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Optical, structural and photo electrochemical properties of Cd1−xZn x S films

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Article  in  Applied Physics A · July 2018

DOI: 10.1007/s00339-018-1910-0

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Applied Physics A (2018) 124:494
https://doi.org/10.1007/s00339-018-1910-0

Optical, structural and photo electrochemical properties of ­Cd1−xZnxS

films grown by chemical bath deposition
W. G. C. Kumarage1,2 · R. P. Wijesundera3 · V. A. Seneviratne1,2 · C. P. Jayalath1,2 · T. Varga4 · B. S. Dassanayake1,2

Received: 11 April 2018 / Accepted: 13 June 2018

© Springer-Verlag GmbH Germany, part of Springer Nature 2018

Abstract
Cd1−xZnxS (0 ≤ x ≤ 0.5) films were fabricated by chemical bath deposition method and characterized by grazing incidence
X-ray diffraction (GIXRD), scanning electron microscopy (SEM), UV–visible spectroscopy and photoelectrochemical (PEC)
cell. The flat-band potential value was found to be tunable from − 441 to − 664 mV with increasing ­Zn2+ concentration in the
reaction solution. GIXRD results indicate that the fabricated ­Cd1−xZnxS are hexagonally oriented and ­Zn2+ is successfully
introduced into CdS. SEM results indicate that high Z ­ n2+ doping concentration can form flake-like C
­ d1−xZnxS morphology.
2+
Furthermore, ­Zn incorporation to the CdS was found to enhance the optical absorbing capability of CdS in visible region.
The optical band gap was found to vary as the composition parameter changed from x = 0.0 to x = 0.5 in the reaction solution.
Best photoactive properties in the PEC exhibited for the samples grown with the deposition bath composition of x = 0.3.

1 Introduction Among numerous ways of synthesizing ­Cd1−xZnxS films,

It has been established that solid solution systems of two
or more semiconductor phases are of great importance in
view of their significant role in technological advancements
[1, 2]. The present work discusses the use of chemical bath
deposition (CBD) technique to deposit semiconductor thin
films with graded composition on fluorine-doped ­SnO2
(FTO) substrates. The ­Cd1−xZnxS films, which is a direct
band gap II–VI ternary compound, is well-known as a win-
dow material of CIGS thin film solar cells and CdTe solar
cells due to its wide band gap, low resistivity and formation
of ohmic contacts [3–8]. However, the use of a C ­ d1−xZnxS
thin films as a window layer also creates challenging prob-
lems as higher zinc concentration can lead to high-resistivity
materials, which can increase the sheet resistance [9, 10].
* B. S. Dassanayake
buddhikad@pdn.ac.lk
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, Kelaniya 11600, Sri Lanka
4
Environmental Molecular Sciences Laboratory, Pacific
Northwest National Laboratory, Richland, WA 99352, USA
CBD stands out as it is a simple and low-cost method to
prepare high-quality thin films which are uniform and highly
adhesive to the substrate [9, 11–13]. The present report dis-
cusses about the fabrication of ­Cd1−xZnxS thin films by CBD
method and the tunability of the optical and electrical prop-
erties of the fabricated samples.
Recombination losses can occur at several different
regions in a solar cell due to discontinuities in the depletion
region, space charge region, and in the bulk due to the dif-
ferent electron affinity levels of the semiconductor materials.
These discontinuities contribute to the low performance in
the PV devices [14]. The traps are responsible for the reduc-
tion of open circuit voltage (VOC) and the fill factor (FF) of
the PV devices. Hence, the tunability of the flat-band poten-
tial value is quite important to fabricate p-n junctions with
less energy traps or spikes in the depletion region. There-
fore, Mott–Schottky measurements are considered as an
important characterization, which offer useful information
on flat-band potential (Vfb) value and the conduction type
of the semiconductor, doping density. However, for n-type
­Cd1−xZnxS films, this behavior has not been studied before
according to the knowledge of authors.
Furthermore, in the reporting work, grazing incidence
X-ray diffraction (GIXRD), which is an ideal method to
investigate the structural changes in surfaces, layers and
thin films due to low penetration, has been used to analyze
crystallographic structures of fabricated C ­ d1−xZnxS films.

