Ceramics International xxx (xxxx) xxx–xxx

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Ceramics International
journal homepage: www.elsevier.com/locate/ceramint

A comparative study of structural, optical and electrical properties of ZnS

thin films obtained by thermal evaporation and SILAR techniques
⁎
K. Priyaa, V.K. Ashitha, Gowrish K. Raoa, , Ganesh Sanjeevb
a
Department of Physics, Manipal Institute of Technology, Manipal University, Udupi, Karnataka 576104, India
b
Microtron Centre, Department of Studies in Physics, Mangalore University, Mangalagangotri, Mangalore, Karnataka 574199, India

A R T I C L E I N F O A BS T RAC T

Keywords: The paper compares structural, optical and electrical properties of ZnS thin films prepared by thermal
Thermal evaporation evaporation and SILAR techniques. Both techniques produced well-adherent films with uniform substrate
SILAR coverage. Films were found to be polycrystalline in both the cases. Crystallite size of the films was found to
Lattice parameter improve with thickness. Thermal evaporated films were found to possess comparatively better electrical
Quantum size effect
properties owing to their superior crystallanity. However optical absorption characteristics of both the films
were found to be similar. Detailed structural, optical and electrical studies reveal that the SILAR technique can
be an effective and economical alternative to thermal evaporation for optoelectronic applications.

1. Introduction substrate forming a thin film of the desired material [22].

In recent times, wide bandgap semiconductors are being exten-
sively studied due to their potential applications in optoelectronics.
Zinc sulphide belongs to II-VI group of compound semiconductors with
energy band gap of about 3.7 eV in the bulk form. This wide bandgap,
which is even greater than ZnO (3.4 eV) and GaN (3.4 eV), makes it
highly suitable for visible-blind ultraviolet photodetectors [1,2]. It also
has several other potential applications such as electroluminescence
devices [3], buffer layer for solar cells [4,5], energy conversion and
storage [6,7] etc.
ZnS thin films have been deposited by various physical and
chemical techniques such as sputtering [8,9], pulsed laser deposition
[10,11], electron beam evaporation [12], thermal evaporation [13,14],
chemical vapour deposition [15], dip coating [16], spray pyrolysis [17],
chemical bath deposition (CBD) [18,19], Successive Ionic Layer
Adsorption and Reaction (SILAR) [20,21], etc.
Among the physical methods, thermal evaporation technique is
known to produce uniform films with good adherence. Conventional
thermal evaporation technique (through resistive heating) involves
evaporation of the source material through a resistively heated boat
under very high vacuum. The source material usually dissociates into
vapour of constituent elements. The particles of this vapour will then
travel the distance between the boat and the substrate (kept directly
above the boat) without getting scattered. High vacuum is therefore
essential to maximize the mean free path of the vapour particles. Once
they reach the substrate, the particles will settle and get adsorbed to the
Although thermal evaporation can yield device quality films, the
technique is time consuming and expensive for large scale production.
Therefore, the commercial viability of the vacuum based manufacturing
techniques is limited. Besides, the new trend in solar cell technology is
to minimize the cost of production (with some compromise in conver-
sion efficiency) so as to make them affordable to everyone. To
accomplish this goal, less expensive, alternative techniques such as
chemical methods are being extensively studied. Successive ionic layer
adsorption and reaction (SILAR) is one such inexpensive chemical
technique which can produce uniform thin films on a large scale.
The SILAR technique is basically a refined version of the chemical
bath deposition. In SILAR, substrates are immersed alternatively in
anionic and cationic precursor solutions kept in separate beakers. The
segregation of precursors minimizes unwanted precipitation (and
hence wastage) of material. The thickness of the film is controlled by
the number of immersion cycles [23,24].
Vacuum deposition can yield films with relatively superior electrical
properties while SILAR technique has the advantage of inexpensive,
large scale production. Thus, a qualitative comparison between the two
methods is highly desirable to decide whether the commercial advan-
tage of SILAR is worthy of the comprise in the device quality of the
films.
In this paper, we have made an attempt to compare various
properties thermal evaporated and SILAR deposited ZnS films. This
comparison is unique and first attempt of this kind.

