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Tunable optoelectronic properties of CBD-CdS thin films via bath

temperature alterations

Article  in  Journal of Physics D Applied Physics · March 2016

DOI: 10.1088/0022-3727/49/9/095109

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 Journal of Physics D: Applied Physics

J. Phys. D: Appl. Phys. 49 (2016) 095109 (7pp) doi:10.1088/0022-3727/49/9/095109

Tunable optoelectronic properties of

CBD-CdS thin films via bath temperature
alterations
W G C Kumarage1,2, R P Wijesundera3, V A Seneviratne1,2, C P Jayalath1,2
and B S Dassanayake1,2
1
  Postgraduate Institute of Science, University of Peradeniya, Peradeniya 20400, Sri Lanka
2
  Department of Physics, Faculty of Science, University of Peradeniya, Peradeniya 20400, Sri Lanka
3
  Department of Physics, Faculty of Science, University of Kelaniya, Peradeniya 11600, Sri Lanka

E-mail: buddhid@gmail.com and buddhikad@pdn.ac.lk

Received 13 August 2015, revised 2 December 2015

Accepted for publication 9 December 2015
Published 2 February 2016

Abstract
The tunability of the band-gap value and electron affinity of the n-CdS by adjusting the
growth parameters is very important as it paves the way to improve the efficiency of CdS-
based solar cells by adjusting the band lineup with other p-type semiconductors. In this
respect, polycrystalline n-CdS thin films were grown on FTO glass substrates at different
bath temperatures (40–80 °C) by the chemical bath deposition technique. The structural,
morphological and optoelectronic properties of CdS thin films were studied using x-ray
diffraction, scanning electron microscopy, UV-Vis spectrometry, profilometry, atomic
force microscopy, photoelectrochemical and Mott–Schottky measurements. Absorption
measurements reveal that an energy-gap value of n-CdS can be adjusted from 2.27 to 2.57 eV
and Mott–Schottky measurements indicate that the flat-band potential is increased from  −699
to  −835 V with respect to a Ag/AgCl electrode by decreasing the deposition bath temperature
from 60 to 40 °C. This tunability of optoelectronic properties of n-CdS is very useful for
applications in thin film solar cells and other devices.

Keywords: CdS, CBD, tunability of optoelectronic properties, flat-band potential

(Some figures may appear in colour only in the online journal)

1. Introduction it is a simple and low-cost method to prepare high quality thin

CdS is an important semiconductor compound of the II–VI
group with appreciable physical and electronic properties.
CdS plays a key role in heterojunction solar cells combining
with p-type semiconductor materials of cadmium telluride
(CdTe) or copper indium diselenide/sulphide (CIS) or copper
indium gallium diselenide/sulphide (CIGS) [1, 2]. The phys-
ical properties of CdS are heavily dependent on the fabrication
methodology. Consequently, numerous ways are available for
synthesizing CdS thin films. Fabrication approaches such as
chemical bath deposition (CBD), thermal evaporation, close-
spaced sublimation, chemical pyrolysis deposition, and metal
organic chemical-vapor deposition are some of the commonly
used techniques. Among all these methods, CBD stands out as
films [3–5]. Even though CdS has a direct band-gap value (Eg)
of 2.42 eV at room temperature, the Eg of the CdS thin film
can vary depending on the deposition parameters and on the
nanocrystalline or mixed-phase nature [6]. Consequently, the
growing kinetics as well as the hydrodynamic conditions of
the reaction solution are directly linked with the optoeletronic
properties of the CBD-CdS thin films [7, 8].
It is known that bath temperature has a significant effect
on the morphology and optical properties of the chemi-
cally deposited CdS thin films. The increase in bath temper­
ature improves the surface morphology of the CdS and also
diminishes pinholes on the films [9]. Moreover, the crystal
structure strongly depends on the deposition temperature,
while increasing the deposition temperature promotes the

