Copyright © 2018 American Scientific Publishers Nanoscience and

All rights reserved Nanotechnology Letters

Printed in the United States of America Vol. 10, 1–9, 2018

Doping Dependent Structural, Optical, Thermal and

Catalysis Properties of Synthesized Cadmium
Sulfide Nanoparticles
W. T. Salam1 † , M. Ikram1 ∗ † , I. Shahzadi2 , M. Imran3 4 , M. Junaid1 , M. Aqeel1 , S. Anjum5 ,
A. Shahzadi2 , H. Afzal1 , U. Sattar1 , A. Asghar1 , A. Wahab1 , M. Naz6 , M. Nafees1 , and S. Ali1 7
1
Solar Cell Applications Research Lab, Department of Physics, Government College University Lahore, 54000, Pakistan
2
Punjab University College of Pharmacy, Punjab University, Lahore, 54000, Pakistan
3
Technical Institute of Physics and Chemistry, Chinese Academy of Sciences, 29 Zhongguancun East Road,
Haidian District, Beijing 100190, China
4
University of Chinese Academy of Sciences, Beijing 100049, China
5
Department of Physics, COMSATS University Islamabad, Lahore Campus, Lahore 54000, Pakistan
6
Biochemistry Lab, Department of Chemistry, Government College University Lahore, 54000, Punjab, Pakistan
7
Department of Physics, Riphah Institute of Computing and Applied Sciences (RICAS), Riphah International University,
14 Ali Road, Lahore, Pakistan

A simple and cost-effective route has been employed to synthesize undoped and copper doped
(2, 4 and 6) % cadmium sulfide (CdS) nanoparticles. Resulting materials were characterized by
various techniques as XRD results confirmed the formation of hexagonal crystal structure for doped
and undoped CdS nanoparticles with crystallite size varying from 11–17 nm calculated by Sherrer
equation. The Williamson Hall (W-H) plot is used to examine particle size and lattice strain of pre-
pared pure and Cu doped CdS nanoparticles and compared the particle size with Sherrer equation.
Moreover, significantly reduced the intensity of diffraction is also evident accompanied by slight
peak-shifting towards higher angles. Agglomerated spherical morphology of the CdS nanoparticles
with decreasing particle size upon Cu doping was observed by SEM. FTIR spectra was found
to consist of stretching vibrations from Cd-S and other related groups with negligible changes in
the vibrational modes upon doping. The UV-Vis analysis demonstrates a significant increase in
absorption intensity upon doping along with slight blue shift leading to an increased bandgap for
doped CdS. The Raman spectroscopy measurement was performed on nanoparticles and thermal
properties in different environment were investigated by DSC/TGA. These studies represent a cost-
effective way to prepare CdS and related materials with tunable bandgap. This report highlights the
effect of bared and various concentrations of Cu doped CdS nanoparticles in the degradation of
cationic dye methylene blue by NaBH4 .
Keywords: CdS Nanoparticles, Copper, FESEM, FTIR, Chemical Precipitation Techniques,
Methylene Blue.

1. INTRODUCTION in bulk form. It is widely used in applications such as het-

It has been commonly observed that the CdS forma-
tion as p-type is very challenging mostly due to self-
compensation effects because of sulfur vacancies.1 Many
research groups introduced dopants to alter the properties
of the inorganic semiconductor to enhance the efficiency
of photovoltaic devices.2 Cadmium sulfide is a group II–VI
semiconductor material with a bandgap (B.G) of 2.42 eV
∗
Author to whom correspondence should be addressed.
†
These two authors contributed equally to this work.
erojunction solar cells, laser materials, optoelectronic and
photoconductive devices, light emitting diodes, and optical
detectors.3–5 CdS shows n-type conductivity to the intrinsic
defects present in it while substitutional doping tends to
generate an acceptor level thus changing its conductivity
from n-type to p-type.6 7
In thin-film solar cells, n-type CdS is used as a win-
dow material4 while in bulk-hetero-junction (BHJ) solar
cells CdS nanoparticles are incorporated as electron accep-
tor materials in the active layer along with electron donor

