J Mater Sci: Mater Electron
DOI 10.1007/s10854-015-3812-7
Influence of molar concentration on triethanolamine added
copper doped tin sulfide (CuxSn12xSy) nano thin films grown
by SILAR method
P. Mani1 K. Manikandan2 J. Joseph Prince1
Received: 24 June 2015 / Accepted: 29 September 2015
Springer Science+Business Media New York 2015
Abstract Thin films of copper doped tin sulphide (Cux
Sn1-xSy) with the complexing agent TEA are deposited on
glass substrates by SILAR technique for various molar con-
centrations (0.010.10 M) at room temperature. The struc-
tural, surface morphology, topography and optical properties
of the films are studied for the varying molar concentrations.
XRD studies reveal the amorphous nature of TEA added Cu
doped SnS films. The surface morphology was observed by
SEM images. Surface topography of the film is studied by
AFM. 2D-AFM images reveals that the grain size, surface
roughness and height decreases for the increasing concentra-
tion. FTIR analysis shows the molecular vibrations. The
optical properties of the deposited films are investigated by
measuring the optical absorbance of the films in a range of
300800 nm with a UVVis spectrophotometer. Other prop-
erties such as transmittance, refractive index, and energy gap
are calculated. Based on the above characterisations, synthe-
sized TEA added copper doped tin sulphide thin film may be
used for small band-gap semiconductors, non-linear materials
and photovoltaic cell materials.
1 Introduction
Previously, CTS thin films are synthesized by various
methods such as spray-pyrolysis [1, 2], CBD [38], co-
evaporation [9], aqueous solutions method [10] magnetron
& P. Mani
maniprahaspathy@gmail.com
1
Department of Physics, Anna University Chennai, BIT
Campus, Tiruchirappalli, India
2
Department of Physics, Bharathidasan University Constituent
Model Womens College, Veppur 621717, India
sputtering [11], electro deposition [12] and successive ionic
layer adsorption and reaction (SILAR) [1316, 18, 22].
SILAR technique is simple, cost effective, able to coat in
large area, used to prepare metal chalcogenide films, less
time consuming and making the process feasible for com-
mercial application. The wastage of material is avoided as no
precipitate is formed during this process. The film properties
are well comparable with the properties obtained by other
chemical methods [17]. This shows the wide applicability of
SILAR method for the deposition of various metal chalco-
genides. It is possible to produce uniform and well adherent
thin films. Ternary compound TEA added CTS are more
promising opto-electronics materials, because their band gap
energy matches the solar spectrum, optimum optical
absorption, their abundance and competitive cost. Further, it
contained more abundant and cheaper elements that are
environmentally safe to handle [9]. Till date, few works have
been reported on CTS [15, 11, 13, 14, 18]. This work is an
attempt to prepare CTS with TEA by varying molar con-
centration. Sn(TEA) complex reduces the release of Sn2?
ions into the solution and the presence of TEA promotes the
deposition of uniform and better quality films [12].
2 Experimental techniques
2.1 Preparation of CuxSn12xSy thin film
with complexing agent
Microscopic glass slides of 26 mm 9 76 mm 9 1 mm
dimension are used as substrates. The substrates are ultra-
sonically cleaned with nitric acid and ethanol solution, then
washed in detergent and purified with deionised water
(conductivity * 1 lX-1 cm-1) for 30 min and then dried
in a clean air atmosphere. TEA added CuxSn1-xSy thin
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 J Mater Sci: Mater Electron