13
Vol.:(0123456789)
 494   Page 2 of 7
Additionally, the Vfb value, which reveals information about
band-edge position and charge transfer kinetics across the
semiconductor interface, has been extensively discussed
in the reporting work. The relative efficiency of detection
of light as a function of wavelength was estimated using
spectral response for the fabricated ­Cd1−xZnxS [15]. Fur-
thermore, surface morphology, optical and electronic prop-
erties of the material has been studied using scanning elec-
tron microscopy (SEM), UV–visible spectroscopy and the
surface properties at the interface has been studied using
photoelectrochemical cell (PEC).
2 Experimental
2.1 Chemical reaction route of ­Cd1−xZnxS
Cd1−xZnxS is formed from the reaction between dissolved
cadmium and zinc ions and thiourea molecules in an alkaline
solution. The reaction chemistry can be described as follows
[11, 16],
CdSO4 → Cd2+ + SO2−
4
, (1)
ZnSO4 → Zn2+ + SO2−
4
. (2)
However, to prevent the formation of cadmium sulfide
and zinc sulfide, instead of forming ­Cd1−xZnxS, ammonia is
introduced as a complexing agent into the reaction solution.
NH3 + H2 O ↔ NH+4 + OH ,
_ reference electrode during the Mott–Schottky measure-
(3)
Cd2+ + nNH3 ⋅ H2 O ↔ Cd(NH3 )2+ + nH2 O, (4)
n
Zn2+ + nNH3 ⋅ H2 O ↔ Zn(NH3 )2+
n
+ nH2 O, (5)
CS(NH2 )2 + 2OH− ↔ S2− + CN2 H2 + 2H2 O, (6)
Finally, ­Cd1−xZnxS is formed as a thin film at the active
point of the substrate surface:
(1 − x)Cd(NH3 )2+ + xZn(NH3 )2+ + S2−
n n
(7)
+ Active Point ↔ Cd1−x Znx S + nNH3 .
2.2 CBD growth of ­Cd1−xZnxS thin films
Cd1−xZnxS thin films were deposited on FTO glass sub-
strate using CBD technique. The substrates were cleaned
before and after the deposition using standard procedure
[9, 17, 18]. The samples were fabricated in an aqueous
solution containing 0.002 M thiourea [CS(NH2) 2, 99%,
MRS Scientific Inc., UK] and 1.1 ml of ammonia solution
­(NH3, 35% w/w, Surechem Products Ltd, England), cad-
mium sulfate (­ 3CdSO4·8H2O, 99%, Breckland Scientific,
UK) and zinc sulfate (­ ZnSO4·7H2O, 99.8%, VWR prolabo,
13
W. G. C. Kumarage et al.
Belgium), in 140  ml of deionized water. The samples
were labeled according to the Cd:Zn molar ratio as shown
in Table 1. The deposition process was carried out at a
bath temperature of 80 °C for 1 h. All samples were later
annealed at 200 °C for 1 h in a tube furnace (BüchiTo-51).
2.3 Characterization
GIXRD was conducted using a Philips X’pert diffractom-
eter to analyze structural properties. The instrument used
CuKα radiation with λ = 1.54184 Å in continuous mode
at a generator voltage of 45 kV and 40 mA tube current.
Scans in the 20°–80° 2θ range were carried out with a
step size of 0.02° and 5 s time per step. The grazing angle
was set to 2°. SEM imaging of CdS was obtained using
a Zeiss EVO|LS15 taken under 50 k magnification, using
a 20 kV beam, to study the morphology of samples. The
absorption and the transmittance spectra for the samples
were obtained using UV-1800 Shimadzu double beam
UV–vis spectrophotometer in the range of 300–800 nm
to examine the optical absorption and the transmittance
variation. An XP-1 profilometer, Ambios Technology was
used to determine the thickness of the fabricated CdS thin
films. The PEC analysis was carried out on PEC Cell L01
with an AM 1.5 simulated solar light irradiation using a
150 W short-arc xenon lamp. The solid/liquid junction was
held at 0.2 V and 1000 Hz with respect to the Ag/AgCl2
ments. HD Hokuto Denko Hab–151 potentiostat and SR
model 830, ESP lock-in amplifier was used for the spectral
response measurements. A 0.1 mol dm−3 ­Na2S2O3 solution
was used as the electrolyte for all the electrical charac-
terizations, while keeping the effective area of the CdS/
electrolyte at 0.25 cm2. Pt and Ag/AgCl2 electrodes were
used as counter and reference electrodes, respectively, for
electrical measurements. The sheet resistance (RS) of the
samples was measured by four-point probe method using
Keithely-485 electrometer.
Table 1  Fabricated ­Cd1−xZnxS composition and the sample code
Sample x CdSO4 (mmol) ZnSO4 (mmol)
Z-0 0 0.67 0
Z-1 0.1 0.6 0.07
Z-2 0.2 0.53 0.14
Z-3 0.3 0.47 0.20
Z-4 0.4 0.40 0.27
Z-5 0.5 0.33 0.34
Optical, structural and photo electrochemical properties of ­Cd1−xZnxS films grown… Page 3 of 7  494

