crystallization of aqueous solution materials from high temperatures at high vapor
pressure. Theoretically, it is defined as the synthesis of single crystals that depend on the solubility of
minerals in hot water under high pressure. The apparatus consists of a pressurized steel container called
an autoclave. The container contains nutrients supplied along with water [46].
This method uses autoclaves made of steel cylinders with tight covers. It is used for holding high
temperatures and pressures inside for a long time [51].
The hydrothermal method is also effective for the preparation of inorganic nanomaterials such as oxides,
sulfides, phosphates, zeolites, and diamonds. The particle size and distribution, phase homogeneity, and
morphology of the material are controlled well in this method [52]. The result of the hydrothermal
process is shown in Figure 5.

Figure 5. ZnS Nanoparticles. The result of the Hydrothermal process with a variety of solvents and
reaction conditions. Figure adopted from Lee [28].

The synthesized ZnS nanoparticles were analyzed by X-Ray Diffraction D-8 Advance Bruker Germany
equipped with graphite for Cu Kα (λ = 2,54056 Å) radiation monochromator. This is to determine the
structural properties of ZnS nanoparticles [35]. The results of the ZnS analysis using XRD are shown in
Figure 6.

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Figure 6. Results of XRD Analysis of ZnS Nanoparticles with Hydrothermal and Coprecipitation
Methods. Figure adopted from Master, et al. [35]

From the figure, it can be concluded that each reflection pattern of (111), (220), and (311) shows the
structure of ZnS nanoparticles is zinc blende or sphalerite.

2.4!Coprecipitation
Coprecipitation and deposition synthesis methods with spin coating are considered cost-effective
methods [20]. In addition, this method is a simple technique, high product yield, and can use for large-
scale production. [32][34]. In his research, Harvey used ZnSO4.7H2O, ammonium sulfate, and thiourea
reagents with a molar ratio of 1:1.5:1.5 [33]. ZnSO4.7H2O and ammonium sulfate mixed with 50 mL of
distilled water. Then ammonia was added to the mixture until a clear metal complex formed (pH
maintained at 9.5). Thiourea dissolved in the previous solution. The sample solution was washed with
distilled water and methanol to remove impurities [33]. The ZnS nanoparticles synthesized by the
coprecipitation method are shown in Figure 7.

Figure 7. ZnS Nanoparticles by coprecipitation method. Figure adopted from Vazquez., et al. [12].

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The results of the synthesis of ZnS nanoparticles are characterized by XRD Rigaku Mini using Cu Kα
radiation (λ = 0.1541 nm). The diffractogram was recorded in the range of 10-80°. The results of the
XRD analysis of ZnS nanoparticles are shown in Figure.5 [53]. The average ZnS particle size was
calculated by the Debye formula and it found that the particle size was 4.9 nm [53]. Bahmani conducted
a similar experiment and obtained data that ZnS nanoparticles tend to show a zinc blende or sphalerite
crystal structure [54].

Figure 8. Results of XRD Analysis of ZnS Nanoparticles with Coprecipitation Method. Figure
adopted from Othman, et al. [53]

2.5!Ultrasonic Radiation
Ultrasonic waves are widely used to produce new materials with unusual properties and can induce the
formation of particles in smaller sizes with a larger surface area compared to other methods [63].
ZnS nanoparticles can be prepared using the method without the use of any stabilizer. ZnO as a source
of Zn mixed with a solution of Na2S as a source of S under ultrasonic radiation in a water bath for 2
hours. After reacted, the resulting product was washed and dried under reduced pressure [21].
The use of ultrasonic irradiation for the production of nanomaterials has become a very interesting
research topic. This is due to the simplicity of the sonochemical method, the low cost of the equipment,
and in most cases, the prepared material obtained in the crystalline phase. The chemical effects of
ultrasonic irradiation come from non-linear acoustic phenomena, especially acoustic cavitation which is
divided into three distinct stages namely formation, growth, and bursting of bubbles [55].
Ultrasonic is a unique interaction between energy and matter due to the chemical effects of ultrasound
arising from the acoustic membrane, including the formation, growth, oscillation, and fall of gas bubbles
in an adsorbed form under the right conditions. The collapse of the gas bubbles is caused by cavitation
which results in intense local heating, high pressure, and a short life span. Acoustic cavitation serves as