0022-3727/16/095109+7$33.00 1 © 2016 IOP Publishing Ltd  Printed in the UK

J. Phys. D: Appl. Phys. 49 (2016) 095109
cubic–hexagonal transformation of CdS films and improves
crystallinity [10]. In order to improve the efficiency of the
CdS-based solar cells, it is very important to match the band
lineup of n-CdS with the other p-type semiconductor (CdTe,
CIS or CIGS). In this respect, the tunability of Eg and the elec-
tron affinity of n-CdS is a great advantage for the fabrication
of highly efficient solar cell structures. In this work, CdS thin
films deposited by CBD technique at different bath temper­
atures are discussed in detail through structural, optical, mor-
phological and electrical aspects in order to investigate the
tunability of the optoelectronic properties of the CBD-CdS
with respect to deposition temperature.
2. Experiment
The experimental setup consists of a water beaker, whose
temper­ature was controlled automatically with a hot plate. The
fluorine-doped tin oxide (FTO, ~10 Ω / □, TEC 10, Sigma-
Aldrich, USA) coated conducting glass substrates were posi-
tioned inside a beaker at an angle of 45° to the solution using a
custom-designed Teflon sample holder for the CBD-CdS pro-
cess. Prior to the deposition, the substrates were cleaned with
detergent to wash away any macroscopic impurities on the
surface. Then, the cleaning was continued with diluted HCl
(ACS reagent, 37%, Sigma-Aldrich, USA), de-ionized water
followed by ultrasound sonication and organic solvents. The
organic solvents used for the cleaning process were acetone
(ACS reagent, ⩾99.5% (GC), Sigma-Aldrich, USA), methanol
(ACS reagent, ⩾99.5% (GC), Sigma-Aldrich, USA) and iso-
propanol (ACS reagent, ⩾99.5% (GC), Sigma-Aldrich, USA).
The substrates were cleaned by dipping them in the above sol-
vents at 70 °C in each, followed by carefully drying them with
nitrogen gas.
All the films were deposited in the reaction beaker con-
taining aqueous solutions of 20 ml of 0.1 M cadmium sulfate
(3CdSO4.8H2O, 99%, Breckland Scientific, UK), 20 ml of
0.2 M thiourea (CS(NH2)2, 99%, MRS Scientific Inc., UK)
which were titrated throughout the experiment, and 1.1 ml of
ammonia solution (NH3, 35% w/w, Surechem Products Ltd,
England) and de-ionized water was used to make the final
volume 140 ml. The deposition was carried out at five dif-
ferent bath temperatures; 40, 50, 60, 70 and 80 °C. The reac-
tion solution was stirred at 200 rev min−1 in order to promote
a heterogeneous growth of CdS on the substrates. Pale yellow
transparent CdS films were obtained by maintaining the above
physical and chemical parameters for one hour in each depo-
sition. Then, the fabricated films were rinsed with de-ionized
water followed by ultrasound sonication to remove loosely-
adherent CdS particles before drying them with nitrogen
gas. The CdS was removed from one side of the substrate
by chemical etching using diluted HCl for optical and elec-
trical characterization. Later, films were successively washed
with de-ionized water and dried with nitrogen gas before
annealing at 200 °C for one hour in a tube furnace (Büchi
To-51, Switzerland).
The x-ray diffraction (XRD) analysis was carried out in the
2θ range of 10–80° with step sizes of 0.5° by using Siemens
2
W G C Kumarage et al
Figure 1.  X-ray diffraction pattern obtained for the CBD-CdS
samples fabricated at 80 °C for 1 h with H-hexagonal and C-cubic
structure.
x-ray diffractometer D 5000, where a Cu Kα1 radiation wave-
length of 1.540 56 Å was used to study the crystal structure of
the fabricated CdS samples. An XP-1 Profilometer (Ambios
Technology) was used to determine the thickness of the
fabricated CdS thin films. Optical transmission and absorp-
tion measurements were conducted at room temperature
under normal incidence in the wavelength range from 300
to 800 nm using a UV-1800 Shimadzu double beam UV-Vis
spectrophotometer. The surface roughness was investigated
using a Veeco Atomic Force Microscope (AFM, model 840-
017-900R) while the scanning electron microscopy (SEM)
measurements of the fabricated CdS surfaces were obtained
using an FEI Helios Nanolab 600 SEM and Zeiss EVO|LS15.
Photocurrent–voltage measurements were obtained in a pho-
toelectrochemical (PEC Cell L01) containing 0.1 M Na2S2O3
(97%, Baxter Smith Labs, USA). The effective area of the