Nanosci. Nanotechnol. Lett. 2018, Vol. 10, No. xx 1941-4900/2018/10/001/009 doi:10.1166/nnl.2018.2839 1

Doping Dependent Structural, Optical, Thermal and Catalysis Properties of Synthesized Cadmium Sulfide Nanoparticles Salam et al.
polymers.3 In thin-film solar cells, use of CdS as n-type
window layer comes with certain disadvantages such as
small band gap and lattice mismatch with p-type thin
films.5 While in BHJ solar cells, an efficient device oper-
ation is determined by the generation of photo-induced
charge carriers at the organic-inorganic interface which
in-turn depends on the difference between the bandgap
energies of organic and inorganic components. A large
difference in the bandgap energies would result in short-
diffusion lengths for charge carriers and corresponding
degraded power conversion efficiency.8–18
Therefore, thin films and BHJ devices can be made
comparatively more efficient by tunning the CdS bandgap.
These requirements can be achieved by the addition of
impurities such as Cu, Ag and Fe into the pristine CdS.
In past, various techniques such as vacuum deposition,19
vacuum co-evaporation,6 spray-pyrolysis,20 mechanochem-
ical alloying and dry process21 have been employed to pro-
duce Cu doped CdS. However, these techniques employ
expensive equipment and generation of high vacuum can
take several hours.
Organic dye effluents are widely used in paper, plas-
tic, textile and food industries, though the hazardous
effects of these coloured materials are the major threat
to the humans and aquatic organisms. Hence it is
essential to remove these toxic materials from waste
water resources.22 23 Traditional treatment methods include
ultrafiltration, adsorption, biodegradation, photochemical
chemical, and electrochemical process24–28 are inappropri-
ate and insufficient to remove huge amounts of organic
dyes from industrial effluents; such as adsorption is a
non-destructive technique, it simply convert these coloured
materials from one phase to another. Nowadays, metal
nanoparticles emerged as an effective nano-catalyst that
rapidly replacing conventional water treatment method due
to their finite size and large surface to volume.29
In this study, we report the synthesis of doped and
undoped CdS nanoparticles using chemical precipitation
technique. Structural, morphological, and optical proper-
ties were evaluated as a function of doping. The catalytic
activity of undoped and Cu doped CdS nanoparticles were
investigated by using them in the degradation reactions of
methylene blue by NaBH4 .
2. MATERIALS AND METHODS
2.1. Materials
Following materials were used for the synthesis of
doped and undoped CdS nanoparticles: cadmium chlo-
ride (CdCl2 · 2H2 O) as the cadmium source, thioacetamide
(C2 H5 NS) for the sulfur source, copper chloride (CuCl2 ·
2H2 O) as dopant metal salt and ethylene glycol (C2 H6 O2 
as a solvent. Methylene blue (MB) and sodium borohy-
dride (NaBH4  were procured from Sigma-Aldrich. All
materials were of analytical reagent grade and purchased
from Merck.
2 Nanosci. Nanotechnol. Lett. 10, 1–9, 2018
2.2. Synthesis
The copper doped CdS nanoparticles were synthesized by
the precipitation method using ethylene glycol as a solvent
and capping agent. Solution (I) was obtained by mixing
0.02 mol of CdCl2 · 2H2 O and an equimolar amount of
C2 H5 NS into 120 ml of ethylene glycol. Different weight
percentages of CuCl2 · 2H2 O were dissolved in ethylene
glycol and mixed slowly in the solution (I). The resulting
solution was stirred at 100  C on a hotplate for four hours
until the appearance of brown precipitates. These precip-
itates were filtered, washed with ethanol and deionized
water, and dried at 100  C. Similar procedure was used to
fabricate pure CdS nanoparticles without the addition of
CuCl2 · 2H2 O in the solution (I)
2.3. Catalytic Reduction of Methylene Blue
Sufficient deionized water was employed to dilute the
300 l of methylene blue solution (1 mM) in quartz cell.
Then, added 400 l of NaBH4 solution (0.1 M) and 300 l
of doped and undoped CdS nanoparticles solution to make
a final volume of 3.00 ml. The decolourisation of the dye
indicate methylene blue degradation because of reducing
agent (NaBH4 . In addition, degradation of the MB at
664 nm was recorded spectrophotometrically. The reaction
in the absence of nano-catalyst is conducted as a control
and absorption spectra were monitored at periodic inter-
vals in the range of 250–750 nm at 25  C.
2.4. Characterization
The structural analysis and phase identification of the pre-
pared samples were performed using the instrument PAN-
alytical X’Pert PRO XRD Company Ltd. Holland operated
at 40 kV with CuK radiation of wavelength 1.54 nm.
The surface morphology was analyzed by using FESEM
JSM-5910 with the accelerating voltage of 20 kV. The
FTIR spectra of CdS and Cu doped CdS nanoparticles
were recorded on Bruker TENSOR II in the range 600–
4000 cm−1 and the UV visible spectroscopy was carried
out on Genesys 10S UV-Vis spectrophotometer for optical
analysis.
3. RESULTS AND DISCUSSION
Figure 1(a) represents powder X-ray diffraction (XRD)
patterns of pure and Cu-doped CdS nanoparticles. The
XRD pattern of as-prepared CdS nanoparticles was fully
matched with JCPDS card number 01-075-1545. The
obtained diffraction peaks from the planes (102) and (103)
are the characteristic peaks of hexagonal close packed
(hcp) structure.30 It can be observed that doping signifi-
cantly reduces the intensity of diffraction peaks resulting in
a decreased crystallite size (Fig. 1(b)). Crystallite size for
doped and undoped samples is shown in Figure 1(c). The
doping effect is also manifested in the slight shifting of
XRD peaks towards higher angles which can be attributed
Salam et al. Doping Dependent Structural, Optical, Thermal and Catalysis Properties of Synthesized Cadmium Sulfide Nanoparticles

