Materials Science in Semiconductor Processing 16 (2013) 825–832

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Materials Science in Semiconductor Processing

journal homepage: www.elsevier.com/locate/mssp

Deposition and characterization of pure and Cd doped SnO2

thin films by the nebulizer spray pyrolysis (NSP) technique
R. Mariappan a, V. Ponnuswamy a,n, P. Suresh b, R. Suresh a, M. Ragavendar c,
C. Sankar a
a
Department of Physics, Sri Ramakrishna Mission Vidyalaya College of Arts and Science, Coimbatore 641020, India
b
Materials Research Centre, Indian Institute of Science, Bangalore 560012, Karnataka, India
c
Department of Physics, RVS college of Engineering and Technology, Coimbatore 641042, Tamil Nadu, India

a r t i c l e i n f o abstract

Available online 8 February 2013 Pure and cadmium doped tin oxide thin films were deposited on glass substrates from
Keywords: aqueous solution of cadmium acetate, tin (IV) chloride and sodium hydroxide by the
Nebulizer spray pyrolysis nebulizer spray pyrolysis (NSP) technique. X-ray diffraction reveals that all films have
XRD tetragonal crystalline structure with preferential orientation along (200) plane. On
SEM application of the Scherrer formula, it is found that the maximum size of grains is
Electrical 67 nm. Scanning electron microscopy shows that the grains are of rod and spherical in
Optical properties shape. Energy dispersive X-ray analysis reveals the average ratio of the atomic
percentage of pure and Cd doped SnO2 films. The electrical resistivity is found to be
102 O cm at higher temperature (170 1C) and 103 O cm at lower temperature (30 1C).
Optical band gap energy was determined from transmittance and absorbance data
obtained from UV–vis spectra. Optical studies reveal that the band gap energy decreases
from 3.90 eV to 3.52 eV due to the addition of Cd as dopant with different concentrations.
& 2013 Elsevier Ltd. All rights reserved.

1. Introduction used techniques. It is a very easy, low cost, safe, and

Tin oxide (SnO2) is an n-type semiconductor material
with direct band gap energy (Eg)  3.9 eV [1–3] finds
many applications in high temperature electron devices,
transparent electron devices and so on. This is due to its
good optical, electrical properties and excellent chemical
and thermal stability [4–6]. It has also been widely used
in devices like sensors for detection of gases [7,8], solar
cells [9], and flat panel collectors with spectral selective
windows [10]. Researchers investigated a variety of tech-
niques to prepare SnO2 thin films, such as chemical vapor
deposition [11,12], co-precipitation method [12,13], dip
coating [14,15], spray pyrolysis [16–19] and sol–gel
method [20,21]. The technique used in this work is known
as the NSP technique which is one of the most widely
vacuum less system of the deposition technique for
preparing transparent conducting oxides compared with
other techniques. The other advantage of this technique is
that it can be easily adapted for production of large area
uniform film coatings.
The aim this work is to study the structural, optical
and surface properties of Cd doped ZnO films deposited by
the NSP technique at substrate temperature 450 1C with
different Cd doping concentrations reported. The main
objective is to employ the nebulizer spray pyrolysis
technique to obtain Cd Doped SnO2 which provides the
appropriate characteristics necessary for the fabrication of
optoelectronic devices.
2. Experimental technique

n
Corresponding author. Tel.: þ91 4 222 692 461;
Analytical grade cadmium chloride, tin (IV) chloride
fax: þ 91 4 222 693 812. and sodium hydroxide pellet were used for the film
E-mail address: marijpr@gmail.com (V. Ponnuswamy). preparation.

1369-8001/$ - see front matter & 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.mssp.2013.01.006
826 R. Mariappan et al. / Materials Science in Semiconductor Processing 16 (2013) 825–832

Fig. 1. Schematic diagram of the nebulizer spray pyrolysis (NSP) setup.