films are prepared by the SILAR technique at room tem- and rinsing operations facilitates heterogeneous reaction
perature. In this method, concentration, pH, temperature of between the solid phase and the solvated ions in the solu-
precursor solutions and the time duration for the dipping tion (Fig. 1). Thus a SILAR cycle consists of these six
process are the key factors which dictate the adsorption and operations and the same is repeated for 30 SILAR cycles
nucleation of the reacting substances and thus effective for all the ten different (0.010.10 M) molar concentra-
coating on the substrate. Hence, by keeping all these tions. Figure 2 shows the schematic representation of
parameters at the optimum level, the films are coated. The SILAR deposition of TEA added CuxSn1-xSy thin film.
deposition process is carried out at room temperature
(30 C) and the reacting solutions are kept undisturbed and
the deposition process is carried out by the following six 3 Results and discussion
steps per dipping cycle (Table 1).
In this present research work, TEA added CuxSn1-xSy thin
1. A pre-cleaned glass substrate is initially immersed in
films are deposited on glass substrates by SILAR technique
the cationic precursor TEA added tin nitrate
at room temperature using copper nitrate (CuNO3) and tin
(Sn(NO3)27H2O) solution for about 35 s.
nitrate (Sn(NO3)2 as cationic ion source and sodium sulfide
2. Then rinsed in deionised water for 35 s to remove the
(Na2S) as anionic source is reported. The deposited films
loosely bound or unadsorbed tin Sn2? ions.
are characterised using X-Ray Diffractometer (XRD),
3. The cationic precursor adsorbed substrate is subse-
Fourier Transform Infra Red spectroscopy (FTIR), Scan-
quently immersed in the anionic precursor solution
ning Electron Microscopy (SEM), Atomic Force Micro-
sodium sulfide (Na2S) for about 35 s, where the S2-
scopy (AFM) and UVvisible Spectrometer techniques.
ions are reacted with the pre-adsorbed Sn2? ions and a
The work also explores the influence of dopant (Cu2?)
layer of SnS thin film is formed.
molar composition on structural, vibrational, surface mor-
4. It is rinsed with deionised water for 35 s to remove the
phology, topography and optical studies of the TEA added
unbound ions.
CuxSn1-xSy thin films.
5. The pure SnS deposited film is dipped again in cationic
precursor solution of TEA added copper nitrate
3.1 XRD analysis
(Cu(NO3)27H2O) for about 35 s to add the Cu2? ions
on the SnS thin films as dopant and
The X-ray diffraction (XRD) pattern obtained for Cux
6. Finally the substrate is rinsed in deionised water for
Sn1-xSy thin films (Cu) x = 0.04, 0.06 and 0.09. Figure 3
35 s to remove the loosely bound or un adsorbed
exhibit the amorphous nature of Cu doped SnS thin film. The
(Cu2?) ions.
diffraction hump is observed at the 2h value of 27.06 for the
The adsorbed Cu2? ions and Sn2? are reacted with the different molar compositions of Cu doped SnS thin films
S2- ions to form TEA added CuxSn1-xSy compounds as an (Cu) x = 0.04, 0.06 and 0.09 at room temperature. Only one
ultra thin coating on the substrate. Each immersion stage is diffraction peak is observed for (Cu) x = 0.09 M in appre-
consisted with a rinsing step. These alternative immersions ciable height on the hump and the other minor peaks reveal

Table 1 Deposition parameters in SILAR controller settings

Source of material Tin nitrate Distilled water Sodium sulfide Distilled water Copper nitrate Distilled water

Volume (ml) 100 100 100 100 100 100

Concentration (M) 0.100.01 0.1 0.010.10
Temperature (C) 30 30 30 30 30 30
Complexing agent TEA (4 ml) NIL NIL NIL TEA (4 ml) NIL
Start position 0 0 0 0 0 0
Dip length (mm) 75 75 75 75 75 75
Dip speed (mm/s) 5 5 5 5 5 5
Retrieval speed (mm/s) 4 4 4 4 4 4
Dip duration (s) 35 35 35 35 35 35
Ex. dip duration (s) 4 4 4 4 4 4
No of cycles 30 30 30 30 30 30
Soluble in Dist. water Dist. water Dist. water
Source of ions Sn2? S2- Cu2?

