Accepted Manuscript

A facile route for synthesis of cadmium sulfide thin films

A. El Kissani, H. Ait Dads, S. Oucharrou, F. Walatta, H. Elaakib,

L. Nkhaili, A. Narjis, A. Khalfi, K. El Assail, A. Outzourhit

PII: S0040-6090(18)30565-0
DOI: doi:10.1016/j.tsf.2018.08.034
Reference: TSF 36844
To appear in: Thin Solid Films
Received date: 5 March 2018
Revised date: 22 August 2018
Accepted date: 23 August 2018

Please cite this article as: A. El Kissani, H. Ait Dads, S. Oucharrou, F. Walatta, H. Elaakib,
L. Nkhaili, A. Narjis, A. Khalfi, K. El Assail, A. Outzourhit , A facile route for synthesis
of cadmium sulfide thin films. Tsf (2018), doi:10.1016/j.tsf.2018.08.034

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A facile route for synthesis of cadmium sulfide thin films

A. El kissani*,H. Ait dads, S. Oucharrou, F. Walatta, H. Elaakib, L. Nkhaili, A. Narjis, A.

Khalfi, K. El assail, A. Outzourhit

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Nanomaterials for Energy and Environment Laboratory, Cadi Ayyad University, PB 2390,

Marrakech, Morocco

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*
E-mail: [email protected]

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ABSTRACT

This study describes a facile spin-coating deposition technique for cadmium sulfide thin

film. The structural analysis revealed the formation of a pure hexagonal cadmium sulfide

phase. The lattice constant, the crystallite size, dislocation density and micro strain were

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calculated. Energy dispersive x-ray analysis confirmed that these as-prepared CdS thin films

are stoichiometric. The surface morphology studies showed homogenous and uniform films

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without any cracks with a low surface roughness of value 9 nm. The optical analysis

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indicated a relatively high transmission, optical band gap of 2.4 eV and Urbach energy value
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of 0.48 eV. All these properties indicate that cadmium sulfide thin films prepared by this

simple route can be used as a window in heterojunction photovoltaic solar cells.

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Keywords: Cadmium sulfide; Spin-coating; Structural properties; Optical properties

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1. Introduction

Cadmium sulfide (CdS) is considered as one of the most widely used II-VI

semiconductors in applications such as n-type windows for CdTe, CuIn(Ga)Se2 and

Cu2ZnSnS4 thin film solar cells [1-3], light emitting diodes [4] and thin film transistors [5].

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Indeed, CdS has a direct band gap of about 2.42 eV to 2.5 eV at room temperature. CdS

possesses two crystalline forms: hexagonal (wurtzite) phase and cubic (zinc blende) phase,

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and it is possible to grow CdS films in both these phases [6]. There are several reports on the

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methods of synthesizing CdS thin film such as evaporation [7], sputtering [8], metal organic
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chemical vapor deposition [9], chemical bath deposition [10,11], spray pyrolysis [12],

electro-deposition [13] and sol gel [14,15,16]. The chemical bath deposition CBD is one of
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the widely used techniques. However, this method requires heating the solutions and a

precise temperature control.

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The present study investigates a facile spin-coating technique for the synthesis of CdS thin
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films. The advantages of this technique are: simplicity, safety, non-vacuum, low-cost and
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low working temperature. In addition, this method can be easily scaled up for large-area thin
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films of the same family. The structural, chemical analysis, morphological, optical and

conductivity type of the prepared films was investigated.

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2. Experimental procedure

2.1 Materials

Reagent-grade cadmium chloride (CdCl2, 99 % purity), thiourea (SC(NH2)2, 99 % purity)

and methanol CH3OH were purchased from Sigma-Aldrich (Steinheim, Germany) and used

for the preparation of the CdS precursor solution.