Fig. 1. XRD patterns of (a) W-H plot (b) and comparison between particle size and lattice strain (c) and crystallite size dependence on the concentration
of Cu in CdS (d).

to the difference in the atomic radii of Cu (1.35 Å) and
Cd (1.51 Å) atoms. Copper may have been doped substi-
tutionally into the CdS causing lattice contraction.7
In order to check the broadening of the peak with lattice
strains, different peaks were utilized from XRD pattern.
The strain induced broadening of the Bragg’s diffraction
peak can be calculated using Wilson and Stokes31 formula
Eq. (1).
 effect due to lattice strain.
 = hkl (1)
4 tan 
The broadening is contribution of lattice strain induced and
crystallite size and can be written as
hkl = D + 
measured crystallite size with W-H plot and Scherer equa-
tion is shown Figure 1(d). With higher amount of dop-
ing (6%), contribution of peak broadening due to lattice
strain is much prominent relative to particle effect broad-
ening which enhanced the induced lattice strain as well
as crystallite size (W-H) Figure 1(c). From Figure 1(d),
the crystallite size decreased gradually according to Sher-
rer equation because it does not consider the broadening
Field emission scanning electron microscopy (FESEM)
was used to analyze the surface morphology of undoped
and Cu doped CdS nanoparticles (Fig. 2). Figure 2(a)
reveals the formation of highly agglomerated spherical
(2) nanoparticles of pure CdS in the range of 0.2–1.5 m.

Using Scherer equation and (1) results in following

Eq. (3)
K
hkl = + 4 tan  (3)
DCos
Rearranging the Eq. (3) gives
K
hkl cos  = + 4 sin  (4)
D
The W-H plot of hkl cos  versus 4 sin  for pure and
doped CdS samples with concentration (0, 2, 4 and 6) %
are shown in Figure 1(b). The extracted values of crystal-
lite size (inverse of Y-intercept) and strain (slope of the
line) induced in the broadening of the peak are shown
in Figure 1(c). It can be seen from Figure 1(b); the lat-
tice strain values are fluctuating due to the increasing Fig. 2. SEM images of (a) pure CdS, (b) 2% Cu:CdS, (c) 4% Cu:CdS
amount of Cu substitution in Cd site. The comparison of and (d) 6% Cu:CdS.