3 Results and discussion -400

The flat-band potential (Vfb) and carrier concentration (ND) -450

were calculated from the X-axis intercept and the slope of
the linear fit of the Mott–Schottky equation [19, 20]; -500

1 2 kT
( )
= V − V − , (8) -550

Vfb (mV)
fb
C2 A2 𝜀𝜀 eN
0 D e

where e is the electron charge, ε (= 8.5) is the dielectric -600

constant, ε0 is the permittivity in vacuum and A is the area
of the solid to electrolyte [21]. The Mott–Schottky plots (not -650
shown) confirm the n-type behavior of all the fabricated
­Cd1−xZnxS thin films. The ND values for all the deposited -700
films were calculated and are tabulated in Table 2. It can
0 0.1 0.2 0.3 0.4 0.5
be seen from the Table 2, all the Zn incorporated samples
Sample (x)
shows higher ND and Vfb values compared to untreated CdS,
while sample Z-3 appears to have a higher ND with respect
to the other fabricated CdS films along with the highest Vfb Fig. 1  Flat-band value variation of the fabricated C
­ d1−xZnxS samples
value (Fig. 1; Table 2). The Vfb value was found to be tuna-
ble with the ­Zn2+ concentration in the reaction solution. The
existence of different Vfb in a same PEC indicates change enhancement in ISC can be associated to the improved ND
in relative band-edge position supports of the fabricated which is evident from Table 2.
­Cd1−xZnxS along with the ­Zn2+ concentration. The tunability Figure 3 shows the sheet resistance of the fabricated sam-
of the relative band-edge position suggests the possibility of ples. The calculated sheet resistance values were found to
obtaining smooth band lineup throughout the p–n junction
[19]. These variations in ND and Vfb affect both short-circuit
current (ISC) and open circuit voltage (VOC) value of the 22.0
(a)
fabricated ­Cd1−xZnxS photoelectrodes [1, 9, 22].
All the fabricated films were electrically characterized by 17.6
ISC (µA)

employing the PEC cell measurements. Figure 2a–c depicts

13.2
the variation of ISC, VOC and ISC × VOC obtained for the
fabricated samples. Out of all the investigated samples, the 8.8
­Cd1−xZnxS samples seems to show higher ISC × VOC values
compared to CdS with C ­ d0.7Zn0.3S (Z-3) being the highest 372
as seen in Fig. 2c and Table 2. (b)
The higher VOC in Zn incorporated samples can be attrib- 310
VOC (mV)

uted mainly to the increased Vfb and the optical band gap
248
(Eg). The increase in Vfb may be caused due to creation of the
donor levels that effectively shift the Fermi level, increasing 186
the amount of band bending and hence the VOC [23]. The

