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ES Energy Environ., 2021, 12, 77-85
© Engineered Science Publisher LLC 2021 ES Energy Environ., 2021, 12, 77-85 | 77
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Fabrication and Characterization of ZnS based Photoelectrochemical Solar Cell Priyanka M. Mana, Pankaj K. Bhujbal and Habib M. Pathan*
Abstract
Zinc sulphide photoanode was prepared by a cost-effective and simple successive Ionic layer adsorption and reaction (SILAR) process on to a fluorine doped tin oxide (FTO) substrate for photoelectrochemical solar cell application. From the optical absorption spectrum, a bandgap of synthesized ZnS photoanode was obtained around 3.47-3.62 eV. The surface morphology of the deposited photoanode was characterized using field emission scanning electron microscopy (FESEM). The average thickness of the deposited film was found to be 2.25 µm. We have fabricated photoelectrochemical solar cells using low crystalline ZnS as photoanode material and Coumarin-343 (C-343) dye as a sensitizer. photoelectrochemical solar cells have been built and their photocurrent, open-circuit voltage, fill factor and efficiency has been measured under one sun. Nyquist plot and Bode plot were plotted using electron impedance spectroscopy (EIS). The effective parameters were found. The photovoltaic properties of the ZnS based photoelectrochemical solar cell were studied. The maximum efficiency of 0.1% was observed for ZnS based photoelectrochemical solar cells.
Keywords: Zinc sulphide (ZnS); SILAR; Photoelectrochemical solar cell; Electrochemical characterizations. Received: 6 August 2020; Accepted: 6 December 2020.
Article type: Research article.
1. Introduction
The era of innovations and discoveries in the field of Solar
cells began in the early 19th century when scientists observed
that the solar energy was directly converted to usable electric
energy. The necessity of large-scale solar electricity
production has become progressively crucial for the reasons
of energy security and climate change mitigation. Utilizing
solar energy for various needs has become easy by the
innovations in the field of solar technologies.[1] To date, solar
energy technologies can be classified into three stages of its
development such as the first generation based on single
crystalline semiconductors,[2] a second-generation based on
inorganic thin films[2], and a third-generation being
photovoltaic solar cells.[3] Semiconducting organic
macromolecules, inorganic nanoparticles, or hybrids play a
key role in third-generation solar cells which are indeed a
solution in the semiconductor industry for tackling the energy
crisis.[4] Compared to conventional silicon solar cells,
photoelectrochemical solar cells[5] are considered with low
fabrication cost and simple structures. Therefore, in the past
fabrication cost and simple structures. Therefore, in the past
two decades, a lot of researches has been reported in
improving photoelectrochemical solar cell efficiency, new
photo-anode materials, study of new electrolytes, and various
dyes for sensitization of the photo-anodes.[6-9]
Surface morphology,[10] band structure, photochemical
stability, and surface area[11] are some of the important factors
to be considered while selecting a photoanode for the
photoelectrochemical solar cell. Nano-sized TiO2 has have
been extensively studied as a photoanode for
photoelectrochemical solar cell because of its porous nature,
appropriate band structure for excitation of dye molecules, and
excellent photochemical stability.[12] Light-harvesting
efficiency of dye molecules[13] plays a vital role in the photo
conversion efficiency of photoelectrochemical solar cells.
High surface area of photoelectrode enables it for large uptake
of dye molecules and to make it for an effective harvest of
incoming light. Higher the light scattering better will be the
light harvesting of the dye molecules for a typical nano-porous
photo-anode.
In this study, we have introduced a metal chalcogenide
family[14] as a photoanode for photoelectrochemical solar cells.
ZnS is the material we have selected as a metal chalcogenide
photoanode for photoelectrochemical solar cell application. A
novel approach of replacing conventional metal oxide nano-
ES Energy & Environment DOI: https://dx.doi.org/10.30919/esee8c1021
Advanced Physics Laboratory, Department of Physics, Savitribai
Phule Pune University Pune-411007.