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J Mater Sci: Mater Electron
Fig. 1 Schematic
representation of SILAR
method
Fig. 2 Schematic
representation of SILAR
deposition of CuxSn1-xSy thin
film
the amorphous nature. CuS and SnS phases are easy to
identify in XRD. When it is present in a phase mixture with
CuxSn1-xSy its diffraction peaks are not distinct. It may have
clear distinct peaks on annealing [1, 2, 13].
3.2 SEM analysis
The SEM analysis are carried out for the different compo-
sitions of Cu0.01MSn0.09MS0.10M, Cu0.02MSn0.08MS0.10M,
Cu0.03MSn0.07MS0.10M, Cu0.04MSn0.06MS0.10M, Cu0.05M-
Sn0.05MS0.10M, Cu0.06MSn0.04MS0.10M and Cu0.09MSn0.01M
S0.10M thin films. The SEM micrograph of
Cu0.01MSn0.09MS0.10M film in 50, 10 and 5 lm is given in
Fig. 4. The SEM micrograph of the Cu0.02MSn0.08MS0.10M
film of 200 and 5 lm is given in Fig. 5. Both of them are
exposing the uniform surface with the formation more
irregular structures in the higher magnification.
The SEM micrograph of Cu0.03MSn0.07MS0.10M film in
200, 50, 20, 10, 5 and 2 lm magnifications is given in
Fig. 6. It exposes the even coating on the substrate. To
know further about the surface, it is magnified to closer
area from 200, 50, 20, 10, 5 and 2 lm. It shows the
improved evenness in the surface. For 200 lm, the surface
is uniform with some different drawing shaped spot. For
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Fig. 3 XRD patterns of CuxSn1-xSy thin films for different molor
composition
50 lm, it is like an aerial view of a sea shore. For 20 lm,
some pores are present. For the closer magnifications (10, 5
and 2 lm), it is clearly formation of spherical particles are
observed and they are evenly distributed over the coating
area. The surface is uniform with few crystals.
The SEM micrograph of Cu0.04MSn0.06MS0.10M thin film
in 200, 50, 20, 5, 2 and 1 lm magnifications is given in
Fig. 7. The coating in 200 lm magnification reveals the
smoothness of the film without pores and cracks. There is
no crystal formation on the surface. The coating in 50 lm
magnification reveals the presence of some pores with
uniform coating. The coating in 20 lm magnification
Fig. 4 SEM images of the Cu0.01MSn0.09MS0.10M film in various magnifications
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J Mater Sci: Mater Electron
confirms the uniform coating. For the closer magnifications
(5, 2 and 1 lm), irregular shape of spherical particles of
few nano meters are observed clearly and they are evenly
distributed over the coating area. These micrographs shows
that the surface is crowded with the flower like structure
which is like the top view of mushroom and the structures
are evenly distributed over the entire surface.
The SEM micrograph of Cu0.05MSn0.05MS0.10M thin film
in 200, 50, 20, 10, 5 and 2 lm magnifications is given in
Fig. 8. Even though the surface is smooth, various domains
are segregated by road like structures in 200 lm magnifi-
cation. There is a bright spot and a huge irregular sized
cluster in 50 lm. It may due to the equal (0.05 M) molar
concentration of cations Cu and Sn. In equal concentration
cations are not mixed properly. So that road like structures,
clusters, pin holes irregular sized particles and irregular
positions are formed. Few of bulk particles are spread over
the surface in 10, 5 and 2 lm magnifications.
The SEM micrograph of Cu0.06MSn0.04MS0.10M thin film
in 200, 50, 20, 5, 2 and 1 lm magnifications is given in
Fig. 9. The SEM micrograph of Cu0.06MSn0.04MS0.10M thin
film shows the uniform and fine surface for 200 and 50 lm.
For 20 lm surface is like neat mat finish. For 5, 2 and 1 lm
the surface is looking like an emery sheet. Here the parti-
cles of various size and shape are uniformly distributed
over the surface. For the increasing composition of copper,
the surface is very smooth with regular shaped particles
comparatively. The well grown spherical particles are
observed approximately in the size of 30 nm.
The SEM micrograph of Cu0.09MSn0.01MS0.10M thin film
in 50, 20, 5, 2, 1 lm and 500 nm magnifications is given in
Fig. 10. The material is coated uniformly over the surface
with cracks and domain groups. An island like structure is
viewed in 20 lm. Newly germinated sprout like structure is
J Mater Sci: Mater Electron

Fig. 5 SEM images of the Cu0.02MSn0.08MS0.10M thin film in various magnifications

Fig. 6 SEM image of the Cu0.03MSn0.07MS0.10M thin film in various Magnifications

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 J Mater Sci: Mater Electron