(c)
5.7
ISC × VOC (µW)

Table 2  The electrical properties of the fabricated ­Cd1−xZnxS samples

3.8
Sample ISC (µA) VOC (mV) ISC × VOC Vfb (mV) ND
(µW) ­(1017 cm−3) 1.9
Z-0 8.00 166 1.33 − 441 0.14
0.0
Z-1 20.67 267 5.53 − 525 2.55 0 0.1 0.2 0.3 0.4 0.5
Z-2 18.67 280 5.23 − 543 2.57
Sample (x)
Z-3 20.87 327 6.82 − 664 2.65
Z-4 19.00 313 5.94 − 657 2.54
Fig. 2  Variation of a ISC, b VOC and c ISC  ×  VOC of fabricated
Z-5 18.33 310 5.70 − 614 2.50
­Cd1−xZnxS samples

13
 494   Page 4 of 7 W. G. C. Kumarage et al.

35 concentration as shown in Table 2 [25]. Figure 3 suggests

Sheet Resistance that higher concentration of ­Zn2+ in the reaction solution
30 reduces the sheet resistance [9]. According to Chavhan et al.
formation of high resistive material with increasing Z ­ n2+
25 concentration could be the reason for the increment of sheet
Sheet Resistance (MΩ)

resistance beyond x > 0.3 [9, 26].

20 Figure 4a–d shows SEM micrographs for four C ­ d1−xZnxS
photoelectrode with the x = 0.0, 0.1, 0.3 and 0.5, respectively.
15 The films fabricated without ­Zn2+ in the reaction solution
(x = 0), shows smooth and uniform spherical grains with-
10 out creaks or pinholes and covered the glass substrate well
(Fig. 4a). Small uniform grains with well-defined grain bound-
5
aries were found, (in the SEM images) along with the incre-
ment of Zn content up to x =  0.3 in the reaction solution, which
0
0.0 0.1 0.2 0.3 0.4 0.5 can potentially increase the roughness of the Zn incorporated
Sample (x) sample. The enhance ISC value in the Zn incorporated samples
can be due increased roughness value. The SEM images of the
­Cd1−xZnxS sample given in Fig. 4c, d reveal a sheet-like mor-
Fig. 3  Sheet resistance value of the Z-0, Z-1, Z-3 and Z-5 samples
phology. The possibility of formation of flake-like or sheet-like
morphology (shown in arrow) has been reported due to the
be lower for all the Zn-assisted CdS thin films compared agglomeration of smaller particles [27, 28].
to that of untreated. The resistivity of a semiconductor In order to determine the short-circuit photocurrent (ISCP) as
material depends on the product of charge carrier density a function of wavelength, the spectral response was employed
and the carrier mobility [24]. The lower sheet resistance on all the fabricated C­ d1−xZnxS photo electrodes. Figure 5
on the Zn-assisted films can be due to the increased carrier shows the spectral response of all the fabricated ­Cd1−xZnxS

(a) (b)

200 nm 200 nm

(c) (d)

200 nm 200 nm

­ d1−xZnxS samples a x = 0, b x = 0.1, c x = 0.3 and d x = 0.5

Fig. 4  SEM micrograms of the fabricated C

13
Optical, structural and photo electrochemical properties of ­Cd1−xZnxS films grown… Page 5 of 7  494

where α is the absorption coefficient of the film, A is a mate-

0.40
x=0 rial dependent constant, h is Planck’s constant and ν is the
0.35 x=0.1 frequency of light. The experimentally observed absorption
x=0.2
values of (αhυ)2 against hυ are plotted in Fig. 6a for different
Normalized photocurrent