CdS/electrolyte was 0.25 cm2 and the junction was illumi-
nated under an AM 1.5 simulated solar light irradiation using
a 150 W short-arc xenon lamp. The Mott–Schottky measure-
ments were carried out in the same PEC at 1000 Hz within the
potential range from  +0.8 to  −0.8 V scanning in the cathodic
direction. For I–V and Mott–Schottky measurements, Pt and
Ag/AgCl electrodes were used as counter and reference elec-
trodes, respectively.
3.  Results and discussion
3.1.  Structural characterization
Figure 1 shows the XRD spectrum of the CdS film grown at the
bath temperature of 80 °C. Six peaks appear in the XRD spec-
trum indicating the reflections from different planes. The peaks
of 2θ values at 26.5°, 30.8° and 43.9° are due to the reflections
from the cubic planes of CdS (1 1 1), (2 0 0) and (2 2 0) while
23.4°, 25.9° and 25.9° are due to the reflection peaks corresp­
onding to hexagonal CdS (1 0 0), (0 0 2) and (1 0 2). These
results reveal that CBD-CdS thin films are polycrystalline
J. Phys. D: Appl. Phys. 49 (2016) 095109
Figure 2.  The plot of the transmittance versus wavelength of
CBD-CdS on FTO at different bath temperatures.
Figure 3.  The plot of (αhυ)2 versus photon energy for the
CBD-CdS on FTO at different bath temperatures.
[11, 12] and consist of hexagonal (wurtzite) and cubic (zinc-
blende) grains in the same CdS thin films.
3.2.  Optical measurements
Figure 2 shows the transmittance measurements of CBD-CdS
on FTO glass at different bath temperatures. The transmit-
tance measurements reveal that the films fabricated at 40 °C
produce the highest transmittance (>85%) as shown in
figure  2. The results indicate that the higher transmittance
values at lower temperatures are due to lower sample thick-
nesses. Furthermore, the transmittance edges at higher bath
temperatures were found to be redshifted compared to the
films fabricated at low temperatures, suggesting that the band
gaps of the deposited films are subjected to alteration, with
respect to the variation of bath temperature. The band-gap
values of CdS thin films were obtained by extrapolating the
linear (αhυ)2 versus hυ plots derived from the equation (2),
to (αhυ)2  =  0 [13, 14] as shown in figure 3, where the optical
absorption coefficient (α) was calculated by using Lambert’s
law (1) [15],
3
W G C Kumarage et al
Figure 4.  The optical band-gap variation (Eg) of the CBD-CdS
deposited on FTO glass substrates at different bath temperatures. The
inset shows the variation of Eg with respect to the sample thickness;
A-45 nm at 40 °C, B-81.6 nm at 40 °C and C-77 nm at 80 °C.
⎛I ⎞
αd = ln⎜ 0 ⎟ = 2.303 Abs
⎝ IT ⎠
(1)
where I0 and IT are intensities of incidence and transmittance
radiation respectively, Abs is the optical absorbance, α is the
absorbance coefficient and d is the thickness of the sample.
The optical band-gap energy (Eg) was derived using the Stern
relation (2) [16];
n
(hν − Eg ) 2
(2)
α=A
hν
where α is the optical absorption coefficient, A is a constant,
h is Plank’s constant and n is equal to 1 for direct band-gap
material such as CdS. CdS thin films grown at 40 °C have
the highest Eg value of 2.57 eV while the lowest Eg value
of 2.27 eV exhibits for the CdS thin films grown at 60 °C
(figure 4). The results reveal that the Eg value of the CBD-CdS
can be manipulated between 2.27 and 2.57 eV by adjusting
the deposition bath temperature. This variation of the Eg
values can be discussed more comprehensively with the aid
of deposition chemistry of CdS thin films. The formation of
CdS can be described through the following chemical reac-
tions [17–20];
The first step is the hydrolysis of ammonia in water which
gives out OH−,
NH3 +  H2O  ↔  NH+
(i) 4 +  OH
−
Then CdSO4 releases Cd2+ ions to the solution;
CdSO4 →  Cd2+ +  SO24 −
(ii)
The above reaction (equation (i)) forms a basic medium of pH
10–11. Thiourea, which was titrated throughout in this experi-
ment hydrolyzes in an alkaline solution to give S2−.
CS(NH2)2 +  2OH− ↔  S2− +  CN2H2 +  2H2O
(iii)
J. Phys. D: Appl. Phys. 49 (2016) 095109
At low temperature;
Cd2+ +  S2− →  CdS ↓
(iv)
At higher temperature; the cadmium ions react in the basic
medium as below,
Cd2+ +  2OH− ↔  Cd(OH)2 ↓
(v)
nCd(OH)2 +  nS−2 ↔ (CdS) n↓  + H2O
(vi)
Cd(OH)2 +  4NH2OH  ↔  [Cd(NH3)4]2+  + H2O
(vii)
Finally, the sulfide ions and [Cd(NH3)4]2+ react to form CdS