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2.2 The CdS film deposition

The cadmium sulfide CdS thin films were prepared by dissolving cadmium chloride

(CdCl2, 0.1M) and thiourea (CH4N2S, 0.1 M) in methanol (CH3OH) in the presence of 1 mL

of water. The solution was stirred at room temperature for 15 minutes until a clear,

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transparent and homogeneous mixture was obtained. A few drops of the as-prepared clear

precursor solution were then deposited by spin-coating technique on a cleaned soda lime

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glass substrate at 2200 rpm for 60 s. The clear films were subsequently baked on a hot plate

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at 200 °C in air for 10 min and their color changed to yellow, which is typical of CdS films.
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The procedure was repeated five times to obtain a thickness of approximately 250 nm of the

film.
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2.3 Characterization of the CdS thin films

The structure of the obtained CdS thin films were characterized by X-Ray diffraction
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(XRD) using Cu Kα radiation (λ= 1.5418 Å) and X’Pert diffractometer (PANalytical, Almelo,
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The Netherlands). The morphological analysis was investigated using atomic force
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microscopy (AFM) (FlexAFM, Nanosurf, Switzerland) and a Tescan Vega 3 scanning

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electron microscopy (SEM) (Tescan Orsay, France). The compositional analysis was

performed by energy dispersive X-ray (EDX) using an EDAX detector attached to the SEM
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equipment. Optical characterization was carried out using an UVPC ultraviolet-visible-near

IR double beam spectrophotometer (Shimadzu, Tokyo, Japan) by recording the transmission

spectra of the thin films in the wavelength range of 200 nm to 2000 nm. The conductivity

type of the CdS thin film was determined by the hot probe method.

3. Results and discussions

3.1 X-ray analysis

Fig. 1 shows the X-ray diffraction of a typical as-prepared cadmium sulfide CdS thin film,
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which reveals that the deposited CdS thin film is polycrystalline. All the observed peaks can

be attributed to lattice planes of the stable hexagonal phase (JCPDS: 41-1049). No impurity

peaks were observed, indicating the high quality of the CdS thin films deposited by this

simple technique. In order to have information about the crystallinity levels, the lattice

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parameters (a, b, c), the full width at half maximum (FWHM, β), the crystallite sizes (D),

interplanar spacing (dhkl), the dislocation density (δ) and the micro strain (ε) were calculated.

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The lattice parameters (a, b, c) were calculated by equations:

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2
a=b = d100
√3
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c = 2d002
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where d100 and d002 are the interplanar spacing, corresponding to the (100) and (002) planes.

These were obtained using Bragg formula;

dhkl = λ/2sinθhkl
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where θhkl is the Bragg angle corresponding to the (hkl) plane, λ is the wavelength of X-ray.
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The calculated lattice parameters and the ratio (c/2a) for CdS thin film are presented in

Table 1. The values of the lattice parameters are in good agreement with the standard values
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from the JCPDS n° 41-1049 data file. The ratio c/2a is found to be 0.81 for the as-prepared
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CdS thin films, suggesting that the unit cell is hexagonal. In comparison with the cubic phase,

the hexagonal phase of CdS thin film is more suitable n-type window for thin films for solar

cell, because of its higher transmission and a good electrical conductivity [17].

The crystallite size (D) is calculated using Scherrer’s equation [18,19],

kλ
D=
βcosθ

where k = 0.9 is the shape factor, λ is wavelength of X-ray in nm, β is the full width at half
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maximum (FWHM) of the peak in radians and θ is Bragg angle of the related peak. The

estimated value of the crystallite size D is shown Table 2 and is on the average 29 nm. In

addition to the interplanar distances (dhkl), the dislocation density (δ) and micro strain (ε)

were calculated for the different peaks (hkl) planes of CdS thin film using the following

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formulas [20]:

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δ=
D2

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βcos θ
ε= NU4

The calculated d-spacing, dislocation density and micro strain of the CdS thin films are also

given in Table 2. It can be seen that the observed d-spacing values are in good agreement
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with the JCPDS powder diffraction data for the hexagonal CdS phase. The average

dislocation and micro strain was respectively about 1.2 1015 lines/m2 and 1.2 10-3, which are
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in good agreement with the reported values for CdS films [11,21]. All of these structural
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parameters confirmed the good crystallinity of the CdS films fabricated by this facile route.
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3.2 Morphological characterization

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The surface morphology of the CdS thin film was studied using scanning electron

microscopy (SEM) and atomic force microscopy (AFM). Fig. 2 (a) and (b) shows the SEM
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and AFM images of spin-coated CdS thin film respectively. The results show that the surface

of CdS thin films is uniform, dense and homogeneous without any cracks or pinholes and

with a relatively narrow grain distribution. The average roughness is on the order of 9 nm,

which is very low compared to the grain size.