⁎
Corresponding author.
E-mail address: kgowrishrao@gmail.com (G.K. Rao).

http://dx.doi.org/10.1016/j.ceramint.2017.05.094
Received 7 April 2017; Received in revised form 12 May 2017; Accepted 12 May 2017
0272-8842/ © 2017 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Please cite this article as: K., P., Ceramics International (2017), http://dx.doi.org/10.1016/j.ceramint.2017.05.094
K. Priya et al. Ceramics International xxx (xxxx) xxx–xxx

2. Experimental procedure

2.1. Vacuum deposition by resistive heating

The glass substrates were immersed in chromic acid (for 24 h) to

etch the surface before deposition. The substrates were then rinsed
with distilled water and cleaned with acetone. ZnS pellets (99.99%
pure, from Sigma Aldrich) were resistively heated in a molybdenum
boat under a residual pressure of about 10−6 Torr. The substrate to
boat distance was kept at 16 cm. The thickness of films was varied by
taking the different amount of ZnS pellets.

2.2. SILAR

The SILAR deposition was carried out in the micro-controlled

HOLMARC™ SILAR deposition unit. The immersion time, stirring
speed, number of immersion cycles etc can be precisely controlled in
this automated SILAR deposition unit. The design and operation of the Fig. 1. Typical transmittance spectrum of ZnS thin films with thickness 550 nm.
unit has been described in one of our previously published paper [23].
Aqueous solutions of anionic (Na2S) and cationic (ZnCl2) precur- thickness of the films [25]. In this method, the interference fringes
sors were taken in separate beakers. Each deposition cycle involved obtained from the transmittance data were plotted against wavelength
following steps: of incident light in the ultraviolet and visible region. For the fringes in
(i) The glass substrate was immersed into the cationic precursor the region of medium and weak absorption, the refractive index is given
solution and stirred for about 40 s. The cations get adsorbed to the by the equation,
surface of the substrate. (ii) Substrate was then immersed in distilled
water to remove any loosely adsorbed ions. (iii) The substrate was 1
⎡ 1 ⎤2
immersed into the anionic precursor solution. Here the anions react n = ⎢N + ( N 2 − s 2 ) 2 ⎥
with the cations to form a thin layer of the material (iv) Finally, the ⎣ ⎦ (4)
substrate was rinsed again in distilled water. These four steps
where
constitute one complete immersion cycle. Repeating this cycle several
times, ZnS thin films of different thickness were obtained. TM − Tm s 2+1
The reactions involved in steps (i) and (iii) are given below: N = 2s +
TM Tm 2
ZnCl2 (Aqueous)→Zn2+ (Adsorbed)+2Cl− (In solution)
and s is the refractive index of the substrate (for glass s=1.5), TM is the
Na2S (Solid)+H2O→2Na++SH− (1) maxima of the interference fringe and Tm is the corresponding minima,
as shown in Fig. 1.
OH− (Insolution)+SH− (In solution)→S2− (In solution)+H2O Thickness of the film can be obtained from the formula

λ1λ 2
Zn2+ (In solution)+S2− (In solution)→ZnS (Adsorbed) (2) t=
2(λ1n 2 − λ 2n1) (5)
The ZnS films obtained from thermal evaporation and SILAR were
where n1 and n 2 are the refractive indices at two adjacent maxima at
then subjected to structural, optical and electrical characterization. X-
wavelengths λ1 and λ 2 . The thickness of the films was calculated using
ray diffraction patterns of the films were obtained by Rigaku Minflex X-
the Eq. (5). The thickness measured from the above two techniques
ray diffractometer (CuKα radiation, λ=1.54 Å). Zeiss scanning electron
were reconfirmed by the cross sectional SEM images of the films
microscope was used to study the surface features of the films.
(Fig. 2).
Elemental analysis was done using EDAX. Optical properties were
obtained from Shimadzu UV 1800 spectrophotometer. Electrical
properties of the films were studied by Hall Effect measurements at
room temperature.

3. Results and discussions

3.1. Thickness measurement

The film thickness was measured using three different techniques,

namely, gravimetric method, Swanepoel technique and cross section
SEM.
In the gravimetric method, thickness (t) of the thin films was
determined from the equation,
m 2 − m1
t=
Aρ (3)
where, m1 and m 2 are, respectively, the masses measured before and
after deposition. A is the area covered by the film and ρ is the density of
the film material (ZnS).
The Swanepoel method is an optical technique to measure the Fig. 2. Typical cross section SEM image of ZnS films of thickness 550 nm.