as below to be deposited as thin films.
[Cd(NH3)4] n2++ S2−  ↔  (CdS) n↓  + 4NH3
(viii)
When the CdS is deposited according to the mechanism in
equation (iv), it is called an ion-by-ion deposition mech­anism,
whereas the CdS deposition at equations  (vi) and (viii) is
called a cluster-by-cluster deposition mechanism. The ion-
by-ion mechanism is less thermally activated compared to
the cluster-by-cluster mechanism. Cd(OH)2 is an important
reaction intermediate in the cluster-by-cluster method. If the
[Cd(NH3)4]2+ complex concentration is not high enough to
prevent the formation of Cd(OH)2, then a relatively small
amount of Cd(OH)2 may be formed as colloids. CdS is then
formed by the reaction of slowly generated S2− ion with
Cd(OH)2 as in equation (vi).
Since the Gibbs free energy (∆G) of the formation of CdS is
more negative than that of Cd(OH)2, (ln Ksp = − ∆G RT , where
R is the gas constant and T is the absolute temper­ature), the
hydroxide cluster can act as a catalyst for thiourea decomposi-
tion. Consequently, sulphide formation will occur favorably at
the surface of the hydroxide rather than nucleating separately
in the solution [18].
The high Eg value at low bath temperatures (below 60 °C)
can potentially be due to the reduction of the dispersion of
ions in the solution due to thermal movement [10] which hin-
ders the rate of the ion-by-ion deposition process at low bath
temperatures while higher bath temperatures (above 60 °C)
predominantly produce CdS by the cluster-by-cluster
mechanism.
The ion-by-ion mechanism is less thermally activated with
respect to the cluster-by-cluster mechanism. Films fabricated
by the cluster-by-cluster mechanism have a higher film thick-
ness due to cluster-wise aggregation with respect to films fab-
ricated under the ion-by-ion mechanism. Since, the deposition
kinetics are governed by the mobility [18] of the ions in the
solution, the film thickness increases with increasing temper­
ature in the ion-by-ion region (up to 60 °C) as well as in the
cluster-by-cluster region, (beyond 60 °C) [14] as can be seen in
figure 5 and table 1.
Since the variation of the Eg values can also be attributed to
the thickness of the samples, films of similar thicknesses were
deposited at 40 and 80 °C at which the ion-by-ion and cluster-
by-cluster mechanisms govern the depositions, respectively.
The inset of figure 4 shows the variation of Eg with respect to
the sample thickness; A-45 nm at 40 °C, B-81.6 nm at 40 °C
4
W G C Kumarage et al
Figure 5.  CBD-CdS film thickness variation with respect to
deposition bath temperature.
Table 1.  Bath-temperature-dependent thickness; roughness of the
CBD-CdS on FTO
Bath temperature (°C) Thickness (nm) Roughness (nm)
40 81.6 —
40 43.0 21.5
50 59.2 14.1
60 65.4 15.2
70 67.8 18.2
80 77.0 25.9
and C-77 nm at 80 °C. This result indicates, though the film
thicknesses are nearly the same (sample B and C), a consider-
able difference in the Eg value prevails. The Eg value variation
is an important aspect in the process of manufacturing CdS-
based photovoltaic (PV) devices, since the Eg value governs
the photoactive properties of PV materials.
3.3.  Morphology characterization
The measured surface roughness values are tabulated in table 1.
According to the results, roughness increases with increasing
bath temperature beyond 50 °C. Even though increasing thick-
ness contributes to higher roughness values [21, 22], in films
fabricated at a deposition bath of 40 °C which produced the
thinnest samples (43 nm), the roughness value was found to
be exceptionally high compared to the others. Considering the
thickness and roughness values recorded at 40 and 80 °C, the
unusually high roughness values seen at 40 °C can be influ-
enced by the difference in the deposition mechanisms.
The SEM images in figure 6 support the existence of the
two deposition mechanisms and also provide solid agreement
for Eg variation as well as surface roughness with respect
to bath temperature. Large cluster sizes were seen (figures
6(b)–(d)) for the CdS films fabricated at a bath temperature of
50–70 °C. This is in agreement with Eg (figure 4) where low
optical band-gap values were observed. The films fabricated
at 40 and 80 °C have relatively low cluster sizes with respect
J. Phys. D: Appl. Phys. 49 (2016) 095109 W G C Kumarage et al