Nanosci. Nanotechnol. Lett. 10, 1–9, 2018 3

Doping Dependent Structural, Optical, Thermal and Catalysis Properties of Synthesized Cadmium Sulfide Nanoparticles Salam et al.
Whereas Figures 2(b)–(d) displaying particles size distri-
bution in the range of 0.05–1.65 m, 0.1–1.25 m and
0.1–1 m respectively. Increasing concentration of Cu
enhances the agglomeration while decreasing the particles
size. This is in agreement with XRD results which reveal
a reduced intensity of Bragg reflections and smaller crys-
tallite size for doped CdS nanoparticles.
Optical properties of pure and Cu doped CdS nanopar-
ticles were probed by UV-Vis spectroscopy (UV-Vis) as
shown in Figure 3(a). Pristine CdS nanoparticles demon-
strate strong absorption in UV region. Doping enhances
the absorption intensity accompanied by a blue shift32
(Fig. 3(a)). This slight shifting in absorption edge is the
consequence of the quantum confinement effect produced
due to increased nucleation rate with doping.33 To mea-
sure the energy band gap from the absorption spectra
for undoped and doped CdS nanoparticles was calculated
using Tauc’s equation as shown in Figure 3(b).
Figure 3(c) shows the effect of lattice strain and crys-
tallite size on band gap of undoped and Cu doped CdS.
The lattice strain (Fig. 3(c)) and crystallite size (Fig. 3(d))
decreased gradually with the addition of Cu and this trend
reverse with higher amount of doping.34 35 Figures 3(c)–(d)
show that the increase in band gap is proportional to dop-
ing concentrations and inversely proportional to crystal-
lite size and strain. As the ionic radius of Cu+2 (0.73 Å)
is smaller than the radius of Cd+2 (0.95 Å). Cu+2 may
occupy Cd+2 sites producing compressive strain that con-
sequently reduces the particle size of Cu doped Cds NPs.
When the size of the CdS nanocrystals becomes smaller
than the exciton radius, a remarkable quantum size effect
leads to a size-dependent increase in the band-gap and a
blue shift in the absorption onset.36
The FTIR spectra of CdS and Cu doped CdS nanoparti-
cles were recorded in the range 400–4000 cm−1 as shown
in Figure 4(a). It can be observed that peaks appear at
same positions for doped and undoped samples reflecting
minimal changes in crystal structures upon doping. Peak
appearing at 670–690 cm−1 is assigned to Cd–S stretch-
ing vibrations37 while 1638 cm−1 is the bending of N–H
originating from the thioacetamide compound.38 The peak
observed at 2361 cm−1 corresponds to S–H stretching
from the hydrogen sulfide gas (H2 S) produced during the
synthesis.39 The peak at 3198 cm−1 is the O–H stretching
that may interact with ethanol through the hydrogen bond-
ing which becomes more prominent in 0.02 % Cu doped
as it has more moisture (8% as described below in DSC-
TGA graph) than other while the other O–H bond attaches
itself on the surface of the CdS shown at 3466 cm−1 .40
The Raman spectra of prepared nanoparticles are shown
in Figure 4(b). The observed peaks for CdS around 295
and 589 cm−1 are attributing to 1st and 2nd order scat-
tering of LO-longitudinal optical phonon mode respec-
tively and well matched with reported.41 The 1st order
peak (295 cm−1  is asymmetric appears like the superpo-
sition of modes (cubic 1LO or hexagonal A1(LO)/E1(LO)
4 Nanosci. Nanotechnol. Lett. 10, 1–9, 2018
peak. The broadening and intensity of the peaks increased
with increasing amount of Cu suggesting compositional
disorder.
Figure 5(a) indicates reducing capacity of NaBH4 with
MB after 40 mins, the addition of undoped CdS with
NaBH4 representing continuous decrease in peak intensity
of MB, Almost 95% reduction of MB was observed in
less than 15 min, indicating the effectiveness of CdS as
nano-catalystn Figure 5(b). 2% Cu doped CdS with NaBH4
reduce the dye within 25 min measured by spectropho-
tometer at the regular interval of approximately 6 min
(Fig. 5(c)). 4% and 6% Cu doped CdS showing succes-
sive decrease in the concentration of MB within 40 min at
the peak intensity of ≈664 nm Figures 5(d)–(e). Catalytic
activity proposing that NaBH4 is not actively participate
for the reduction of methylene blue whereas undoped CdS
representing significant catalytic potential as compare to
Cu doped CdS nanoparticles. The decreased catalytic effi-
ciency of Cu doped CdS nanoparticles might be attributed
due to increased agglomeration between particles. In addi-
tion, the reduction process was found to be accelerated in
the presence of CdS NPs which exhibits rapid decrease
in absorption intensity of MB solution. CdS NPs sup-
ports in electron relay from BH4 (donor) to MB (acceptor
material). BH4 ions are nucleophilic in nature while MB
is electrophilic in nature. Where the CdS accept electron
from BH4 ions and convey them to MB. By the addition of
Cu, the acceptance rate of doped NPs is decreased as Cu
(1.90) is more electronegative relative to Cd (1.69) restrict
the charge mobility of electrons leads to decrease the cat-
alytic activity. The degradation phenomena of MB in the
presence of reducing agent with undoped and doped CdS
NPs are represented in Eq. (5).
(5)
Methylene blue reduced to leucomethylene blue in the
presence of NaBH4 and nano catalyst (undoped and Cu
doped CdS) at room temperature as shown in above
equation.42 43 The presence of NaBH4 in solution increases
the pH of system; which ultimately retard the degradation
of BH− +
4 ions, liberating H ions that reduce MB.
42 43
Thus
the metal nanoparticles are efficient catalysts, suitable for
removing MB from industrial effluents and can be produc-
tively used in waste water treatment.
Salam et al. Doping Dependent Structural, Optical, Thermal and Catalysis Properties of Synthesized Cadmium Sulfide Nanoparticles

