Optical Materials 117 (2021) 111212

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Optical Materials
journal homepage: www.elsevier.com/locate/optmat

Research Article

Influence of Cu doping on structure, morphology and optical characteristics

of SnO2 thin films prepared by chemical bath deposition technique
Sabah Ibrahim Abbas a, **, Saba Farhan Hathot b, Awatif Sami Abbas a, d, A.A. Salim c, *
a
Department of Medical Physics, College of Science, Al-Karkh University of Science, Baghdad, 10011, Iraq
b
Department of Physics, College of Science, Wasit University, Kut, 52001, Iraq
c
Laser Center & Physics Department, Faculty of Science, Universiti Teknologi Malaysia, Johor Bahru, Johor, Malaysia
d
Department of Geophysics Science, College of Remote Sensing &Geophysics, Al-Karkh University of Science, Baghdad, 10011, Iraq

A R T I C L E I N F O A B S T R A C T

Keywords: This paper reports various properties of four Cu-doped SnO2 thin films (hereafter called CuSnO-TFs) synthesized
SnO2 thin film on glass substrate at temperature 80 ◦ C via the standard chemical bath deposition method. The as-deposited films
Cu doping were annealed at 400 ◦ C for 1 h. The as-prepared samples were characterized at room temperature using
Chemical bath deposition
different analytical tools to determine the effects of varying Cu doping contents (0–3 wt%) on their structures,
Transmittance
Structure and optical traits
morphologies, and optical characteristics. The XRD analyses of the studied CuSnO-TFs showed their body-
centered tetragonal structures in rutile phase with high purity and good polycrystallinity. The average crystal­
lite size was increased from 17.6 to 34.52 nm with the increase of Cu contents from 0 to 3%, respectively. The
SEM images of the grown films revealed agglomerated morphologies with the nucleation of spherical clusters or
granules. Both visible transmittance and optical band gap energies of the films were decreased with the increase
of Cu levels. In addition, the values of the refractive index, extinction coefficient, and dielectric constant of the
deposited films were gradually increased and shifted towards higher wavelengths with the increase of Cu doping
proportion. It was shown that by tuning the Cu contents overall properties of the proposed SnO2 thin films can be
customized which are desired for diverse functional applications.

1. Introduction Amongst all these TCOs, the optical and structural properties of the
Cu-doped SnO2 thin films have been highly focused owing to their
In recent times, transparent conductive oxides have generated distinct characteristics such as high transparency, high electrical con­
intense research interests due to their diverse applications feasibility in ductivity, and strong stability at high temperature [5–8]. Interestingly,
the fields of optoelectronics, automotive and aircraft windows, solar these TCOs in the parent phase have n-type electrical conductivity with a
cells, and anti-reflective coatings [1,2]. Different metal oxide semi­ high concentration of charge carriers (electrons). Besides, these thin
conductors including ZnO, SnO2, In2O3, and CdO have commonly been films with impurities doping when deposited under appropriate condi­
used in the organic optoelectronic devices because of their unique op­ tions become visually transparent with improved electrical conductivity
tical transparency (very high) and electric resistivity (very low) [3]. One [9]. In fact, SnO2 has high melting point transmission does not easily
of the most important types in this category is the transparent con­ react with oxygen and water vapor [8,9], thus offering great potential
ducting oxides (TCOs) semiconductors. These oxides are advantageous for the fabrication of efficient gas sensors, optical, and electrical devices
for combining two important qualities namely their high optical trans­ [8]. In addition to high electrical conductivity and large band gap en­
mittance (transparency to the visible light) and high electrical conduc­ ergy (3.3 eV), both high visible transmittance and reflectance in the
tivity [4]. Therefore, such oxides have intensively been studied for both infrared region at room temperature make SnO2 a prospective candidate
theoretical and applied purposes to achieve better coating materials for for the applications in blue, violet, and ultraviolet light-emitting diodes
the windows, audio waves, thermal mirrors, and various other appli­ (LEDs) and laser diodes (LDs) [10].
cations [5]. Researches revealed that different properties of thin films of various

* Corresponding author.
** Corresponding author.
E-mail addresses: [email protected] (S.I. Abbas), [email protected] (S.F. Hathot), [email protected] (A.A. Salim).