*Email: [email protected] (H. M. Pathan)
Research article ES Energy & Environment
78 | ES Energy Environ., 2021, 12, 77-85 © Engineered Science Publisher LLC 2021
Table 1. Physical properties of ZnS film.
Physical Properties
Parameters Reference
Energy Band gap (eV) 3.68 at 300K [23]
Density (g/cm3) 4.090
[22]
Refractive index 2.356
Electron mobility (cm2/V-s) 250
Thermal Expansion Coefficient
(μm/m°C) 6.36
Relative dielectric constant 8.9
porous photoanode with metal chalcogenide was done
effectively. For this demonstration, zinc sulfide (ZnS) is
selected as the photo-electrode as it is an important II-VI
semiconducting material, nontoxic, low-cost chemical and
better chemical stability. The important physical properties of
ZnS film are summarised in Table 1. The ZnS facilitates the
incident photons of high energy to arrive at the window-
absorber junction, improving the blue response of the
photovoltaic cells, which provides better performance of the
PEC cell. The position of the conduction and valance band of
ZnS is at -4.25 and -7.45 eV respectively. The highest
occupied molecular orbital (HOMO) and lowest unoccupied
molecular orbital (LUMO) levels of the Coumarin-343 (C-343)
dye are -5.7 and -3.11 eV respectively. The LUMO level
position and the ZnS conductive band are compatible. Since it
is suitable as a photoanode in PECs. Fig. 1 shows the band
diagram and electron transport mechanism of C343 sensitized
ZnS photoanode based DSSC.
Fig. 1 Band diagram & electron transport in C-343 ZnS
photoanode based PEC.
Various researchers have reported that ZnS thin films have
been deposited using different physical and chemical methods,
as pulsed laser deposition,[15] thermal evaporation,[16]
sputtering,[17] electrodeposition,[18] metal organic chemical
vapor deposition,[19] chemical bath deposition,[20] SILAR
(Successive Ionic Layer Adsorption and Reaction),[21] etc.
Among these techniques, the SILAR technique is simple and
economical. It is a unique method by which thin films of
compound semiconductors can be deposited by alternate
immersion of a substrate into solutions containing ions of each
precursor. We can easily control the growth of the film by
simply varying the deposition parameters.
In this report, optical studies were done for various SILAR
cycles and the Tauc plot was plotted. It was observed that as
the number of SILAR cycles increases the bandgap of ZnS
photoelectrode was found to be decreasing. FESEM
morphology of ZnS photoelectrode was showing a nano-
porous nature which seems good for a photoelectrochemical
solar cell photoanode. XRD pattern was showing alow
crystalline nature of ZnS thin films. Later-on increasing the
number of SILAR cycles the crystalline nature of thin films
may be observed. M. Ragam et al.[22] reported a ZnS based
photoelectrochemical solar cell with maximum solar
conversion efficiency (η) of the photoelectrochemical solar
cell with iodide electrolyte up to 0.016% with Methyl Blue
sensitizer and 0.099% with Eosin-Y dye.
2. Experimental section
2.1 Materials
Zinc nitrate hexahydrate and sodium sulfide were purchased
from Sigma Aldrich respectively. H2O was purified by
distillation and filtration. Pure double distilled water is used
for SILAR cycles. Liquid electrolyte (EL141) containing I-/I3-
redox couple were supplied by Dyesol Co. Fluorine-doped tin
oxide (FTO) glass (e14 ohm/square) was from Pilkington.
2.2 Experimental methods
2.2.1 Pre-cleaning of FTO and glass substrates
The pre-cleaning of FTO and Glass substrates was achieved
by sonicating it in soap solution, ethanol and distilled water.
The zinc sulphide thin film was prepared at room temperature
on thus pre-cleaned FTO and glass substrates.
2.2.2 Preparation of cationic and anionic precursors
Zinc Sulphide thin films were deposited on FTO using
Zn(NO3)2 as cationic precursor and Na2S as anionic precursor.
0.1M equivalent Zn(NO3)2 and Na2S were taken and dissolved
in 25 ml of DDW water respectively. Parameters used for the
deposition of ZnS thin film are summarized in Table 2.