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Table 1
Structural properties of ZnS films deposited by thermal evaporation and SILAR.

Method of Thickness D (nm) from a (Å) S (×108)

Deposition (nm) Scherrer formula from N m−2
XRD

Thermal 330 19 5.28 14.9

Evaporation 440 29 5.30 20.5
550 32 5.33 24.3

SILAR 330 4.1 5.53 22.3

440 6.2 5.52 20.1
550 12.4 5.52 9.3

2dsinθ = nλ (6)

For cubic lattice, the lattice constant, a, is given by,

Fig. 3. Typical ZnS thin films deposited by (a) thermal evaporation, (b) SILAR.
3.2. Structural properties
The photographs of the ZnS films obtained by thermal evaporation
and SILAR techniques are shown in Fig. 3. The thermal evaporated
films were almost violet and SILAR deposited films were bluish white
in color. The visible color of the films indicates that the absorption edge
is in the ultraviolet region.
The XRD patterns of thermal evaporated and SILAR deposited ZnS
films are shown in Fig. 4. In both the cases, the films were found to be
polycrystalline with dominant cubic phase. Many other authors have
reported similar result [14,21]. The XRD patterns of thermal evapo-
rated films show a strong, single peak corresponding to (111) plane. On
the other hand, the XRD patterns of SILAR deposited films show three
peaks corresponding to (111), (220) and (311) planes.
The interplanar spacing, d, was calculated using Bragg's equation
[26],
a = d h2 + k 2 + l 2 (7)
where h, k, l are the Miller indices.
The values of a calculated for thermal evaporated and SILAR
deposited films are tabulated in Table 1. The lattice parameter obtained
for thermal evaporated ZnS films was close to 5.3 Å and that for SILAR
deposited films was about 5.5 Å, which agrees with earlier reported
values [9,27].
The position of prominent XRD peaks was found to shift as
thickness of the films increased. In the case of thermal evaporated
films, the 2θ value of (111) peak shifted from 29.24° to 28.94° with
increase in thickness. The same was from 27.4° to 27.62° for SILAR
deposited films. The XRD unit (Rigaku Minflex) used for this XRD
studies has an accuracy of 0.02° (in 2θ values). Since the observed shift
in 2θ values is more than 0.02° it can be safely concluded that the shift
arises from the changes in crystal structure of the films and not because
of the instrumental error. As a result of the shift in 2θ values, the lattice
constant also changed correspondingly. Maximum deviation in lattice
constant (from the standard value of 5.41 Å for bulk ZnS) was observed
in the films with least thickness. As the thickness increased, the lattice

Fig. 4. The XRD patterns of ZnS films (with different thickness) deposited by thermal evaporation (a to c) and SILAR (d to f).

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constant value approached the value of 5.41 Å which corresponds to

ZnS material in bulk form [28]. The variation of lattice constant value
can be caused by stress which can arise due to difference in thermal
expansion coefficients of the film and substrate material or due to
lattice mismatch between the substrate and the film [29,30]. The
intrinsic stress can be calculated from the equation [31].
(ao − a )Y
S=
2aoσ (8)

where ao and a are the lattice parameters in bulk and thin film form of
ZnS. Y is the Young's modulus=8.64×1010 N m−2 and σ is the Poisson's
ratio=0.428 for ZnS, respectively.
In the case of thermal evaporated films, the stress increased with
increase in film thickness (Table 1). This is in good agreement with
earlier reports [32,33] which claim that during vacuum deposition of
high melting point materials, the stress increases with film thickness.
On the contrary, stress in SILAR deposited films decreased with
increase in film thickness (Table 1) [34]. It should be noted that the
thermal evaporation process involves high temperatures. The vapour
atoms impinging on the substrates have high thermal energy. Besides,
once a thin layer of film is formed by thermal evaporation, the
continuation of deposition process (to increase the thickness) exposes
the already deposited bottom layer of the film to the heat radiated from
the evaporation boat. Therefore prolonged thermal deposition process
increases the stress. On the other hand, SILAR deposition takes place
at room temperature. Due to slow rate of SILAR deposition, both
substrate and the ions are almost at the same temperature. The low
thickness SILAR deposited films may have some stress arising because
of the formation of polycrystalline grains on amorphous substrates. But
as the thickness increases, the subsequent layers of film material will be
formed on the film layers which are already deposited on glass. Hence
the stress decreases.
The crystallite size D was calculated from the XRD patterns using
the Scherer formula:
0. 9λ
D=
βcosθ (9)
Fig. 6. The SEM image of ZnS films of thickness 550 nm deposited by (a) thermal
The variation of crystallite size with thickness is shown in Fig. 5. evaporation (b) SILAR.