Pure and Cd doped SnO2 films deposited at substrate Table 1

temperature 450 1C with film thickness of 222 nm, Optimized preparative parameters for nebulizer sprayed pure and Cd
doped SnO2 thin films.
227 nm, 232 nm and 239 nm through the nebulizer
spray pyrolysis (NSP) technique. Taking the ionic radius Deposition spray rate 0.5 ml/min
into account, the radius of Sn (0.69 Å) is lower than that Cd concentrations 1%, 3% and 5%
of Cd (0.97 Å) and the doping of Cd leads to the increase Substrate temperature 450 1C
of the film thickness and crystallite size. Schematic pH of the solution 7
Deposition time 10 min
diagram of the NSP setup is shown in Fig. 1. The spray Nozzle to substrate distance 5 cm
solution was prepared by dissolving 0.1 M tin (IV) Carrier gas pressure 30 psi
chloride dissolved in 25 ml of de-ionized water and
the solution was stirred for 10 min using magnetic
stirrer. NaOH solution was added slowly with tin (IV) (Philips Model XL 30), respectively. The electrical resis-
chloride solution from a buret held vertically until pH tivity of the films was studied using a four probe setup.
value reached to 7. Similarly 0.1 M cadmium chloride Optical absorption spectrum was recorded using a JASCO-
solution was also prepared. Cadmium chloride solution V-570 spectrophotometer.
was added to the above tin (IV) chloride solution with
(Cd/Sn) nominal volume proportions 1%, 3% and 5%. The 3. Results and discussion
stirring was continued for 30 min to get clear and
homogeneous spray solution. The prepared solution 3.1. Structural analysis
was sprayed onto ultrasonically cleaned glass
substrates kept at 450 1C. Films prepared by this The X-ray diffraction patterns of the pure and Cd
method have uniform thickness and well adherent doped SnO2 thin films deposited at 450 1C with different
with the substrate. The optimized preparative para- Cd concentrations are shown in Fig. 2a–d. X-ray diffrac-
meters for pure and Cd doped SnO2 thin films are listed tion spectra reveal the polycrystalline nature of the films
in Table 1. with tetragonal structure. The most intense peak was
X-ray diffraction data of the nebulizer sprayed pure observed at (200) plane and additional peaks were along
and Cd doped SnO2 films were recorded with the help of a (110), (101), (200), (211), (002), (310) and (112) planes.
Philips Model PW 1710 diffractometer with Cu Ka radia- The peak intensity observed at (200) plane was found to
tion (l ¼0.1542 nm). Surface morphological studies and increase gradually with the increase of Cd concentration
compositional analysis were carried out using a scanning from 1% to 5%. The different peaks in the diffractogram
electron microscope and energy dispersive X-ray analysis were indexed and the corresponding values of interplanar
setup attached with scanning electron microscopy spacing ‘‘d’’ were calculated and compared with standard
 R. Mariappan et al. / Materials Science in Semiconductor Processing 16 (2013) 825–832 827

Fig. 2. X-ray diffraction patterns of Cd doped SnO2 thin films: (a) pure
SnO2, (b) 1% Cd sample, (c) 3% Cd sample and (d) 5% Cd sample.

Fig.. 3. X-ray diffraction peak position of the pure and Cd doped SnO2
thin films: (a) pure SnO2, (b) 1% Cd sample (c) 3% Cd sample, and (d) 5%
Cd sample.

values of Joint Committee on the Powder Diffraction

Spectra data (JCPDS 88-0287). It is found that higher Cd
concentration leads to the formation of well-crystallized
films. It is also observed from Fig. 2d that higher Cd
concentration gives in good quality films with improved
crystallinity as evidenced by intense diffraction peaks.
The Cd doped SnO2 thin films deposited at 450 1C with Cd
concentration (5%) are found to be well crystalline in
nature. The height of (200) peak in X-ray diffraction
pattern for Cd doped SnO2 thin films deposited at higher
Cd concentration (5%) has shown sharper peaks and small
FWHM data as indicated in Fig. 2d. The peak at (200)
plane is found to be shifted for pure and Cd doped SnO2
films as shown in Fig. 3. A peak developed by a well
Fig. 4. Variation of lattice constant (a,c) with Cd concentration of Cd
doped SnO2 thin films, (b) variation of grain size and microstrain with Cd
concentration of pure and Cd doped SnO2 thin films and (c) variation of
dislocation density and stacking fault with Cd concentration of pure and
Cd doped SnO2 thin films.
prepared Cd doped film was used as a reference to
compare the peak position shift due to different reflec-
tions and hence to evaluate the microstructural
parameters.
828 R. Mariappan et al. / Materials Science in Semiconductor Processing 16 (2013) 825–832