Fig. 3. UV visible spectra (a) and Tauc plots (b), graph between bandgap and lattice strain with Cu concentration (c) and crystallite size versus band
gap for pure and doped CdS (d).

The DSC-TGA analysis of prepared undoped and doped
2, 4, 6 % doped CdS were performed in different envi-
ronments (in air, N2 gas) keeping ramp rate of 5  C/min
as shown in Figures 6(a)–(d) and (e)–(h) respectively. The
exothermal peaks are deliberated in up direction. Anal-
ysis of TGA curves for doped and pure CdS in both
environmental conditions show a mass loss (upto 2%–8%,
Table I) starting from about 150  C to 260  C, most
probably due to remove of water of crystallization and
organic material contents used for washing purpose dur-
ing the synthesis process.44 45 The corresponding DTGA
peaks appear after 225  C moreover DSC/DDSC curves
10(a)–(d) also confirm the endothermic nature of transi-
tion in same temperature range. Another common mass
loss (8%–30%, Table I) recognized by TGA/DTGA curves
for all graphs, clearly visible in the temperature range of
about 550  C to 650  C. This endothermic transition as
vet by DSC/DDSC curves are owing to expected subli-
mation of ultra-fine nanoparticles of doped and pure CdS
presence in the samples. These samples treated in N2 envi-
ronment suffer a final and complete mass loss after 900  C
as demonstrated by TGA and DTGA curves; this endother-
mic sublimation of remaining particle with comparatively
big particle size is correspondingly supported by respective
DSC and DDSC plots. Doped and pure CdS nanoparticles
sublime at relatively low temperature in control and inert

Fig. 4. FTIR spectra (a) and Raman spectroscopy of various ratios of Cu in CdS nanoparticles (b).

Nanosci. Nanotechnol. Lett. 10, 1–9, 2018 5

Doping Dependent Structural, Optical, Thermal and Catalysis Properties of Synthesized Cadmium Sulfide Nanoparticles Salam et al.