It can be seen that, irrespective of the method with which the films
were grown, there was a significant increase in the crystallite size of the
films when the thickness is increased. This behavior is in accordance
with earlier reports [13,34,35,36]. When the film thickness is very low,
there will be a strong interaction between impinging atoms and the
substrate. But as the film thickness increases, the impinging atoms face
the previously settled layer of polycrystalline ZnS. Therefore, the
Fig. 5. Variation of crystallite size of thermal evaporated and SILAR deposited ZnS thin
films with thickness.
interaction between substrate and subsequent impinging atoms re-
duces as the thickness increases which results in better crystallinity
[22].
It can also be seen that thermally evaporated films possess better
crystallinity than SILAR deposited films, for a given thickness. This can
be attributed to higher surface mobility of the impinging atoms in the
case of thermal evaporation. The vapour atoms possess high thermal
energy and hence they have higher surface mobility upon impinging on
the substrate [22]. Since the SILAR deposition takes place at room
temperature the surface mobility of the adatoms is comparatively less.
The SEM images (Fig. 6) of the ZnS films revealed that all these
films have good substrate coverage. The films were pin hole free and
the grains were continuous unlike the work reported by Qi Liu et al.
[37] and Dhanya et al. [38]. The SEM images of the SILAR deposited
films show that the films are made up of nano-sized grains. However,
no such grains are visible in the same magnification (50 K) SEM image
of the thermal evaporated films. As mentioned earlier, the crystallite
size of SILAR deposited films (calculated from XRD) is less than that of
the thermal evaporated films. Hence the grains visible in the SEM
image of SILAR deposited must be composed of several smaller
crystallites. Such type of granular structure is common in films
obtained by chemical methods. The limited surface mobility of adatoms
in SILAR deposition results in the formation of localized groups of
small crystallites.
The chemical composition of the ZnS films was determined by
EDAX. A typical EDAX spectrum of the films is shown in Fig. 7. Both
thermal evaporated and SILAR deposited films were found to have

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Fig. 7. Typical EDAX spectrum of ZnS thin film.

Fig. 9. Typical I-V characteristics of ZnS thin film.
Table 2
EDS results of ZnS films prepared by thermal evaporation and SILAR. stoichiometric composition (Table 2). Different authors in the past
have reported that thermal evaporation technique yields non-stoichio-
Thickness (nm) Atomic ratio (Zn/S)
metric ZnS films,due to difference in the vapour pressure of Zn and S
Thermal evaporation SILAR atoms [8,30]. But, in the present work, the ZnS films obtained by
thermal evaporation technique were almost stoichiometric. Since the
330 1.10 0.99 SILAR technique does not involve the dissociation of ZnS, the
440 1.06 0.98
550 1.05 0.97
stoichiometry is maintained.

Fig. 8. The absorbance spectra of (a) thermal evaporated and (c) SILAR deposited films with corresponding Tauc plots (b and d).

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Table 3 less than that of SILAR deposited films.

Electrical properties of thermal evaporated and SILAR deposited ZnS thin films. Although the thermal evaporated ZnS films have superior electrical
properties when compared to SILAR deposited films, the optical
Method of Thickness Resistivity Carrier Carrier
Deposition (nm) (ohm-cm) Concentration Mobility absorbance of SILAR deposited films is relatively high. Hence, in the
(×1014 cm−3) (cm2 V−1 S−1) case of optoelectronic applications, SILAR deposition can still be a
competent alternative to thermal evaporation. The reduced conductiv-
Thermal 330 10.8 26 23
ity of SILAR deposited films is well compensated by higher absorption
Evaporati- 440 8.4 52 31.6
on 550 4.3 73 37.5 power and higher conversion efficiency.