The lattice constant (a,c) was calculated using Eq. (1) variation of crystallite size and microstrain with Cd
for the pure and Cd doped SnO2 films [22]: concentration of Cd doped SnO2 films is shown in
Fig. 4b. In Fig. 4b, it is observed that the crystallite size
2 2 2
1 ðh þ k Þ l increases along (002) plane with Cd concentration
2
¼ þ 2 ð1Þ
d a2 c increase and attains a maximum 67 nm at 450 1C. It is
The variation of lattice constant (a,c) with different Cd observed that (Fig. 4b), a sharp increase in crystallite size
concentrations for Cd doped SnO2 films is shown in and decrease in microstrain with the increased Cd con-
Fig. 4a. It is observed that (Fig. 4a) the lattice constant centration. The variation of dislocation density and stack-
(a,c) value of SnO2 thin film is slightly decreased with the ing fault probability with Cd concentration of the films is
increased Cd concentration as compared with Joint shown in Fig. 4c. For Cd concentration (5%), the minimum
Committee on the Powder Diffraction Spectra data (JCPDS values for dislocation density and stacking probability of
88-0287). the film (Fig. 4b) are obtained. Pure and Cd doped SnO2
The dislocation density, microstrain and stacking fault films with lower strain, dislocation density and stacking
probability of the pure and Cd doped films were calcu- fault probability improve the crystallinity of the films
lated using the following equations [22-24]: which in turn increase the volumetric expansion of the
films. The lattice constant (a,c), crystallite size, micro-
l b
e¼  ð2Þ strain, dislocation density and stacking fault probability
D siny tany
results of the films are given in Table 2. It is concluded
1 from the structural analysis that the addition of Cd has a
d¼ lines=m2 ð3Þ strong effect on the structural properties of the films.
D2
" #
2p2
a¼ b ð4Þ 3.2. Surface morphology analysis
45ð3 tanyÞ1=2

The crystallite sizes of pure and Cd doped SnO2 thin
films were evaluated using the Scherer formula [25]:
0:9l
D¼
bcos y
where D is the mean crystallite size, b is the full width at
half maximum of the diffraction line, y is the diffraction
angle, and l is the wavelength of the X-radiation. The
Pure and Cd doped SnO2 films were deposited at
450 1C with different Cd concentrations from 1% to 5%.
Scanning electron micrographs of the deposited films
ð5Þ with 1500 and 10,000 magnifications are shown in
Fig. 5. The morphology changes of the films with respect
to Cd concentrations and the corresponding grain size
estimations are depicted in Fig. 5. The pure tin oxide
(SnO2) film demonstrates many pellets like grains as

Table 2
To calculate the structural parameters of pure and Cd doped SnO2 thin films.

2y d- FWHM (hkl) Lattice Lattice Crystallite Dislocation density, Microstrain e Stacking fault,
Spacing [2y] Crystal constant constant size (nm) d (10  14 lin/m2) (10  4 lin  2 m  4) a (10  4 J/m2)
[Å] system a, (Å) c, (Å)

Pure 26.592 3.352 0.299 110 28.497 12.31 14.10 27.20

SnO2 33.823 2.650 0.149 101 57.955 02.98 05.48 11.99
37.844 2.377 0.224 200 4.7472 3.1893 39.077 06.55 07.29 16.94
51.687 1.767 0.456 211 20.212 24.48 10.49 28.96

1% Cd 26.490 3.364 0.187 110 45.571 04.82 08.85 18.04

33.792 2.652 0.093 101 92.721 01.16 03.43 07.50
37.852 2.376 0.224 200 39.078 06.55 07.29 16.94
51.629 1.770 0.187 211 4.7455 3.1583 49.277 04.12 04.31 11.88
57.817 1.594 0.448 002 21.118 22.42 09.05 26.69
61.775 1.501 0.897 310 10.771 08.61 16.71 51.29
65.872 1.416 0.547 112 18.062 03.06 09.41 30.05

3% Cd 26.553 3.357 0.187 110 45.577 04.81 08.83 17.02

33.822 2.650 0.187 101 46.364 04.65 06.85 14.99
37.896 2.374 0.187 200 46.900 04.55 06.07 14.11
51.661 1.769 0.224 211 4.7507 3.1307 41.069 05.96 05.16 14.26
61.816 1.500 0.299 310 32.324 09.57 05.57 17.09
65.898 1.416 0.410 112 24.086 17.24 07.05 22.53