Fig. 5. (a–e) time dependent UV–vis spectra for the reduction of MB, MB with NaBH4 (a), MB with NaBH4 + CdS (b), MB with NaBH4 + 2% Cu
doped CdS (c), MB with NaBH4 + 4% Cu doped CdS (d) and MB with NaBH4 + 6% Cu doped CdS (e).

environment (N2 Gas) as bulk CdS has higher sublimation
point 980–1000  C.
The DSC-TGA analysis of prepared undoped and doped
2, 4, 6 % doped CdS were performed in different envi-
ronments (in air, N2 gas) keeping ramp rate of 5  C/min
as shown in Figures 6(a)–(d) and (e)–(h) respectively. The
exothermal peaks are deliberated in up direction. Analysis
of TGA curves for doped and pure CdS in both environ-
mental conditions show a mass loss (upto 2%–8%, Table I)
starting from about 150  C to 260  C, most probably due
to remove of water of crystallization and organic mate-
rial contents used for washing purpose during the synthe-
sis process.44 45 The corresponding DTGA peaks appear
after 225  C moreover DSC/DDSC curves 10(a)–(d) also
confirm the endothermic nature of transition in same tem-
perature range. Another common mass loss (8%–30%,
Table I) recognized by TGA/DTGA curves for all graphs,
clearly visible in the temperature range of about 550  C to
650  C. This endothermic transition as vet by DSC/DDSC
curves are owing to expected sublimation of ultra-fine
nanoparticles of doped and pure CdS presence in the sam-
ples. These samples treated in N2 environment suffer a
final and complete mass loss after 900  C as demonstrated
by TGA and DTGA curves; this endothermic sublima-
tion of remaining particle with comparatively big particle
size is correspondingly supported by respective DSC and
DDSC plots. Doped and pure CdS nanoparticles sublime at
relatively low temperature in control and inert environment

6 Nanosci. Nanotechnol. Lett. 10, 1–9, 2018

Salam et al. Doping Dependent Structural, Optical, Thermal and Catalysis Properties of Synthesized Cadmium Sulfide Nanoparticles

Fig. 6. DSC/TGA graphs of CdS (a–b) and Cu doped CdS 0.02, 0.04 and 0.06% (in N2 and air) (c–h) respectively.

(N2 Gas) as bulk CdS has higher sublimation point
980–1000  C.
Doped and undoped CdS demonstrate completely dif-
ferent thermal behavior in air after 650  C around 750  C
to 820  C can be seen in DSC and DDSC curves
Figures 6(e)–(h). This behavior reveals the exothermic
nature of this transition but corresponding TGA and
DTGA plot show very fascinating and curious behavior.
It is noteworthy that the control CdS and 2% Cu doped
CdS suffered a weight loss while 4% and 6% doped

Nanosci. Nanotechnol. Lett. 10, 1–9, 2018 7

Doping Dependent Structural, Optical, Thermal and Catalysis Properties of Synthesized Cadmium Sulfide Nanoparticles Salam et al.

Table I. DSC/TGA result extracted from Figures 11 and 12. CdS samples possess a mass gain due to formation of sul-
Temperature Mass Thermal fates by thermal oxidation. The undoped CdS nanoparti-
range (sample) Environment Transition variation behavior cles are proved to be remarkably competent catalyst by
150 to 260  C Air and N2 Removal of Mass loss Endothermic
reducing methylene blue in less than 15 min, inspite of this
(all samples) gas water of Cu doped (2–6)% CdS nanoparticles degrade MB within
crystalliza- 25–40 min. This novel approach of CdS nanoparticles gain
tion valuable attractions and offer an efficient and economic
550 to 650  C Air and N2 Sublimation of Mass loss Endothermic
(all samples) gas ultrafine
route to environmental protection.
particles
900 to 1000  C Air Sublimation of Mass loss Endothermic Acknowledgment: Authors would like thank to
(all samples) heavy Higher Education Commission-HEC, Pakistan for finan-
particles
750 to 820  C N2 Oxidation Mass loss Exothermic
cial support through Start Research Grant Project
(pure and along with 21/1669/SRGP/R&D/HEC/2017) and CAS-TWAS Presi-
2% decomposi- dent’s Fellowship for international PhD students China.
Cu–CdS) tion
750 to 820  C N2 Oxidation Mass Exothermic
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Received: 28 June 2018. Accepted: 26 October 2018.
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