We have selected simple and cost-effective chemical route
successive ionic layer adsorption and reaction (SILAR) for the
synthesis of ZnS thin film photo-anodes. One SILAR cycle
contains four steps: (a) the immersion of the substrate into the
first beaker containing the aqueous cationic precursor, (b)
rinsed with water, (c) immersion into the anionic precursor
solution, and (d) rinsing with water. Numbers of SILAR cycles
were repeated for uniform deposition of ZnS films on the pre-
cleaned FTO substrate.[24-29]
ES Energy & Environment Research article
© Engineered Science Publisher LLC 2021 ES Energy. Environ., 2021, 12, 77-85 | 79
Table 2. Parameter’s used for the deposition of ZnS thin film.
Parameters Precursors Solutions
Zinc Nitrate Sodium Sulphide
Concentration 0.1 M 0.1 M
pH ~9 ~9
Immersion Time (s) 15 15
Rinsing Time (s) 30 30
Number of SILAR cycles 40-70 40-70
Temperature (K) 300 300
2.2.3 Sensitization using coumarin-343
Before solar cell testing, the prepared films were immersed in
standard metal-free organic Coumarin-343 dye (Sigma
Aldrich, USA) with a concentration of 0.3 mM solution in
ethanol for 180 minutes for sensitization. Table 3 shows the
detailed description of the dye used for the sensitization of the
ZnS photoanode.
Table 3. Detail description of dye used for sensitization of ZnS
photoanode.
Nomencla-
ture
IUPAC
Name
Chemical
formulae
Molecular
Weight
(g/mol)
Concent-
ration
(M)
Coumarin
C343
5-(1,4,7,10-
tetraoxa-13-
azacyclopentadeca
ne-13-carbonyl)-3-
oxa-13-
azatetracyclo
[7.7.1.0^{2,7}.0^{
13,17}]
heptadeca-
1,5,7,9(17)-
tetraen-4-one
C26H34N
2O7
486.565 3 × 10-3
Fig. 2 Schematic of ZnS photoanode based photoelectrochemical
solar cell.
2.2.4 Solar cell assembly
Fig. 2 shows the schematic of ZnS photoanode based
photoelectrochemical solar cell. Platinum coated FTO used as
a counter electrode facing the ZnS photoelectrode was held
together using binder clips on the opposite end. Poly-iodide
solution was used as a liquid electrolyte consisting of 0.5 M
lithium iodide (SRL, India), 0.05 M iodine (Fisher Scientific,
USA), and 0.15 M tertiary butyl pyridine (ACROS Organics,
Belgium) in 100ml acetonitrile (SDFCL, India). Three to Five
layers scotch-tape of thickness about 30-45 μm were used as
spacers placed at the edge of the ZnS working electrode with
the active area of 0.25 cm2. Just before the analysis, drops of
prepared poly-iodide electrolytes were added in the prepared
sandwiched cell till no air bubble is present. The light was
introduced such that light gets penetrate through the FTO back
contact to the dye adsorbed onto the ZnS photo-anode.
3. Experimental characterizations
The microstructural properties of amorphous and crystalline
nature of SILAR deposited ZnS thin films were carried out
using X-ray diffractometer model Bruker D8 with CuKα
radiation of wavelength 1.5405 Å in the range of 20°-80°using
Rigaku D/Max-IIIC diffractometer. The Surface morphology
has been studied using Field emission scanning electron
microscopy (FESEM: FEI Nova NanoSEM450)with an
attached energy dispersive X-ray spectrometer (EDS: Bruker
XFlash 6130) to qualitatively measure the sample
stoichiometry. The sintered films were found porous
signifying its suitability for photoelectrochemical solar cell
applications. The absorption spectra of ZnS thin films with
different SILAR cycles were measured with an optical JASCO
V-770 UV-Vis spectrophotometer. The Absorption spectra
were plotted in the wavelength range of 300-800 nm.