5% Cd 26.464 3.368 0.149 110 56.961 03.08 07.09 13.69

33.763 2.655 0.448 101 19.319 26.79 16.47 36.00
37.901 2.374 0.131 200 67.002 02.23 04.25 09.87
51.623 1.771 0.187 211 4.7486 3.1352 49.275 04.12 04.31 11.89
61.871 1.499 0.299 310 32.333 09.57 05.56 17.08
65.829 1.417 0.274 112 36.115 07.67 04.71 15.03
 R. Mariappan et al. / Materials Science in Semiconductor Processing 16 (2013) 825–832 829

observed in the image of scanning electron microscopy. 3.3. Compositional analysis

The estimated grain sizes form the SEM images are in the
range 350–4500 nm. As the Cd concentration increases
from 1% to 3%, the surface formed is found to have rods
and spherical structures with average grain size are
450 nm and  500 nm. The grain size transformation
from rod to spherical is observed for the Cd doped SnO2
film deposited 450 1C with 5% Cd concentration and the
average aggregate size lies between 500 and 600 nm.
The chemical composition of sprayed pure and Cd
doped SnO2 thin films deposited at substrate temperature
450 1C with different Cd concentrations from 1% to 5% is
shown in Fig. 6a–d. The spectra depicted in Fig. 6a–d are
for pure and Cd doped SnO2 thin films which has peak of
1.8 keV due to the presence of silicon in the substrate used
for the film preparation [26]. The peaks corresponding to

Fig. 5. Scanning electron microscopy images of pure Cd doped SnO2 thin films: (a) pure SnO2, (b) 1% Cd sample, (c) 3% Cd sample and (d) 5% Cd sample.
830 R. Mariappan et al. / Materials Science in Semiconductor Processing 16 (2013) 825–832

Fig. 6. Energy dispersive X-ray analysis spectra of pure and Cd doped SnO2 thin films: (a) pure SnO2, (b) 1% Cd sample, (c) 3% Cd sample and
(d) 5% Cd sample.

Si, Cd, Sn and O are observed in the EDAX indicating the

formation of Cd doped SnO2 product and the atomic
percentages of Cd, Sn and O and their values are listed in
the inset (table) of Fig 6.

3.4. Electrical properties

Resistivity measurement of pure and Cd doped SnO2

Fig. 7. Change of resistivity (r) with temperature of pure and Cd doped
SnO2 thin films: (a) pure SnO2, (b) 1% Cd sample, (c) 3% Cd sample and
(d) 5% Cd sample.
films is very important from the application point of view.
The electrical resistivity of the films was measured using a
four probe setup in the temperature range 30–170 1C as
shown in Fig. 7. The measurement is performed by making
four electrical contacts with the sample surface. Two of the
probes are used to measure the current and the other two
probes are used to measure the corresponding voltage. The
electrical resistivity of the pure and Cd doped films was
calculated using the following relation [27]:
V
r¼ 2pS ð6Þ
I
where r is the electrical resistivity, V is the voltage, I is the
 R. Mariappan et al. / Materials Science in Semiconductor Processing 16 (2013) 825–832 831

current and S is the distance between interpair of probes. The following relation [30]:
resistivity of pure and Cd doped SnO2 films decreases with 2:303xlogðTÞ
increase in temperature indicating the development of semi- a¼ ð8Þ
d
conducting nature. It is observed (Fig. 7a–d) that the resis-
tivity decreases non-linearly with the temperature increase. where d is the film thickness and T is the transmission.
It is well known that electrical properties of polycrystalline The absorption coefficient (a), energy gap (Eg) and photon
films are strongly influenced by their structural character- energy (hu) are related as [24]:
istics and nature of purity. From Fig. 7a, the electrical ðahuÞ ¼ AðhuEg Þn ð9Þ
resistivity of the film is found to be 8.79  103 O cm at lower
temperature and 1.99  103 O cm at higher temperature. where u is the frequency, A is a constant and n assumes
When Cd concentration increases upto 5%, the electrical values 1/2, 2, 3/2, and 3 depending on the mode of
resistivities of the films are in the range between
5.43  103 O cm and 4.53  102 O cm. The decrease may be
due to the crystallite size increase of the films. The tempera-
ture dependence of the activation energy can be accounted
using the Arrhenius relation [28]:
 