3.3Composition analysis

The chemical composition of CdS thin films was investigated by using energy dispersive

X-ray analysis (EDX) measurements. This analysis was performed at different spots, in
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order to have an accurate chemical composition and to check it uniformity. Fig. 3 shows the

EDX spectrum of CdS thin films. It shows that the films contain the elements Cd and S. The

presence of other elements Si, O, Na, Ca, Mg and Al is due to the soda lime glass substrates

on which the films were deposited. The atomic percentage of Cd and S were estimated from

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the EDX results, as shown in Table 3. The EDX analysis reveals that the Cd:S ratio for the

as-prepared CdS thin films is about one, which indicates the formation of the high-quality

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and stoichiometric CdS films.

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3.4 Optical characterization NU
Fig. 4 shows the optical transmittance spectrum of the as-prepared cadmium sulfide

(CdS) thin film. From this figure, it can be seen that the films exhibit a high transmittance in
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the visible and near-infrared regions. The transmittance of CdS decreases rapidly for

wavelengths below 500 nm. It should be mentioned that high transmittance in the visible
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region is one of the key features for window films in hetero-junction solar cells. The
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absorption coefficient (α) was calculated from transmittance spectra in the strong absorption
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region using the following equation:

ln(100⁄T)
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α=
e
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where ‘T’ is the transmittance and e = 250 nm is the thickness of the film. Fig. 5 shows the

variation of absorption coefficient (α) of the CdS thin film with wavelength. For

wavelengths lower than 500 nm, the CdS films possess a larger absorption coefficient.

However, α is lower for wavelengths higher than 500 nm. The high transmittance and low

absorption coefficient obtained for these CdS thin films in the wavelength region above 500

nm make them suitable for window layers in solar cell.

Since CdS is a direct band gap material, the band gap value Eg of the CdS thin film was
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obtained by extrapolating the linear portion of (αhν)2 vs. photon energy (hν) plot to α = 0 as

shown in the inset of fig. 5. The obtained value of Eg is 2.4 eV, which is in good agreement

with the experimental values reported by other researchers [20,22,23]. Furthermore, the sub

band gap absorption coefficient is related to transition between band tails and increases

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exponentially with the photon energy according to the Urbach relation [18],

hν

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α = α0 exp( )
EU

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where α0 is a constant, hν is the photon energy and EU is the Urbach energy related to the

width of tails of the local states in the band gap. It’s noted that the Urbach energy depends on
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the structural defects, dislocation density and impurities. Fig. 6 illustrates the plot of ln(α)
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versus photon energy (hν). EU is thus found to be 0.48 eV from the reciprocal of the slope of

linear portion. This value is lower than that found by other authors [20,24,25], indicating a

lower structural disorder and improved stoichiometry of the as-prepared CdS thin films.
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3.5 Conductivity type

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The type of conductivity of the CdS thin films was determined using hot-probe method. It

was found that the prepared CdS thin films are n-type semiconductors.
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4. Conclusion
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In short, good quality, adherent and uniform cadmium sulfide thin films were

successfully prepared by a facile synthesis route at lower temperatures, using spin coating

technique, without sulfurisation and without any harmful chemicals reagents. The x-ray

diffraction studies revealed a pure hexagonal CdS phase. The crystallite size of CdS thin

films calculated by Scherer relationship was found to be on the order of 29 nm. The analysis

of CdS thin films by SEM and AFM showed uniform and dense films without cracks or

pinholes. The band gap energy and Urbach energy of CdS thin films are respectively 2.4 eV
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and 0.48 eV. The EDX analysis confirms that the CdS thin film is stoichiometric with no

impurities. All these properties indicate that the CdS thin films prepared by this simple route

can be used as a window in heterojunction photovoltaic solar cell.