Fig. 7 SEM image of the Cu0.04MSn0.06MS0.10M thin film in various magnifications

Fig. 8 SEM image of the Cu0.05MSn0.05MS0.10M thin film in various magnifications

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J Mater Sci: Mater Electron

Fig. 9 SEM image of the Cu0.06MSn0.04MS0.10M thin film in various magnifications

Fig. 10 SEM image of Cu0.09MSn0.01MS0.10M thin film in various Magnifications

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Fig. 11 3D AFM images of
TEA added CuxSn1-xSy thin
films of various concentrations
observed in 5 lm magnification. The particles on the uni-
form coating are like tiny flakes in 2 lm. The morpho-
logical property of the thin film surface indicates that the
formation of nano particles are evenly sized and uniformly
distributed over the entire surface. The average sizes of the
particles are found to be in the range below 15 nm.
Micrograph in 5 and 2 lm magnifications disclose the
formation of nano crystals in surface. It is like the stars in
night sky. The particles appears to be the broken shining
glass pieces in 1 lm and 500 nm.
For the SEM micrographs Cu0.01MSn0.09MS0.10M and
Cu0.02MSn0.08MS0.10M, surface is uniform with the formation
more irregular structures. The following different
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composition of SEM micrographs of Cu0.03MSn0.07MS0.10M,
Cu0.04MSn0.06MS0.10M, Cu0.06MSn0.04M S0.10M and Cu0.09M
Sn0.01MS0.10M are showing smooth surface with well grown
particles. For the lower and higher copper composition and
equal concentration of cations Cu and Sn (Cu0.05MSn0.05M
S0.10M) the comparative variation in morphology is observed.
The particles improve in its size regularly for the high com-
position of copper for the respective higher magnification.
3.3 AFM analysis
The surface topography analysis of the thin films is
examined by AFM studies for the different compositions of
J Mater Sci: Mater Electron
Fig. 12 2D AFM image of
Cu0.03MSn0.07MS0.10M thin film
Fig. 13 2D AFM image of
Cu0.04MSn0.06MS0.10M thin film
Cu0.01MSn0.09MS0.10M, Cu0.02MSn0.08MS0.10M, Cu0.03M
Sn0.07MS0.10M, Cu0.04MSn0.06MS0.10M, Cu0.05MSn0.05M
S0.10M, Cu0.06MSn0.04MS0.10M and Cu0.09MSn0.01MS0.10M
thin films. Figure 11 shows 3D AFM images of CuSnS thin
film of various concentrations. All the 3D AFM images are
recorded in 3 lm area. For 0.03 and 0.04 M the particles
are mostly in equal size. The surface is smooth. But for
0.05 M, the particles are not in equal size. The surface
height varies and the surface roughness differs. So this film
is not smooth in equal concentration of the cations Cu and
Sn. For 0.06 and 0.09 M the particles are grown well. Both
of them are more or less having equal surface roughness
and height. Coating of these five films are coincides with
the results of SEM micrograph.
2D AFM images are shown in the Figs. 12, 13, 14, 15
and 16. In the minimum copper and maximum tin con-
centration (x = 0.03 M and 0.04 M) of CuxSn1-xSy thin
films of 2D-AFM images reveals that the grain size, surface
roughness and height decrease for the increasing concen-
tration. For the equal concentration of cations Cu and Sn,
the grain size, surface roughness and surface height
increase. In the maximum copper and minimum tin
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Fig. 14 2D AFM image of
Cu0.05MSn0.05MS0.10M thin film
Fig. 15 2D AFM image of
Cu0.06MSn0.04MS0.10M thin film
concentration (x = 0.06 M) of CuxSn1-xSy thin films of
2D-AFM images reveals that the grain size, surface
roughness and surface height increase comparatively with
equal concentration of cations Cu and Sn. For x = 0.09 M
of CuxSn1-xSy thin films, the grain size, surface roughness
and surface height decrease. These values are tabulated in
the Table 2.
3.4 FTIR analysis
The FTIR spectrum of Cu doped SnS composite thin film
for the concentration 0.010.05 M is shown in Fig. 17.
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J Mater Sci: Mater Electron
FTIR measurements have been made in the wave number
range 4004000 cm-1. The absorption bands observed at
569.00 and 686.66 cm-1 are possibly due to the stretching
vibration of SnS. The presence of water is also confirmed
by its bending vibration observed at 1800 cm-1. Medium
strong band position at 18001000 cm-1 is possibly due to
stretching vibrations of sulphide group. The absorption
peak appears around 1925 and 2081.25 cm-1 may be due
to C=C vibration suggesting the organic contamination
from the source materials [16, 1921]. The weak absorp-
tion band at 3495, 3521 and 2911 cm-1 is assigned to OH
stretching vibration of the adsorbed water in the sample.
J Mater Sci: Mater Electron