Ea
s ¼ s0 exp ð7Þ
RT

where s and s0 are the electrical conductivities, R is the ideal

gas constant and T is the temperature. The electrical con-
ductivities of the pure and Cd doped SnO2 films deposited at
substrate temperature (450 1C) with different concentrations
are listed in Table 3. It can be seen (Table 3) that the electrical
conductivity increases with the increase of Cd concentration.
The activation energies of pure and Cd doped SnO2 films
were found to be in the range between 0.40 eV and 0.41 eV
in the lower temperature region (30 1C) and 0.55 eV to
0.49 eV in the higher temperature region (170 1C). The
calculated values of electrical resistivity, conductivity and Fig. 8. Transmittance spectra of Cd doped SnO2 films.

activation energy of pure and Cd doped SnO2 films are listed

in Table 3. The above results confirm the stability of the pure
and Cd doped SnO2 films and their employability in optoe-
lectronics devices.

3.5. Optical properties

The transmittance spectra of pure and Cd doped SnO2

thin films were studied by UV–vis–NIR double beam
spectrophotometer in the range 250–2000 nm. The pre-
sence of transmittance maxima at wavelength region
345 nm is observed (Fig. 8) and the shift toward higher
wavelength region is found with Cd concentration
increase in the pure and Cd doped SnO2 films. The
higher-energy electronic transitions from valence to con-
duction bands confirm the direct type semiconducting
nature of the material [29]. The absorption coefficient (a)
was calculated from the transmission data using the Fig. 9. Plot of (ahn)2 versus hu for Cd doped SnO2 thin films.

Table 3
Electrical resistivity, electrical conductivity and activation energy of the pure Cd doped SnO2 thin films.

Resistivity r (O cm) Conductivity s (O cm)  1 Activation energy Ea (eV)

30 1C 170 1C 30 1C 170 1C 30 1C 170 1C

Pure SnO2 8.79  103 1.99  103 1.14  10  4 5.01  10  4 0.41 0.55
1% Cd 8.79  103 1.35  103 1.41  10  4 7.36  10  4 0.41 0.53
3% Cd 5.71  103 9.06  102 1.75  10  4 1.10  10  3 0.40 0.52
5% Cd 5.43  103 4.53  102 1.84  10  4 2.21  10  3 0.40 0.49
832 R. Mariappan et al. / Materials Science in Semiconductor Processing 16 (2013) 825–832
interband transition, i.e., direct, allowed indirect, direct
forbidden and indirect forbidden transition, respectively.
For allowed direct type of transitions
ðahuÞ ¼ AðhuEg Þ1=2
A typical plot of (ahu)2 versus hu for pure and Cd doped
SnO2 films are shown in Fig. 9. Extrapolating the linear
portion of the curve to touch the energy axis which gives
the value of energy gap for pure and Cd doped SnO2 films.
The band gap value is estimated as 3.9 eV (pure SnO2) and
is in agreement with the band gap energy of pure SnO2
[31–33]. The band gap of films is found to be decreased
with increasing Cd concentration upto 5%, correspond-
ingly the direct band gap energy decreases from 3.90 to
3.52 eV. This reduction in band gap energy may be due to
the decrease of hole concentration with the increase of Cd
doping in the doped thin films.
4. Conclusions
The nebulizer sprayed cadmium doped tin oxide
(Cd:SnO2) thin films were deposited on glass substrate
at substrate temperature 450 1C with different Cd con-
centration. X-ray diffraction confirms the tetragonal
structure with preferred orientation along (200) plane.
Crystallite size is found to be increased with Cd concen-
tration. The scanning electron microscopy studies reveal
that the pure tin oxide (SnO2) film demonstrates many
pellets like grains. The average grain sizes of the grains
are in the range of 350–400 nm. The presence of elemen-
tal constituents was confirmed from energy dispersive
X-ray analysis. The electrical resistivity of pure and Cd
doped SnO2 films was estimated and found to be in
between 5.43  103 O cm at lower temperature (30 1C)
and 4.53  102 O cm at higher temperature (170 1C). The
maximum optical transmittance 80% was obtained for
pure and 5% Cd doped SnO2 film deposited at substrate
temperature (450 1C). From the optical studies it is
observed that the band gap energy decreases from 3.90
to 3.52 eV with increase of Cd concentration. The inves-
tigation results of the pure and Cd doped SnO2 films
prepared by the NSP technique ensure the stability of the
films and their employability in optoelectronics device
applications.
Acknowledgments
The authors are very much grateful to Sophisticated
Test and Instrumentation Centre, Cochin, and Alagappa
University, Karaikudi, for providing instrument facilities.
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