https://doi.org/10.1016/j.optmat.2021.111212
Received 8 April 2021; Received in revised form 3 May 2021; Accepted 13 May 2021
Available online 27 May 2021
0925-3467/© 2021 Elsevier B.V. All rights reserved.
S.I. Abbas et al. Optical Materials 117 (2021) 111212

materials are very much dependent on the synthesis methods [8–11]. examined via the X-ray diffractometer (XRD, SHIMADZUs-6000) with
Depending on the types of materials and specific properties for appli­ Cu Kα1 radiation of wavelength 1.5406 Å. The surface morphology of
cations, several techniques have been introduced to achieve diverse the deposited TFs was recorded using the 2D scanning electron micro­
types of films. These approaches include the spray pyrolysis, chemical scopy (SEM), model Tescan, VegaIII with resolution 1 μm.
vapor deposition, thermal evaporation processes, laser deposition by the
pulsed lasers, chemical bath deposition, and others [7,12]. The existing 3. Results and discussion
preparation techniques for the thin films are classified according to the
medium sedimentation, where the deposition of films is performed from 3.1. XRD analysis
the liquid media (such as the thermo-chemical decomposition).
Conversely, in the physical growth process, the deposition is carried out Fig. 1 illustrates the XRD patterns of all samples which consisted of
from the gaseous media (steam) via atomization or vacuum evaporation several significant peaks, indicating the polycrystalline structures of the
[12]. Amongst all the growth techniques of thin films, the deposition deposited films. The obtained crystal structures of the prepared thin
route is preferred due to its various notable benefits such as the films were compared with the American Standard for Testing Materials
simplicity of the processing steps, accuracy, and low cost. On top, it uses (ASTM) card number and showed a good match. The patterns revealed
cheaper precursors that affect the formation of nanosized and homo­ sharp diffraction peaks at 26.12◦ , 32.44◦ , and 51.70◦ corresponding to
geneity of the films. Roy S. S. et al., have studied the pure and copper the lattice planer orientation of (110), (101) and (211) for the body-
doped with different concentrations from (1 up to 8 wt%) SnO2 nano­ centered tetragonal structures of SnO2 (in rutile phase) which tallied
crystalline thin films with large specific surface areas fabricated by with the JCPDS card number 72–1147 of the standard pattern [17]. The
chemical bath deposition technique [13]. It is observed that the high major diffraction peak of (110) in the case of doped samples (Cu 1, 2,
crystalline peak for SnO2 decreases while Cu increases with the increase and 3 wt%) shifts slightly towards the smaller diffraction angle as
of the Cu doping, the band gap increases with the increase of Cu con­ compared to pure SnO2 [17]. The peaks appeared at 38.24◦ corre­
centration. It was also observed that refractive index increases for higher sponded to the lattice plane of (111) for the monoclinic tenorite phase of
Cu concentrations which may be due to the increase of inhomogeneity CuO structure along with the tin dioxide peaks according to the JCPDS
and surface roughness of the films [13]. S. S. Roy 1 and J. Podder. [14], card number 94.00384821 [18]. The XRD peak intensities of the sam­
have worked on the pure and Cu doped tin oxide thin films are prepared ples were increased with the increase of Cu contents which were due to
by spray pyrolysis technique from SnCl2 precursor. Where X-ray the higher polycrystallinity. Mishra, R. K., and his co-authors stated that
diffraction (XRD) patterns of SnO2 films showed the polycrystalline the crystallite size of Cu doping SnO2 nanoparticles was effected on the
nature of the films with preferential orientation along the (101) planes structural, photoluminescence and formaldehyde sensing properties.
that a reason for the band gap shifting into lower energies and then While, Vadivel, S. et al., have specified the pure and copper doped with
increased with further increasing of Cu doping concentrations. Along, it different doping concentrations (0, 1, 5, and 10 wt%) of SnO2 nano­
is observed that the refractive index increases further for higher doping crystalline thin films. It is clearly observed by XRD spectra, the crys­
of Cu. Despite many studies, the synthesis of high-quality Cu-doped tallinity of SnO2 decreases as the Cu doping concentration increases. The
SnO2 thin films with customized properties remains challenging [14, decrease in crystallinity is due to the fact that Cu incorporation in the
15]. host SnO2 system allows for more nucleation sites, which inhibits crystal
Considering the fundamental and applied interests of Cu-doped SnO2 grain formation, resulting in an increase in lattice strain [17]. Along
thin films (CuSnO-TFs), we prepared such samples on glass substrate with our current report, the peaks of (110) and (101) were used to
using the versatile chemical bath deposition method. As-deposited thin measure the crystallite size of the samples. The crystallite size for 3% of
films were characterized at room temperature via different analytical Cu was 32.23 nm. This indicated the crystallite size decreases with the
instruments to examine the role of various Cu contents (0, 1, 2, and 3 wt increasing Cu doping concentration. It can be seen from Fig. 1, a
%) on their structure, morphology, and optical attributes. Results were decrease in the crystallite size when doping with 3%. The observed
analyzed, interpreted, discussed, compared, and reconciled with some decrease in the diffraction peak intensity at a higher Cu level (3 wt%)
existing state-of-the-art reports.