Figure 6.  SEM images of CBD-CdS deposited at (a) 40 °C, (b) 50 °C, (c) 60 °C, (d) 70 °C and (e) 80 °C of bath temperature under 100 K
magnification. The scale in samples (a), (c) and (e) is 500 nm while that of (b) and (d) is 200 nm.

Table 2.  Bath-temperature- and thickness-dependent optical-

electrical results of the CBD-CdS on FTO
Bath
temperature Thickness Eg Voc Isc Flat-band
(°C) (nm) (eV) (mV) (μA) potential (mV)
40 81.5 2.43 228 1.50 −835
40 43.0 2.55 198 2.23 −830
50 59.2 2.36 180 1.20 −752
60 65.4 2.27 141 0.54 −699
70 67.8 2.25 208 1.88 −753
80 77.0 2.34 318 1.95 −792

trend of Voc variation with the bath temperature in figure 7(a)

Figure 7.  Voc and Isc variation with respect to the deposition bath
temperature and Voc and Isc variation with respect to the different
thickness; A-45 nm at 40 °C, B-81.6 nm at 40 °C and C-77 nm
at 80 °C of the CBD-CdS on FTO.
to the samples fabricated at other bath temperatures. In addi-
tion, the SEM images of the samples fabricated at 50–70 °C
provide evidence for CdS particle aggregation as can be seen
in figures  6(b)–(d), which can potentially be due to the co-
existence of both the deposition mechanisms; ion-by-ion and
cluster-by-cluster. Cluster size variation strongly correlates
with the effective area of the films and hence the electrical
properties of the thin film. Therefore, it is very important to
study the correlation of electrical properties of deposited CdS
with deposition bath temperature.
3.4.  Photoactive characterization
Figure 7 shows the Voc and Isc variations with different growth
conditions. The results of PEC characterization is shown in
table 2. The lowest Voc value (figure 7(a)) was found for the films
deposited at a bath temperature of 60 °C, while Voc was found
to increase with a bath temperature above and below 60 °C.
The trend of the Isc value variation with respect to deposition
bath temperature follows a similar trend to Voc. The correla-
tion between the cluster sizes and Isc can be clearly under-
stood by figures 6 and 7(a). Films fabricated at 40 and 80 °C
show smaller cluster sizes and hence larger surface area. Since
the effective area of the fabricated film affects the electrical
properties, higher Isc values at 40 and 80 °C with respect to
the films fabricated at 60 °C can be due to the effects of the
enhanced effective surface area.
The variation of Voc can be related to the existence of
different electron affinity levels in the semiconductor. The
could be due the alteration of electron affinity levels with the
increasing bath temperature. Consequently, the Voc value vari-
ation trend with bath temperature is also in agreement with
the Eg value variation with films grown at higher and lower
temperatures, which have high Eg values compared to films
grown at 60 °C, showing greater Voc values.
A proper comparison of electrical properties can be car-
ried out for films of similar thicknesses since the electrical
properties of the fabricated films are dependent on the diffu-
sion length. Figure 7(b) illustrates the variation of Voc and Isc
values for samples A, B and C. The comparison between sam-
ples B and C indicates that the films fabricated at 80 °C have
high Voc and Isc values compared to films fabricated at 40 °C,
both of which are of almost similar thicknesses. It can be
concluded that this trend might be due to the crystal struc-
ture variation from cubic to hexagonal with increasing bath
temper­ature [19, 23, 24].
3.5. Mott–Schottky analysis
The carrier concentration (ND) and the flat-band potential
(Vfb) were obtained from the slope and the x-axis intercept of
the linear fit of the Mott–Schottky equation (3) [25].
1 2 ⎛ kT ⎞
⎜V − Vfb − ⎟
εεoND ⎝ e ⎠
=
(3)
2
C
where e is the electron charge, ɛ is the dielectric constant,
ɛo is the permittivity in vacuum. The Mott–Schottky plots
confirmed the n-type behavior of the fabricated CdS thin
films. The flat-band potential variation (table 2) of the fab-
ricated films with respect to the bath temperature obtained
from the x-axis intercepts of the Mott–Schottky plot is
shown in figure  8. The flat-band potential was found to