Photovoltaic parameters of the fabricated cell were measured
using a solar simulator (Oriel Sol-2A, Newport, USA). AM1.5
sunlight filters with illumination intensities50 mW/cm2 and 33
mW/cm2 LED (Nvis Clean Tech, India). Keithley source meter
2420 (Keithley Instruments Ltd., USA) was used to measure
J-V characteristics. The incident intensity of illuminating light
sources was measured using sun meter (Solatron DSM 01,
India) and digital lux meter (Lutron LX-101A, Lutron
Electronic Enterprise CO., LTD., Taiwan). Optical
luminescence of illuminated light source was measured using
an optical spectrometer (Ocean Optics HR 4000, USA). The
J-V curve of the solar cell was obtained in the dark condition.
The J-V characteristics used to obtain open circuit voltage
(Voc), short circuit current density (Jsc), fill factor (FF),
efficiency (Eff). Electrochemical impedance measurements
were carried out using potentiostat/galvanostat (Vertex
IVIUM Technologies, Netherlands).
4. Results and discussion
4.1 Optical study
The Absorption Spectra of as-deposited ZnS films with varied
numbers of SILAR cycles were plotted as shown in Fig. 3. The
absorption peaks were in the visible range of the spectrum.
Research article ES Energy & Environment
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Fig. 3 The absorption spectrum of ZnS thin films for various
SILAR cycles.
Fig. 4 shows the tauc plot for various cycles of as-deposited
ZnS films. The band-gap was found to be 3.62 eV - 3.47 eV
for various deposition cycles.[23-24]The calculated values are
given in Table 4.
Fig. 4 The tauc plot of ZnS thin films for various SILAR cycles.
Table 4. The calculated bandgap Energy for the varied thickness
of ZnS photoanodes.
Varied SILAR Cycles Energy Gap
(eV)
ZnS (40) 3.62
ZnS (50) 3.54
ZnS (60) 3.52
ZnS (70) 3.50
It was observed that as the number of SILAR cycles
increases the optical bandgap was found to be decreasing. The
energy gaps of the films of various temperatures have been
determined by extrapolating the linear portion of the plots of
(αhν)2 against hυ (eV) to the energy axis.[32] Sensitization of
ZnS photoanode using Coumarin-343 in ethanol medium was
carried out and the absorption spectrum was plotted in the
wavelength range 200-800 nm.
Fig. 5 The UV-Visible spectra for the C-343 sensitized ZnS
photoanode.
The UV-Visible spectra for the C-343 sensitized ZnS
photoanode is as shown in Fig. 5. The spectrum shows two
distinct peaks at 316 nm and 426 nm. The spectrum is
attributed to organic dye C-343 and the absorption results are
in reasonable agreement with the literature.[33] It can be noted
that the C-343 absorption spectrum consists of one sole peak
at 460 nm.
Fig. 6 Low crystalline nature of deposited ZnS thin films
deposited on an FTO substrate.
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Fig. 7 FESEM images of Low Crystalline ZnS photo-anode.
4.2 Structural studies
The SILAR Deposited ZnS films deposited on the glass
substrate has been characterized by X-ray diffraction (XRD).
Fig. 6 shows the Low Crystalline nature of deposited ZnS
films on an FTO substrate were studied. From the XRD Graph,
it was observed that peak at 28.7° (111) which confirmed the
presence of ZnS in a low crystalline form which was matched
with JCPDS Card No: 05-0566. Here in this article, the low
crystalline nature of ZnS is exploited as an advantage in the
sense that it provides a more uniform coverage of the FTO
substrate by ZnS without gaps between the grains. The bilayer
form of solar cell assembly plays an added advantageous since
a second new layer will not come into direct contact with the
FTO front through any possible gaps between ZnS grains.
4.3 Morphological studies
A field emission scanning electron microscope has been used
to study the morphology of ZnS surface films. Fig. 7 shows
the FESEM images of deposited films in the magnification
range of 30000 and 100000. The FESEM image establishes
the mesoporous nature of ZnS films which is a suitable
morphology for the application of a photoelectrochemical
solar cell. The average thickness of the ZnS film was found to
be 1.43 µm using cross-section measurement in FESEM.