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a means to concentrate dead sound energy. In an extreme environment, it can accelerate the condensation
or hydrolysis reaction [56]. During cavitation, falling bubbles generate intense transient hot spots, high
pressures, and short service life, consequently promote high-energy chemical reactions. A series of
ultrasonic applications increase chemical reactivity [61]. The chemical effects of ultrasonic radiation
cause many unique properties in irradiated solutions. With these extreme conditions, ultrasonic radiation
methods are used to prepare nanoscale metals, metal oxides, metal sulfides, and others [57].
Ultrasonics are widely used in organic synthesis over the past few years. Compared with the traditional
method, this method is better used and the reaction can be carried out with higher yields, shorter reaction
times, and lighter conditions under ultrasonic radiation [58].
ZnS nanoparticles will be prepared using an inert-gas evaporation technique with induction heating.
Furthermore, ZnS nanoparticles mixed with Na2S solution under ultrasonic radiation. The product
obtained was washed and separated by centrifugation and followed by drying. The synthesis product of
ZnS using the ultrasonic radiation method with various solvents and reaction conditions is shown in
Figure 9.

.
Figure 9. ZnS Nanoparticles. The results of the synthesis by ultrasonic radiation method with a variety
of solvents and reaction conditions. Figure adopted from Lee [28].

The product obtained by ultrasonic radiation method tested with XRD, TEM, UV-VIS
spectrophotometer, and photoelectron spectrophotometer [3].

2.6!Microwave Irradiation
Synthesis of ZnS nanoparticles can be done by the microwave irradiation method. The advantages of
this method are using commercially available precursors, shorter reaction times, lower operating
temperatures, carried out under ambient atmospheric conditions, and the product has a high purity [22].

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Microwaves have lower quantum energy than the ionization energy of compounds, which is about 1.24
× 10-6 -1.24 × 10-3eV. Microwaves produce a dielectric heating effect [59].
The heat is caused by the interaction of the molecular dipole moment with high-frequency
electromagnetic radiation, which is 2.45GHz. Water has a high dipole moment so it is widely used as a
solvent in reactions with microwaves [62].
The precursors used in the microwave irradiation method included zinc salts, such as zinc acetate and
thioacetamide [37]. The stages of ZnS synthesis using the microwave irradiation method are as follows:
•! Zinc acetate solution (Zn(CH3COOH)2.2H2O) and thioacetamide solution (CH3CSNH2) were
prepared and combined stoichiometrically.
•! The solution was diluted to 400 mL with the addition of distilled water.
•! The solution is stored in a magnetic stirrer for one hour at a speed of 840 rpm to make a
homogeneous solution.
•! The solution was placed in a microwave oven (LG make) with a power of 900W for 12 minutes.
•! A white precipitate was obtained and it was washed with distilled water and dried in an oven at
60° for 6 hours [37].
The representation of zinc sulfide nanoparticles in the form of a micrograph is shown in Figure 10.

Figure 10. ZnS micrograph form. The result of the synthesis by microwave irradiation method. Figure
adopted from Vazquez., et al. [12].

Conclusion
Semiconductor nanostructure materials recently attracted a lot of interest. One of them is zinc sulfide.
This is because zinc sulfide has very diverse and useful applications. Its abundant source in the form of
sphalerite is also one of the factors that zinc sulfide is easy to obtain.
Several ZnS nanoparticles synthesis methods can be carried out, including the one-pot process, sol-gel
formation, hydrothermal process, coprecipitation, ultrasonic radiation, and microwave irradiation. Some

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of these methods have advantages and disadvantages. In terms of material availability, time efficiency,
and quality of results, the microwave irradiation method has advantages over other methods and it is
more proper, especially on an industrial scale. The results of the XRD analysis of ZnS nanoparticles
showed that ZnS has a Zinc Blende (Sphalerite) structure.

Acknowledgments
We acknowledged Bangdos Universitas Pendidikan Indonesia.

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