5
J. Phys. D: Appl. Phys. 49 (2016) 095109
Figure 8.  (a) Flat-band potential against Ag/AgCl reference with 0.1 M Na2S2O3 electrolyte at room temperature at 1000 Hz with respect to
the CBD-CdS deposition bath temperature, (b) the energy-band diagram of the CdS/electrolyte system.
be at its lowest at 60 °C, while it increased when devi-
ating away from 60 °C. The highest flat-band potential was
observed for the film fabricated at the bath temperature
of 40 °C which has the lowest cluster size as well as the
lowest film thickness.
When the flat-band potential is high, the electric field
strength in the space charge region of the semiconductor is
expected to be high. This can be clearly seen in figures 7(a)
and 8(a) where both Isc and the flat-band potential have similar
trends with respect to the deposition bath temperature. Even
though films fabricated at 40 °C have the higher flat-band
potential, the highest product of Voc and Isc is shown by the
films fabricated at a bath temperature of 80 °C with a carrier
concentration in the order of 1016 cm−3.
Furthermore, it can be clearly understood from figures 8(a)
and (b) that the possibility of altering the conduction band
position and hence the flat-band potential of the CdS thin films
can be manipulated by altering the bath temperature, which
results in a shift of electron affinity of the CdS. The possi-
bility of altering the electron affinity of the semiconductor
material is of great importance in the energy band lineup in
p-n junction manufacturing since the potential discontinui-
ties (spikes) in the depletion region can be effectively over-
come by engineering of the electron affinity. The tunability of
electron affinity and energy-gap values of n-CdS by adjusting
the growth condition (bath temperature) will pave the way to
use them in efficient low-cost solar-energy-converting device
applications.
4. Conclusions
Polycrystalline CdS was successfully deposited on FTO glass
substrate by the CBD technique. A variation of the energy-gap
values from 2.27 to 2.57 eV and the flat-band potential value
from  −699 to  −835 V with respect to Ag/AgCl of n-CdS
thin films can be adjusted by changing the deposition bath
6
W G C Kumarage et al
temper­ature from 60 to 40 °C, respectively. However, the best
power was generated in PECs when the films were grown at
80 °C. The carrier concentration of the CdS grown at 80 °C
is in the order of 1016 cm−3. In conclusion, our study reveals
that optoelectronic properties of CBD n-CdS thin films can be
effectively altered by varying the deposition bath temperature
which results in tunable flat-band potential (electron affinity),
Eg, Voc and Isc values, altogether suggesting its suitability for
fabricating low-cost highly efficient PV devices.
Acknowledgments
Financial assistance from the National Science Foundation
(RG/12/BS/03) of Sri Lanka, the support of the Higher Degree
Committee of the University of Peradeniya (AC/URF/2014/03)
and Professor S Sivananthanthan of the University of Illinois,
Chicago, USA are gratefully acknowledged. Professor M A K
L Dissanayake of the National Institute of Fundamental Stud-
ies (NIFS), Sri Lanka and Dr M Nandasiri of the the Western
Michigan University, USA are acknowledged for their valu-
able suggestions and support.
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