Acknowledgements

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This research did not receive any specific grant from funding agencies in the public,

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commercial, or not-for-profit sectors.

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Figure Captions
Fig. 1 X-ray diffraction patterns of cadmium sulfide thin film. Reference JCPDS

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card number 41-1049 is also shown for comparison.

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Fig. 2 (a) Scanning electron microscopic images of cadmium sulfide thin film.

(b) Atomic force micrographs of cadmium sulfide thin film, deposited onto soda
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lime glass by spin-coating technique.
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Fig. 3 EDAX spectrum for CdS thin film deposited on soda lime glass substrate.

Fig. 4 Transmittance spectra of cadmium sulfide thin film deposited on soda lime

glass substrate.
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Fig. 5 The absorption coefficients as a function of wavelength of a CdS thin film.

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The inset shows variation of a tauc plot of (αhν)2 versus photon energy (hν).

Fig. 6 The plot of Ln(α) versus photon energy (hν) for CdS thin film.
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Table Captions

Table 1 The lattice parameters (a, b, c) and the ratio c/2a of cadmium sulfide thin film

Table 2 The values of full width at half maximum (FWHM), crystallite size (D),

interplanar spacing (dhkl), dislocation density (δ) and micro strain (ε) of the cadmium

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sulfide (CdS) films

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Table 3 EDAX elemental analysis of cadmium sulfide thin film

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Table 1. The lattice parameters (a, b, c) and the ratio c/2a of cadmium sulfide thin film
Lattice parameters (Å) a=b c c/2a
CdS 4.13 6.71 0.81
JCPDS: 41-1049 4.14 6.71 0.81

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Table 2. The values of full width at half maximum (FWHM), crystallite size (D),
interplanar spacing (dhkl), dislocation density (δ) and micro strain (ε) of the cadmium
sulfide (CdS) films
2 ( F D d d δ ε
15
θ h W ( h JCP (10 (

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h k H n k DS lines/ 1
k l M m l 41- m2) 0

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-
l ) ( ) 104
3
( d X 9(n

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d e R m) )
e g D
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g ) (
) n
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m
)
2 ( 0 3 0 0.3 0.850 1
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4 1 . 4 , 586 .
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. 0 2 , 3 0
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8 0 3 2 5 1
7 ) 7 9 8
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2 ( 0 3 0 0.3 0.997 1
6 0 . 1 , 359 .
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. 0 2 , 3 0
5 2 5 9 3 9
7 ) 6 0 5
2 ( 0 3 0 0.3 1.097 1
8 1 . 0 , 163 .
. 0 2 , 3 1
2 1 7 1 1 5
6 ) 1 8 6
4 ( 0 2 0 0.2 1.336 1
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3 1 . 7 , 070 .
. 1 3 , 2 2
8 0 1 3 0 7
0 ) 3 6 7
4 ( 0 2 0 0.1 1.319 1

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7 1 . 7 , 899 .
. 0 3 , 1 2

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9 3 1 5 8 6
6 ) 6 3 9

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5 ( 0 2 0 0.1 1.667 1
1 1 . 4 , 762 .
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. 1 3 , 1 4
9 2 6 4 7 2
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3 ) 1 9 6
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Table 3. EDAX elemental analysis of cadmium sulfide thin film

Compound Element Atomic Ratio
% Cd/S
CdS S K 49.66 1.01
Cd L 50.34

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Highlights

 CdS thin films were spin coated on glass from methanolic CdCl2-thiourea complex.
 As-prepared films crystallize in the hexagonal wurtzite structure.
 Optical properties of the filmssuitable for window layers.
 Processing temperature lower than in other CdS deposition methods.

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Figure 1
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