ISSN 1070-4272, Russian Journal of Applied Chemistry, 2017, Vol. 90, No. 2, pp. 292−297. © Pleiades Publishing, Ltd.

, 2017.

VARIOUS TECHNOLOGICAL
PROCESSES

Synthesis and Characterization of CdS Nanoparticles

Prepared by Precipitation in the Presence of Span 20
as Surfactant1
S. A. Walya,b*, M. M. Shehatab,c**, and H. H. Mahmoudc
a Second Research Reactor, Nuclear Research Center, Atomic Energy Authority, Cairo, Egypt
b Radiation Chemistry Department, National Center for Radiation Research and Technology,
Atomic Energy Authority, Cairo, Egypt
c Central Laboratory for Elemental and Isotopic Analysis, Nuclear Research Center,

Atomic Energy Authority, Cairo, Egypt

e-mail: *shf_waly@yahoo.com, **m_shehata2100@yahoo.com

Received March 9, 2017

Abstract—Cadmium sulfide nanoparticles with average size of ≈16 nm have been synthesized using chemical
precipitation reaction of CdCl2 and Na2S in the presence of nonionic surfactant stabilized reverse emulsions.
Sorbian monolaurate (Span 20) is used for the stabilization of emulsions. The influence of Span 20 on controlling
the size and properties of CdS nanoparticles were studied. The obtained CdS nanoparticles were characterized by
scanning electron microscopy (SEM), transmission electron microscopy (TEM), Energy-dispersive x-ray (EDX),
and X-ray diffraction (XRD). The optical properties of CdS nanoparticles are investigated systematically by
UV-visible absorption spectroscopy. The blue shift in the absorption region and increase in the bandgap to the
larger value (2.77 eV) are attributed to the nanosize of the obtained particles.
DOI: 10.1134/S1070427217020203

INTRODUCTION as the S–2 source at higher temperature [16] and chemical

Cadmium sulfide (CdS) nanoparticles is one of
the most promising semiconducting material because
it has many applications such as in solar cells, electronic,
optoelectronic semiconducting devices, display devices
and as photocatalyst [1, 2]. Synthesis, characterization
and studies of optical properties of cadmium sulfide
have been researched, by several research groups [3–6].
However due to the high cost of preparing such a material,
several methods are reported for the preparation of CdS
in powder and thin film forms using a relatively simple,
inexpensive and scalable technique [7–14].
The synthesis of CdS nanoparticles have been carried
out by different methods such as the direct reaction
of metals with sulfur powder under high temperature,
the thermal decomposition of molecular precursors
containing M–S bonds [15] or the use of poisonous H2S
1 The text was submitted by the authors in English.
precipitation method [17].
Various sources of sulfur for preparation of CdS nano-
particles have been reported [18]. However, only sodium
sulfide, hydrogen sulfide gas and thiourea are most
commonly used. Sodium thiosulfate upon irradiation by
gamma rays as well as by direct use has also been used
for preparation of CdS nano-particles and powder [19].
Different wet chemical methods have been developed
for the preparation of CdS nanoparticles and reverse
emulsion method was accepted for the synthesis [20–26].
The knowledge of structural and optical parameters such
as optical band gap, optical absorption, transmission, and
dielectric constants, etc. are essential prerequisite to know
the optimal use of this material in device applications.
The using of the surfactants provides a means to
achieve control over the CdS nanoparticle size and size
distribution, which is essential for tailoring optical,
electrical and structure properties of nanoparticles for