2. Experimental

Four Cu-doped SnO2 TFs were prepared of a clean glass substrate

using the chemical bath deposition technique. Depending on the dopant
contents 0, 1, 2, and 3 wt%, these samples were named as CuSnO-TF-
0 (undoped or pristine), CuSnO-TF-1, CuSnO-TF-2, and CuSnO-TF-3.
High purity analytical reagents of copper (II) dihydrate chloride
(CuCl2.2H2O) and tin (II) dihydrate chloride was used as Cu and Sn
sources, respectively. First, tin (II) dihydrate chloride was dissolved in
deionized water (0.1 M). Copper (II) chloride solution at 0, 1, 2, and 3 wt
% were used wherein the resultant solution was extracted for 15 min
without heating. Next, some drops of aqueous NH3H2O were added to
the resulting solution for 30 min at the temperature of 60 ◦ C under
constant stirring. During this process, the solution pH was frequently
checked and regulated to pH 9. Microscope glass slides with a dimension
of (76 mm × 26 mm × 1 mm) were used as substrates for the deposition
of the proposed thin films [16]. These substrates were placed vertically
in the reacting heat bath at 80 ◦ C. Thereafter, the deposited films were
dried in the air, washed by pure water, and then oven-dried for 1 h at
400 ◦ C before being kept in moisture free conditions for further char­
acterizations. The optical absorbance and transmittance of the samples
in the range of 300–1100 nm were measured using an ultraviolet spec­
trophotometer. The structures and phases of the CuSnO-TF were Fig. 1. XRD patterns of various CuSnO-TFs.

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S.I. Abbas et al. Optical Materials 117 (2021) 111212