0.30 x=0.3
x=0.4 compositions of x in the reaction solution.
0.25 x=0.5 The shift in the absorption peak can be due to two rea-
0.20
sons, (1) quantum confinement and (2) alloying [34]. The
bulk band gaps of ZnS and CdS are 3.6 and 2.4 eV, while
0.15 Bohr radii of exciton are ~ 2.2 and ~ 3.0 nm, respectively
0.10
[35]. The crystallite sizes of the fabricated samples (not
shown) are found to be greater than Bohr radius of exciton.
0.05 Therefore, quantum confinement effect can be ruled out as
0.00 the cause of the shift in the absorption peak and the shift is
350 400 450 500 550 600 650 indicative of the formation of a solid solution.
Wavelength (nm.) The Eg is calculated from the x-axis intercept of the
plots that are shown in Fig. 6a [36–38]. From the results of
Fig. 5  Spectral response of the fabricated ­Cd1−xZnxS samples Fig. 6b, Eg for the C
­ d1−xZnxS thin films seem to be improved
from 2.33 to 2.51 eV with an increase of Zn concentration
from x = 0.0 to 0.5. The higher Eg values of C­ d1−xZnxS com-
(x = 0.0–0.5). The lower ISCP on the shorter wavelength region pared to CdS, is due to the introduction of Zn, suggesting
may be due to the absorption of light in the electrolyte and that ­Cd1−xZnxS thin films enable more photons to transmit
the higher number of surface recombination of the photogen- through compared to CdS [39]. According to the Zhou et al.
erated minority carriers. The smaller photocurrent at longer the higher transmittance of an n-type window layer is impor-
wavelengths may be possible due to the lower absorption of tant to form efficient solar photovoltaic cells [40]. Addition-
the light at the photoanode used [30]. The spectral response is ally, the variation observed in the residual strain can be a
highest for Z-3 compared to the other ­Cd1−xZnxS samples with reason for the variation of Eg with the x value in the reaction
the peak shifting towards shorter wavelengths with increasing solution.
Zn concentration. Figure 7a–c display GIXRD patterns of the C ­ d1−xZnxS
As the C­ d1−xZnxS is a direct band gap semiconductor, the photoelectrode for x = 0.0, 0.3 and bare FTO glass, respec-
absorption coefficient can be related to the frequency of inci- tively. It can be seen from Fig. 7a, b that the diffraction
dent light using the Eq. (8) [21, 29–33] peaks of all samples are in good agreement with the hex-
)1∕ agonal phase of CdS (JSPDS card no. 41–1049). No peaks
𝛼h𝜈 = A h𝜈 - Eg 2 (8) of any other phases or impurities are noticed. Thus, it can
(

(a) (b)

Fig. 6  a The plot of (αhυ)2 against hυ for the fabricated ­Cd1−xZnxS samples, b variation of Eg value of the fabricated C
­ d1−xZnxS samples

13
 494   Page 6 of 7 W. G. C. Kumarage et al.

(a) CdS 3.5

002 H
11.4
o
3.0

7.6
2.5 100

101 H
100 H
002

110 H

103 H
3.8 2.0
o o 101
o
o 110

TC
0.0 1.5
103
(b) CdZnS 1.0
21.9
Intensity (× 103)

0.5
14.6
0.0
7.3 x=0 x=0.3
Sample
0.0
(c) FTO
12.3 Fig. 8  Variation of the texture coefficient of CdS (x = 0) and
­Cd0.7Zn0.3S (x = 0.3) films
8.2