292
 SYNTHESIS AND CHARACTERIZATION OF CdS NANOPARTICLES
O CH2(CH2)9CH3
O
O CdCl2·2.5H2O(aq) + Na2S·9H2O(aq)
HO
H OH
OH
Fig. 1. The chemical structure of Span 20.
specific applications. High surfactant concentration
decreases surface tension and stabilizes newly developed
surfaces during homogenation and production of smaller
particles [30]. Span 20 surfactant has a polar head and
a non-polar tail as shown in Fig. 1; orient themselves
according to the polarities of the involved chemical
substituents. It is known that the structures of products
depend on the rate of nucleation and growth of the
reaction products.
In the present work a simple route for the preparation
of cadmium sulfide (CdS) nanoparticles is presented. The
effect of Span 20 as surfactant on the properties of CdS
NPs prepared by precipitation method is investigated.
The structural, morphology and optical parameters of
the prepared CdS nanoparticles have also been studied.
EXPERIMENTAL
Synthesis of CdS nanoparticles. All reagents
(CdCl2, Na2S, and ethanol) were of analytical grade
and Span 20 was purchased from Sigma-Aldrich. High
purity double distilled deionized water (18 Megaohm
cm) was used in all dilutions during the study. The CdS
nanoparticles were synthesized by chemical reaction
50 μm
Fig. 2. SEM images of the synthesized CdS NPs in the presence of 5 % of Span 20.
RUSSIAN JOURNAL OF APPLIED CHEMISTRY Vol. 90 No. 2 2017
293
of CdCl2 solution with Na2S solution according to the
following equation:
Room temperature
––––––––––––––→ CdS(S) + 2NaCl + 11.5H2O. (1)
Aqueous solutions of CdCl2 with concentration of
0.05 M were mixed with 0.05M Na2S. A support solvent
was prepared by mixing 5 and 10 % volume of Span 20
surfactant. The precipitate CdS was washed five times
with deionized water (18 Megaohm cm) to eliminate NaCl
and then diluted with ethanol. The formed emulsions was
centrifuged at 4000 rpm for 15 min at room temperature,
after the centrifugation process the supernatant was
decanted and the precipitate was then dried in the drying
oven at 50°C. Scanning electron microscope analysis
was performed to visualize the external morphology of
the synthesized CdS nanoparticles (SEM: JEOL JSM
5600 LV; Tokyo, Japan). The particle size and shape
were studied by transmission electron microscopy (TEM:
JEOL JEM 1200EX II) while X-ray diffraction patterns
were recorded to study structure of the CdS nanoparticles
(NPs). Energy-dispersive X-ray analysis (EDX) was used
to determine the purity of the obtained CdS NPs. The
optical properties of the obtained CdS NPs were studied
by UV-visible absorption spectroscopy (Lamda-25;
PerkinElmer; Waltham, Massachusetts) between 280
and 800 nm.
RESULTS AND DISCUSSION
The effect of nonionic Span 20 on the size of CdS
nanoparticles was investigated. Span 20 was used to
decrease the reaction rate at a lower temperature and
lower reactant concentrations. This indicates that the
10 μm
294
cps Cd
300
S
200 C
100
0
0 5
Fig. 3. EDX spectra of the synthesized CdS NPs in the presence of 5% of Span 20.
non-ionic surfactant Span 20 plays a critical role in
the formation of CdS nanoparticles.
Scanning electron microscopy (SEM-EDX).
The surface morphology of the synthesized CdS
nanoparticles were investigated using scanning electron
microscope (SEM) and Energy Dispersive X-Ray
Spectrometry (EDX) to determine the surface structure
and elemental composition. The SEM images of CdS
nanoparticles are shown in Fig. 2. This indicates the
formation of spherical particles. The related EDX
analysis for understanding the elemental composition
of CdS NPs by matching the relative ratio between the
two elements showed that the ratio between S and Cd is
stoichiometric. Figure 3 represents EDX spectra of CdS
NPs, which show that CdS nanoparticles are free from
impurities. The presence of carbon and copper peaks in
(a)
6.75 nm 7.88 nm
9.14 nm
100 nm
Fig. 4. TEM images of the synthesized CdS nanoparticles in the presence (a) 5, (b) 10 % of Span 20 surfactant ratio.
RUSSIAN JOURNAL OF APPLIED CHEMISTRY Vol. 90 No. 2 2017
WALY et al.
Cu
10 15 20
Energy, keV
the spectra was due to the holder and carbon paste used
in the spectrometer.
Transmission electron microscope (TEM). The
transmission electron microscope images of CdS
nanoparticles prepared at 5 and 10 % ratios of Span 20
surfactant added to CdCl2 and Na2S were recorded as
shown in Fig. 4. The TEM images confirm that the CdS
was formed in closed packed domain which revealed
that some of nanocrystals spherical shapes and a number
of well dispersed are observed with a fairly even size
distribution. TEM analysis shows that the particle size is
mostly in the ranges from 4.5 to 54.0 nm and the average
particle size is 16 and 28 nm in case of 5 and 10% of
Span 20, respectively.
UV-visible spectroscopic study. The UV-visible
absorption spectra and transmittance spectra of
(b)
54.0 nm
100 nm
 SYNTHESIS AND CHARACTERIZATION OF CdS NANOPARTICLES 295
A.U., %