4.4 Compositional analysis
Energy Dispersive X-ray Spectrometer (EDS) was used to
study the compositional analysis of SILAR deposited ZnS
films. Fig. 8 shows the EDS spectrum of the surface film. The
elemental analysis shows the presence of Zinc (Zn) and
sulphur (S) along with some other elements. In the spectra, a
carbon peak is observed due to the substrate holder and an
oxygen peak might be due to the partial oxidation of the film.
Presence of Si and Sn results from the substrate. The relative
average atomic percentage ratio of Zn:S is nearly 1:1 for the
films, indicating the formation of a film with stoichiometric
composition.
Research article ES Energy & Environment
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Fig. 8 The EDS spectra of ZnS photoanode.
The EDS spectra shows two peaks for the Zn atom
attributable to the Kα and Lα. EDS characteristic peaks (keV)
for Zn are 8.630 (Kα) and 1.012(Lα) respectively. Although
Zn atom has a peak (keV) characteristic at 2.307 (Kα).
4.5 Solar cell characteristics
Fig. 9 shows J-V Characteristics the C-343 sensitized ZnS
photoanode photoelectrochemical solar cell with Platinum as
counter and polyiodide as electrolyte. The J-V characteristics
of the thus fabricated solar cell was carried out using a solar
simulator (Oriel Sol-2A, Newport, USA). AM1.5 sunlight
filters with illumination intensities 50 mW/cm2 and 33
mW/cm2 LED (Nvis Clean Tech, India). Keithleysource meter
2420 (Keithley Instruments Ltd., USA) was used to measure
J-V Characteristics. The incident intensity of illuminating light
source was measured using sun meter (Solatron DSM 01,
India) and digital lux meter (Lutron LX-101A, Lutron
Electronic Enterprise CO., LTD., Taiwan). The characteristics
such as open circuit voltage (Voc), short circuit current density
(Jsc), fill factor (FF), efficiency (𝞰) were found as 0.52 V, 0.35
mA/cm2,0.59 and 0.1%, respectively. The calculated values
are given in Table 5. Since ZnS is usually attempted as a
collecting layer; here we try to study ZnS separately for solar
cell applications. Further refinement will be done to enhance
the efficiency with some efficiently.
Fig. 9 J-V Characteristics of SILAR prepared ZnS Photoanode for a) 40, b) 50, c) 60 and d) 70 SILAR cycles respectively sensitized
with C-343 Dye for photoelectrochemical solar cell application.
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Table 5. The Solar Cell parameters from J-V Characteristics under one Sun condition.
Fig. 10 shows the Bode plot of a) 40, b) 50, c) 60 and d) 70 SILAR
cycles respectively sensitized with C343 Dye using EIS
characterisation for photoelectrochemical solar cell applications.
4.6 Electrochemical impedance spectroscopy
Electrochemical Impedance spectroscopy was carried out in
MHz to Hz frequency range with -0.8 V constant applied
potential. Fig. 10 shows the Bode plot with characteristic
frequency peak in the middle frequency range. The mean
electron lifetime calculated from the relation:
τmax=1
2𝜋𝑓𝑚𝑎𝑥 (1)
Where, fmax is the maximum frequency. The electron lifetime
was observed under dark conditions. When light is incident on
the cell, the electrons are generated and current flows through
the external circuit, which reduces the charge recombination
resistance and this reduces the electron lifetime. The EIS study
is carried out to determine electron transport and
recombination resistance. Fig. 11 shows the Nyquist plot for
the ZnS based photoelectrochemical solar cell.