Fig. 16 2D AFM image of

Cu0.09MSn0.01MS0.10M thin film

Table 2 Surface properties of grain size, surface roughness and surface height
Molar concentration of Grain Surface Surface
TEA added CuxSn1-xSy size (nm) roughness (nm) height (nm)

Cu0.03MSn0.07MS0.10M 148.5 51.1545 179.4715

Cu0.04MSn0.06MS0.10M 132 14.812 40.7185
Cu0.05MSn0.05MS0.10M 136.5 53.4465 117.2975
Cu0.06MSn0.04MS0.10M 176.5 32.995 72.1055
Cu0.09MSn0.01MS0.10M 103 20.638 76.007

Fig. 17 FTIR spectrum for 0.010.05 M concentrations

Figure 18 depicts the FTIR values of CuSnS thin film
with TEA for 0.060.10 M. The absorption bands
observed at 620 and 725 cm-1 are possibly due to the
stretching vibration of SnS. The presence of water is
Fig. 18 FTIR spectrums for 0.060.10 M concentrations
also confirmed by its bending vibration observed at
19802180 cm-1. Medium strong band position at
18001000 cm-1 is possibly due to stretching vibrations

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 J Mater Sci: Mater Electron

Fig. 19 Absorbance versus wavelength for CuxSn1-xSy thin films for 0.010.05 and 0.060.10 M

Fig. 20 Transmittance versus wavelength for CuxSn1-xSy thin films for 0.010.05 and 0.060.10 M

of sulphide group. The weak absorption band at 3520,
3280 and 2825 cm-1 is assigned to OH stretching
vibration of the adsorbed water in the sample. FTIR
spectrum is observed for the different molar concentra-
tions of CuSnS thin film with TEA prepared by SILAR
method. The value of the absorption peak is shifted
according to nature of material and is shifted for the
increasing concentrations. Transmittance % is changes
according to the increasing molar composition.
3.5 UVVIS spectra analysis
3.5.1 Optical absorbance analysis
Absorbance and transmittance values are observed for
CuxSn1-xSy thin films in the wavelength range of
300900 nm using UVVis spectrometer analysis. Fig-
ures 19, 20 shows the plots of absorbance verses wave-
length for CuxSn1-xSy thin films. For the decreasing

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J Mater Sci: Mater Electron
Fig. 21 Plots of (Ahm)2 versus
hm for TEA added CuxSn1-xSy
thin films for 0.010.10 M
wavelength of incident photon, absorbance of CuxSn1-xSy
thin films increases. There is a very slow increase of
absorbance in visible region for the decreasing wave-
length for different compositions. The absorbance
increases with the decreasing wavelength and reaches a
small absorption peak with absorption maxima around
370 nm. The absorption edge of the films shifted towards
longer wavelength in the near visible region (below
600 nm) with the increasing molar composition. So, here
more number of valence electrons are converted into
conduction electron. The incident photons liberate more
number of electrons in the coated material. Photon to
electron conversion starts at the wavelength 650700 nm
for different composition.
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Fig. 21 Plots of (Ahm)2 versus
hm for TEA added CuxSn1-xSy
thin films for 0.010.10 M
3.5.2 Optical transmittance studies
Transmittance versus wavelength plot for CuxSn1-xSy thin
films for different molar concentration is given in Fig. 20.
Transmittance decreases for the minimum concentration of
copper and the maximum concentration of tin in the film
(Cu0.01Sn0.09S, Cu0.02Sn0.08S and Cu0.03Sn0.07S). Trans-
mittance increases for the maximum concentration of
copper and the minimum concentration of tin in the film
(Cu0.06Sn0.04S, Cu0.07Sn0.03S, Cu0.08Sn0.02S and Cu0.09
Sn0.01S). For the equal concentration of Copper and Tin,
the transmittance is higher it is slightly constant (Cu0.05
Sn0.05S and Cu0.04Sn0.06S). When tin is having maximum
concentration and in the absence of copper, the transmit-
tance is higher and slightly constant. All the absorbed
photons are transmitted to the next layer of the material in
copper maximum region (Cu0.09Sn0.01S). The process of
photons to electron conversion is very slow. This is very
similar in the case of tin maximum region (Cu0.00Sn0.10S)
but the process of photons to electron conversion to some
extent increases moderately to some extent.
For the increasing doping concentration, photon to
electron conversion is increasing. But the point of photon
to electron conversion is not constant. It may shift to longer
(red shift) or shorter (blue shift) wavelength region based
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J Mater Sci: Mater Electron
on the doping concentration. For the solar cell fabrication
doping of appropriate materials are advisable to increase its
efficiency.
3.5.3 Refractive index
The refractive index of the TEA added CuxSn1-xSy thin
film can be derived from the transmission spectrum using
the following Eq. 1
p
1 1  Tmax 2
ns 1
Tmax
This formula may fit for extremely little circumstances. If
the transmittance is higher, there is a meagre chance for
change of medium. In such type of situation, absorption is
neglected. So the transmission maximum is dominating in
the particular wavelength. The various refractive indices
(ns) for the increasing molar concentration are recorded in
Table 2.
3.5.4 Band gap analysis
Band gap energy of CuxSn1-xSy thin film observes the
graph of the absorption coefficient (Ahm)2 versus photon
energy (hm). Show the Fig. 21, the ternary material
J Mater Sci: Mater Electron