SILAR 330 62.5 0.8 6.5 4. Conclusions

440 51.3 4.5 10
550 37.6 10 18.5
3.3. Optical properties
The absorbance spectrum of the ZnS films were obtained in the
wavelength range 300–800 nm as shown in Fig. 8. The absorption
coefficient α is given by the relation.
αhν = A(hν − Eg )n
where Eg is the energy gap, hν is the photon energy and A is a constant
depending upon the transition probability for direct transition. For
1 However, the SILAR deposited films were found to possess relatively
allowed, direct transitions n = 2 and for allowed indirect transitions
n = 2 . The band gap was determined by extrapolating the straight line
portion of the Tauc plots to energy axis at α = 0 .
It can be seen that ZnS films have high absorption in UV region.
The band gap value was found to be close to 3.5 eV as reported earlier
[39,40]. The values of band gap slightly deviate from the bulk value of
3.7 eV. The band gap of both thermal evaporated SILAR deposited
films decreased with increase in the thickness, as shown in Fig. 8(b)
and (d). The variation was close to 100 meV in case of thermally
evaporated films. This can be attributed to the fine grain structure of
the films [41,42,43]. In both thermal evaporation and SILAR deposi-
tion, the observed bandgap of the ZnS films is almost same. However,
since the SILAR deposited films have a granular structure they exhibit
relatively high absorption in UV region compared to thermal evapo-
rated films. The high absorption coefficient of SILAR deposited films
implies that they can absorb UV light more efficiently than the thermal
evaporated films and hence they can yield high opto-electric conversion
efficiency.
3.4. Electrical properties
In order to study the electrical properties of the ZnS films, silver
(Ag) ohmic contacts were deposited on top of the films by thermal
evaporation of 99.9% pure silver. The I-V characteristics of ZnS thin
films with Ag contacts (Fig. 9) was found to be linear, proving that the
contacts were ohmic.
Electrical resistivity (ρ), carrier mobility (µ) and carrier concentra-
tion (n) of the ZnS films were determined by Hall effect measurements
using Van der Pauw geometry [44] at room temperature.
The electrical resistivity of the films decreased with the increase of
thickness as shown in Table 3. As mentioned earlier, the films with very
low thickness have smaller crystallite size and hence larger grain
boundary region between them. The grain boundary region is the most
disordered region in the polycrystalline films. The defects arising in the
grain boundary regions act as carrier traps and produce a potential
barrier for the charge carriers [45,46]. Hence low thickness films are
more resistive with low free charge carrier density and mobility. As the
thickness of the films increases, the crystallite size also increases which
in turn reduces the grain boundary region. Hence thicker films show
increase in free charge carrier density and mobility [47]. The mobility
and the carrier concentration of the thermal evaporated films were
found to be several times greater than that of SILAR deposited films.
Correspondingly, the resistivity of the thermal evaporated films was
ZnS thin films of different thickness were deposited using thermal
evaporation and SILAR deposition techniques. The films obtained from
both the techniques were polycrystalline in nature and exhibited cubic
phase. Crystallite size improved with increase in thickness of the films
irrespective of the growth technique. However, the crystallite size of
thermal evaporated films was higher than that of SILAR deposited
films which can be attributed to the higher adatom mobility. The
bandgap of the films was found to be almost same (3.5 eV) in both the
(10) cases. Relatively superior crystal structure of the thermal evaporated
ZnS films enabled them to have higher charge carrier density, mobility
and electrical conductivity compared to SILAR deposited films.
high absorbance in UV region than thermal deposited films. Thus in
spite of the low electrical conductivity of the films, the SILAR
deposition technique can still prove to be an effective and inexpensive
alternative for optoelectronic device applications due to their higher
light absorption power and better opto-electric conversion efficiency.
Acknowledgement
The authors are thankful to DAE-BRNS, Govt. of India for funding
the above research work (sanction no: 34(1)/14/37/2014). The authors
are also thankful to the Manipal Institute of Technology, Manipal
University and the Microtron Centre, Mangalore University.
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