was due to the occupation of Cu+2 in the lattice structure of Sn, leading film thickness was found to be approximately 150–185 nm. The pure
to the micro-strain mediated lattice distortion [19,20]. For instance, a (undoped) film (Fig. 2 (a)) did not show any definite morphology rather
film with 2% of Cu showed an increase in the peak intensity of (110), varies crystallite sizes regardless of the cubic structure. The thickness of
indicating that an improvement in the crystallinity of the sample and an the films was determined using a micro gravimetrical method. The films
increase in the crystallite size. This in turn reduced the average crys­ deposited on clean glass slides whose mass had previously been deter­
tallite sizes in the film [20]. The most intense (110) XRD peak was used mined [23]. After the deposition, each substrate itself is weighted again
to calculate the average crystallite size in the SnO2 thin films following to determine the quantity of deposited SnO2. Measuring the surface area
the Scherrer’s formula given by Ref. [20]: of the deposited film, taking account density of SnO2 of the film, the
thickness was determined using the relation. All the nanocrystallites
0.9λ
G= (1) showed a strong agglomeration tendency to form some randomly
β cos θ
distributed clusters. However, all the doped films (Fig. 2(b–d)) revealed
where G is the average grain size (nm), β is the full width at half the existence of spherical nanocrystallites with smaller sizes and random
maximum (FWHM) of the intense XRD peak located at Bragg’s diffrac­ distribution. Doped samples disclosed smaller granules in the form of
tion angle θ. Table 1 shows the average crystallite sizes for all samples clusters having normal sizes and random distributions. In addition, some
with their code and other crystal parameters. large crystallites with irregular sizes were nucleated without any cracks.
The values of distortion parameter (L) being a measure of the lattice These irregular sizes of the nanocrystallites with inhomogeneous dis­
strain was calculated via [21]: tribution were responsible for the development of lattice strain and
distortion.
β
L= (2)
tan θ
3.3. Optical characteristics
The interchain distance (m) and interplanar distance (p) of the lattice
yields:
The optical properties of semiconductors are significant for devices
5 λ fabrication where electronic transitions across the band gap plays a vital
m= (3)
8 sin θ role. In this work, the optical properties of the proposed CuSnO-TFs were
determined from the transmittance and absorbance spectral analyses.
λ The optical band gap energy for the direct electronic transitions was
p= (4)
2 sin θ estimated and the absorption coefficient was calculated. Later, all these
where d (hkl) is the distance between two adjacent crystal planes. The information were used to evaluate the extinction coefficient, refractive
strength of the X-ray aberration was calculated as a function of the index, and dielectric constant (both real and imaginary parts) of the
diffraction angle and the prevailing orientation of the samples. The CuSnO-TFs. The transmittance spectra of the pure thin film were grad­
deflection was used to determine the crystalline phase and structural ually decreased with the increase of Cu (Fig. 3) which was due to the Cu
properties of the obtained CuSnO-TFs. The film containing 3 wt% of Cu impurities-mediated generation of local levels within the forbidden
displayed the lowest value of the distortion parameter (lattice strain). energy gap. This in turn enhanced the absorbance and reduced the
The width of the major XRD peak was decreased with the increase of Cu transmittance of the films [24,25]. With the increase of film thickness,
contents, indicating the enlargement of the mean crystallite sizes which more photons were absorbed by the film which may be due to the
was attributed to the effects of quantum confinement. Both interplanar densification of the finer crystallites and large surface area. Conse­
and interchain distance in the SnO2 thin film was strongly affected by quently, it was difficult for light to penetrate the surface of these films
the Cu contents [22]. (decrease in light speed in a denser medium) as indicated by the increase
of refractive index with the increase of Cu contents [20].
The optical band gap energy (Eopt ) of the deposited CuSnO-TFs was
3.2. SEM images estimated (by assuming a direct transition between the valence and
conductive band edge) using the Tauc’s model [26]:
Fig. 2(a–d) displays the SEM images of the samples together with the /
α = B (hv − Eopt )r hv (5)
corresponding histogram distributions of the particle size (Fig. 2 (a1-
d1)), which consisted of inhomogeneous and agglomerated spherical
where B is a constant, α is the absorption coefficient, hv is the incident
nanocrystallites. The grain sizes obtained from the SEM image analysis
photon energy and r is the exponent that takes different values
were ranged from 50 nm to several hundreds of nanometers. In this
depending on the nature of interband transitions (where r = 2 and r = ½
estimation, over 100 particles were captured, then calculated using the
for the direct allowed and indirect allowed transitions, respectively. The
Image Processing and analyzed by Java Software (ImageJ software). The
absorption coefficient (α) was calculated in terms of the thickness (t) and
software individually analyzed the optimum images of the grains and
absorbance (A) of the film using [27]:
calculated the average particle size as well as their distribution [2]. The
A
α = 2.303 (6)
Table 1 t
Copper contents-dependent variation in the average crystalline size, interchain Fig. 4 shows the Tauc’s plot for the evaluation of the optical band gap
distance and distortion parameter (Lattice strain) of the deposited films. energies of the deposited films. The intercept of the linear part of each
Samples Mean Interplanar Interchain Lattice Strain plot on the horizontal axis provided the value of the optical band gap
Crystallite Size Distance Distance (%) energy. The value of Eopt for the pure thin film was highest (3.72 eV.
(nm) (Å) (Å)
However, the values of Eopt for the doped films were decreased from
CuSnO- 17.62 3.44 4.24 3.72 2.90 to 2.55 eV with the increase of doping contents from 1% to 3%,
TFs-0
respectively. This observation was ascribed to the attainment of a high
CuSnO- 32.61 3.32 4.21 1.98
TFs-1 density of the local impurity levels formed by the agglomerated atoms in
CuSnO- 33.15 3.35 4.20 1.88 the forbidden energy gap region [13]. In addition, an increase of carrier
TFs-2 concentration in the doped thin film led to the up-shift of the Fermi level
CuSnO- 32.23 3.29 4.18 2.05 into the conduction band [28].
TFs-3
The refractive index (n) of the deposited films in terms of their

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S.I. Abbas et al. Optical Materials 117 (2021) 111212

Fig. 2. SEM images of (a) CuSnO-TFs-0, (b) CuSnO-TFs-1, (c) CuSnO-TFs-2 and (d) CuSnO-TFs-3 (corresponded images (a1-d1): Histograms of particle size
distributions).

reflectivity (R) was calculated using the Lorentz-Lorenz equation given

αλ
by Ref. [28]. k0 = (8)
4π
/
R = (n − 1)2 (n + 1)2 (7) The values of k0 were increased with the increase of Cu doping
Fig. 5 displays the variation of the refractive index values of the films contents which was due to the increase in the absorption coefficient (Eq.
as a function of wavelength. The values of refractive indices were (6)). This increase in the values of k0 was mainly due to the enhanced
increased with the increase of Cu contents which was consistent with the surface roughness-assisted scattering in the films [29].
transmittance results. In addition, the nature of the refractive index Figs. 7 and 8 illustrate the doping contents-dependent variations in
variation was almost similar to the changes in the reflectivity of the the values of the corresponding real part (ϵ1) and imaginary part (ϵ2) of
films. The increase of the refractive index of the films with the increase the dielectric constant of the prepared films. The value of real and
of Cu contents may be due to the increase in the polarization, indicating imaginary part of the dielectric constant as a function of the photon
a direct correlation between the refractive index and polarizability of energy of the prepared films were estimated using the relations:
the films [13,29]. ε1 = n2ο − Kο2 (9)
Fig. 6 shows the extinction coefficient values of the films as a func­
tion of wavelength. The extinction coefficient (k0 ) of the films was ε2 = 2nο Kο 10)
calculated using the expression [30]:

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S.I. Abbas et al. Optical Materials 117 (2021) 111212

Fig. 3. Transmittance spectra of the deposited CuSnO-TFs. Fig. 5. Doping contents-dependent variation in the values of refractive indices
of the prepared films.

Fig. 4. Tauc’s plot for the evaluation of the optical band gap energies of the
deposited films. Fig. 6. Doping contents-dependent variations in the values of extinction coef­
ficient of the prepared films.
The real part of the dielectric constant showed a similar trend as that
of the refractive index of the films. Furthermore, the imaginary part of
the dielectric constant showed a similar trend as that of the extinction
coefficient of the films. This similar nature of the variation confirmed
the existence of a strong correlation between refractive index and real
part of the dielectric constant as well as extinction coefficient and
imaginary part of the dielectric constant of the deposited films [31]. The
values of the imaginary and real part of the dielectric constant strongly
depended on the polycrystalline structure, grain size distributions, sur­
face roughness, and thickness of the films [32]. The increase in ε2 with
concentration is due to the films becoming increasingly absorbers at
high concentrations, resulting in a high coefficient extinction and, as a
result, the imaginary portion of the dielectric constant reaching its
highest values [17–19]. The values of both refractive indices and real
part of the dielectric constant of the film doped with 3 wt% of Cu showed
rapid variation with wavelengths, indicating successful incorporation of
Cu into the SnO2 lattice structures [13,14,30–32]. This rise may be
attributed to the densification of films, since a denser material has a
higher refractive index and contains a larger number of particles [17].

5
S.I. Abbas et al. Optical Materials 117 (2021) 111212

Fig. 7. Doping contents-dependent variations in the values of the dielectric

constant (real part) of the prepared films.

4. Conclusion

Four Cu-doped SnO2 thin films were synthesized on glass substrate

using the chemical bath deposition technique and characterized using
various techniques. The concentrations of Cu were varied from 0 to 3%
to modify the structural, morphological, and optical traits of the grown
SnO2 thin films. The XRD analysis disclosed excellent polycrystalline
structures of the films and increasing crystallite size (from 17.6 to 32.23
nm) with the increase of Cu contents. The visible transmittance and
optical band gap energy of the pure or undoped film was higher (3.72
eV) compared to the doped films (varied from 2.90 to 2.55 eV). Irre­
spective of the Cu contents the deposited films showed agglomeration
Fig. 8. Doping contents-dependent variations in the values of the dielectric tendency where spherical particles with varying sizes were nucleated.
constant (imaginary part) of the prepared films. The values of refractive index, extinction coefficient, real and imaginary
parts of the dielectric constant of the proposed SnO2 thin films were
found to be sensitive on the Cu doping levels. It is established that the
structures, morphologies, and optical properties of the SnO2 thin films
can be tailored by adjusting the doping contents of Cu. Present results
may contribute towards the development of diverse devices based on
Cu-doped SnO2 thin films.

CRediT authorship contribution statement

Sabah Ibrahim Abbas: Writing – original draft, Formal analysis.

Saba Farhan Hathot: Investigation, Data curation, Validation. Awatif
Sami Abbas: Conceptualization. A.A. Salim: Supervision, Writing –
review & editing.

Declaration of competing interest

The authors declare that they have no known competing financial

interests or personal relationships that could have appeared to influence
the work reported in this paper.

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S.I. Abbas et al. Optical Materials 117 (2021) 111212

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S. Reddy, M. Poloju, Effect of Ti doping on structural, optical and electrical
properties of SnO2 transparent conducting thin films deposited by sol-gel spin
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Education Malaysia under grant no. MOHE FRGS/1/2019/STG02/ [16] H.A.A. Thjeel Al-Ogaili, R.A. Al-Wardy, S.I. Abbass, Affect the precipitation times
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versiti Teknologi Malaysia (RMC-UTM) for supporting under Post­ photoluminescence and formaldehyde sensing properties of SnO2 nanoparticles,
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