Fig. 22 Optical properties for the increasing molar concentration

Table 3 Absorbance, transmittance, refractive indices and the band gap of TEA added CuxSn1-xSy films
Molar concentration Absorbance Transmittance Refractive Band
CuxSn1-xSy (A.U.) (%) Index gap
(y = 0.10 M) (eV)

Cu0.01Sn0.09S 0.18 85 3.757 1.79

Cu0.02Sn0.08S 0.21 71.33 3.189 2.16
Cu0.03Sn0.07S 0.69 37.23 3.031 2.17
Cu0.04Sn0.06S 1.45 30.30 2.154 2.24
Cu0.05Sn0.05S 0.09 89.06 1.314 1.95
Cu0.06Sn0.04S 1.25 40.16 1.240 2.15
Cu0.07Sn0.03S 0.49 61.56 1.792 2.14
Cu0.08Sn0.02S 0.45 69.64 1.723 2.26
Cu0.09Sn0.01S 0.13 89.26 1.339 2.27
Cu0.10Sn0.00S 0.28 89.30 1.240 2.28

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CuxSn1xSy shows three different characters as follows. It
shows lower band gap for lower concentration of copper,
higher band gap for higher concentration of copper. The
step by step increasing flow of band gap is suddenly
arrested and gives the lower band gap energy value for
equal concentration of copper and tin. Band gap reaches
the maximum for the maximum concentration of copper.
Figure 22 shows the optical properties for the increasing
molar concentration. The absorbance and transmittance
data from the UVvisible spectrum analysis and the
manipulated data i.e., refractive index and band gap values
are recorded for the increasing copper and decreasing tin
composition (Table 3). The increasing concentration of the
material the change of property is observed. The main
deviation in the curve is due to the equal concentration of
both the materials. The graph reveals it clearly.
4 Conclusion
Copper doped SnS thin films (CuxSn1-xSy) (x = 0.01
0.10 M; y = 0.10 M) have been deposited by SILAR
technique. The structural, morphological and optical
properties of the nano thin films are investigated. As per
XRD studies CuSnS films are in amorphous nature. Binary
nature of the CuS and SnS materials are changed when they
converted into ternary material of Cu doped SnS thin films
are clearly observed with the help of optical properties like
absorbance, transmittance and band gap energy. Surface
morphology and topographical studies are explained with
the help of SEM and AFM by their grain size, roughness
and height. The above properties are observed for varying
molar concentrations. Cu and Sn are not mixed properly in
the film deposited for equal concentration. It may know
from the maximum value of their surface roughness.
Acknowledgments Authors acknowledge Department of Physics,
Anna University, Trichy for their UVvis-analysis, FTIR, AFM
support and National Institute of Technology, Tiruchirappalli for their
SEM and XRD support.
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J Mater Sci: Mater Electron
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