4.1 of the fabricated films were influenced by the Cd/Zn molar

ratios. The average transmittance in the wave length range of
0.0 500–800 nm was found to be higher for C ­ d1−xZnxS (> 80%)
20 30 40 50 60 70 80
compared to CdS (73%), whereas the transparency increases
2θ (deg.)
with increasing Zn ion content. The slopes of transmittance
spectra were found to be varied with respect to composition
Fig. 7  GIXRD of the a CBD–CdS (Z-0), b Zn-doped CBD–CdS
‘x’. Different slopes obtained of these spectra could be due
(Z-3) and c Bare FTO substrate
to changes in stoichiometry [44]. The nature of this transmit-
tance (> 80% in the transmittance edge) variation suggests
be concluded that ZnS does not exist in the prepared sam- its suitability as a window material for fabrication for solar
ples. However, the intensity of (100), (101), (110) and (103) cells [45]. In addition, absorption edge blue shifted as Zn
reflections are significantly decreased with the increase of concentration increased, indicating an increase in their opti-
­Zn2+ concentration in the reaction solution. Additionally, the cal band gap values.
observed peak broadening from the GIXRD patterns indi-
cates a decrease in size of the crystallites as the concentra-
tion of ­Zn2+ increases.
The texture coefficient ­(TChkl) of samples Z-0 and Z-3 100
was calculated to investigate the preferential crystallite ori- x=0
entation in the films. The T­ Chkl was calculated considering x=0.1
all the reflection planes mentioned above in Fig. 6a, b using 80 x=0.2
the equation [41–43]; x=0.3
Transmittance (a.u%)

x=0.4 100
I(hkl) ∕I0(hkl) x=0.5
TChkl = 1∕n [ ni=1 I(hkl) ∕I0(hkl) ]
∑ , (9) 60
Transmittance (a.u%)

80

where I(hkl) is the measured relative intensity of a plane hkl,

and I0(hkl) is the standard intensity of the plane hkl taken from 40 60
the JCPDS data (JCPDS 06-0314), and n is the number of
X-ray diffraction peaks. The ­TChkl for samples Z-0 and Z-3 40
are shown in Fig. 8. According to the results, (002) appears 20 460 480 500 520 540 560

to be the most preferred orientation for both ­Cd1−xZnxS and Wavelength (nm.)

CdS samples investigated. 300 400 500 600 700 800

The structural changes in the ­Cd1−xZnxS samples with Wavelength (nm.)
introduction of Zn can cause changes in the optical trans-
mittance of the fabricated ­Cd1−xZnxS samples, as observed Fig. 9  Optical transmittance spectra of the fabricated C
­ d1−xZnxS sam-
in Fig. 9. It is clearly seen that the transmittance properties ples. Inset: the partial enlarged pattern ranging from 460 to 560 nm

13
Optical, structural and photo electrochemical properties of ­Cd1−xZnxS films grown…
4 Conclusions
Cd1−xZnxS thin films of hexagonal structure with high effec-
tive surface area were grown using the low-cost chemical
bath deposition technique at a bath temperature of 80 °C.
­Cd1−xZnxS causes a blue shift in absorption resulting the
optical band gap to vary from 2.33 to 2.50 eV as composi-
tion parameter changes from x = 0.0 to x = 0.5. The films
fabricated with the composition of x = 0.3 showed the best
ISC and VOC values compared to other investigated samples
due to enhanced carrier concentration and Eg, respectively.
Moreover, ­Cd1−xZnxS thin films fabricated with the compo-
sition of x = 0.3 were found to exemplify the higher Vfb and
ISCP. From the results, it can be concluded that the optoelec-
tronic properties of CdS can be effectively improved with
introduction of Zn to the reaction solution.
Acknowledgements  The authors would like to acknowledge National
Science Foundation (RG/12/BS/03) of Sri Lanka, Sivananthan Labo-
ratories, Inc., Bolingbrook, Illinois, USA and Postgraduate Institute of
Science, University of Peradeniya, Sri Lanka, for the financial assis-
tance. Prof. S. Sivananthan of University of Illinois at Chicago, USA,
Prof. M.A.K.L. Dissanayake of National Institute of Fundamental Stud-
ies, Hanthana, Sri Lanka, is acknowledged for his valuable suggestions,
support and guidance. Part of the research was performed using the
Environmental Molecular Sciences Laboratory (EMSL), a national
scientific user facility sponsored by the US Department of Energy’s
Office of Biological and Environmental Research, and located at Pacific
Northwest National Laboratory (PNNL).
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