Fig. 5. UV-visible Spectrum of the synthesized CdS-NPs (a) Optical absorption spectrum, (b) transmission absorption

the synthesized CdS nanoparticles in the wavelength

range 280−800 nm as shown in Fig. 5. CdS is a direct
band gap material, with absorption edge for the bulk CdS
at 51 2 n m which has the band gap energy ~2.4 eV [27].
From the absorption spectrum of CdS nanoparticles, a
well-defined absorption peak at 497 nm is observed. The
exciton absorption observed at about 497 nm, which is
blue shifted compared with the characteristic absorption
of bulk CdS may be due to quantum confinement effects
[28].
The optical band gap energy characteristic plays
a crucial role in the utilization of the materials in the
optoelectronic applications. The relation between
absorption coefficient and optic band gap is given by
Tauc relation as the following: Fig. 6. Direct band gap determination of the synthesized CdS
nanoparticles.
αhυ = A(hυ – Eg)p. (2)

where hυ is the photon energy and Eg is the band gap, υ is
the frequency of the incident radiation, and h is Planck’s
constant and A is the constant which is different for
different absorption. The exponent p takes a value of 1/2
for direct allowed transitions.
The direct energy band gaps of the CdS nanoparticles
were determined by extrapolating the linear portion of
the plots of (αhυ)2 against (hυ) to the energy axis, as
shown in Fig. 6. The calculated direct band gap for the
CdS nanoparticles is estimated to be Eg = 2.77 eV. The
increase in the band gap as compared to the reported
values of the bulk material (2.40 eV) for CdS [29], may
be due to the formation of nanograins or originated
from reduced particle size for the synthesized CdS
nanoparticles. The band gap values originate from the
quantum confinement effect, which is caused by the
nanosize of the materials.
X-ray diffraction. It has been observed that CdS
nanoparticles display both cubic and hexagonal structures
depending upon the synthesis method used. Thermal
annealing causes phase transition from cubic to hexagonal
with resultant band gap shift in CdS. It is very difficult
to differentiate the cubic from the hexagonal because the
cubic (111) and the hexagonal (002) main peaks almost
overlap, coinciding within 1%.
Structural analysis of synthesized CdS nanoparticles
was studied using X-ray diffraction. X-ray diffraction
pattern of CdS nanoparticles is shown in Fig. 7. Three
broad and symmetric peaks were observed at 2values
of 26.514°, 43.762°, and 52.0° corresponding to the three

RUSSIAN JOURNAL OF APPLIED CHEMISTRY Vol. 90 No. 2 2017

296 WALY et al.
256 26.514°
196
144
100
64
36
16
0
10 20 30
Fig. 7. XRD pattern of CdS nanoparticles in the presence of 5 % Span 20.
crystal phases of (111), (220) and (311), respectively. The
diffraction peaks obtained in the XRD pattern show the
cubic structure of CdS (JCPDS 10–454). This shows that
the samples have zinc blende. The XRD peaks of the cubic
CdS are bread due to the small grain size and low degree
of the crystallinity of the nanoparticles. Also no other
significant peaks are seen, which reflects the high purity
of the obtained CdS NPs. The average particles size of
the CdS nanoparticles calculated using Scherer formula
is 16 nm which agree with the result obtained by TEM:
t = 0.9λ/B cos θ, (3)
where t is the average particle size, λ is the wavelength
of X-ray radiation, B is the full-width at half-maximum
(FMWH) of the peak, and θ is the angle of diffractionp.
CONCLUSIONS
In the present study, we have successfully synthesized
CdS nanoparticles using co-precipitation method. EDX
analysis confirmed the high purity of CdS nanoparticles
obtained from the chemical reaction between CdCl2 as
the source of Cd+2 and Na2S as the source of S–2 in the
presence of Span 20 as surfactant. XRD pattern of the
obtained CdS nanoparticles indicates to formation of the
cubic CdS nanoparticles. SEM and TEM images reveal
that the homogeneous morphology of the obtained CdS
nanoparticles and the spherical CdS particle size lies
between 4.5−54.0 nm with median diameter of 16 and
28 nm in case of 5 and 10% of Span 20, respectively.
RUSSIAN JOURNAL OF APPLIED CHEMISTRY Vol. 90 No. 2 2017
43.762°
52.0°
40 50 60
2θ, deg
The direct band gap energy of the CdS nanoparticle was
found to be 2.77 eV. The increase in the direct band gap
as compared to the bulk material (2.40 eV) for CdS,
may be due to the formation of nanograins or originate
from reduced particle size for the synthesized CdS
nanoparticles.
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