The series resistance of solar cell was calculated from the
Nyquist plot as ~16.6 ohms. The EIS equivalent circuit fitted
parameters Rtr and Rct can be used to calculate the parameters
such as diffusion length (Ln), charge collection efficiency (𝞰cc),
effective electron diffusion coefficient (Deff), effective
electron diffusion length (Leff), which is useful to study the
electron transport properties of the solar cell. With the help of
the EIS Nyquist plot, the diffusion length is calculated using
formula Ln =√(Rct/Rtr).[34] Further effective electron diffusion
co-efficient in the photoanode is given by Deff = (Rct/Rtr) ×
(l2/τeff).[35] Where l is the thickness of ZnS thin film. Charge
collection efficiency is calculated using 𝞰cc= 1-(Rtr/Rct).[36]
Effective electron diffusion length calculated using
Leff=√(Deff × τ eff).[37] Effective electron diffusion length
calculated using τ D = τeff * (Rtr/Rct).[38] The calculated values
are given in Table 6.[39]
Table. 6. Detailed report of EIS study of SILAR prepared ZnS photoanode (40-70 cycles) for photoelectrochemical solar cell
application.
Sample in Dark
Room (No. of cycles) RTR RCT RCT/RTR
Ln
(μm)
𝞰cc
(%)
τeff
(ms)
τd
(ms)
Deff
(cm2/s)
Leff
(μm)
Sample1: ZnS (70) 24.29 254 10.45 3.233 0.904 1.59 0.15 1.343 4.62
Sample 2: ZnS (60) 310.8 2170 6.981 2.64 0.856 0.014 2.03 0.031 6.60
Sample 3: ZnS (50) 428.9 1026 23.92 4.89 0.958 0.012 0.50 0.079 9.73
Sample 4: ZnS (40) 11050 11490 10.39 3.22 0.903 0.010 0.96 0.021 4.58
Sample
(No. Of Cycles)
J sc
(mA/cm2)
V oc
(V)
Fill Factor
Efficiency
(%)
ZnS (40) 0.118 0.108 0.24 0.0031
ZnS (50) 0.004 0.040 0.25 0.0004
ZnS (60) 0.023 0.353 0.27 0.0022
ZnS (70) 0.350 0.520 0.59 0.1000
Research article ES Energy & Environment
84 | ES Energy Environ., 2021, 12, 77-85 © Engineered Science Publisher LLC 2021
Fig. 11 shows the Nyquist plot of a) 40, b) 50, c) 60 and d) 70
SILAR cycles respectively sensitized with C343 Dye using EIS
characterisation for photoelectrochemical solar cell application.
5. Conclusions
We reported a low crystalline or amorphous nature of zinc
sulfide (ZnS) as a photoanode for photoelectrochemical solar
cell applications. For the synthesis of ZnS thin film photo-
anodes, we used simple and cost-effective chemical route
successive ionic layer adsorption and reaction (SILAR)
method. The dye sensitized ZnS nanoparticles show a strong
visible absorption at 460 nm in UV-Vis analysis. The fill factor
and efficiency of the device was found to be 0.59 and 0.1%
respectively. Electrochemical studies of thus prepared ZnS
photo-anode were carried out. The mean electron lifetime and
effective electron diffusion length were calculated as 1.59 ms
and 4.62 μm respectively under dark condition. Structural
Analysis shows that the nanoporous and crystalline nature of
the ZnS thin films which implies that it is a suitable and
considerable candidate for photoanode in the
Photoelectrochemical solar cell.
Acknowledgment
HMP acknowledges the Department of Science and
Technology, Government of India for financial support vide
Sanction order DST/TMD/SERI/S173 (G).PM acknowledges
Bharat Ratna JRD Tata Scholarship (2018-19).
Conflict of interest
There are no conflicts to declare.
Supporting information
Not applicable
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Author information
Priyanka M. Mana is a M.Phil.Student at
the Advanced Physics Laboratory,
Department of Physics, Savitribai Phule
Pune University, Pune, India with
Dr.Habib M.Pathan. She received his
master’s degree in Physics from
University of Calicut,Kerala. Her
research interests include Thin films,
Quantum Dots and DSSCs.
Pankaj K. Bhujbal is a research fellow
in Physics at the Advanced Physics
Laboratory, Department of Physics,
Savitribai Phule Pune University, Pune,
India with Dr.Habib M. Pathan. He
received his master’s degree in Physics
from the Fergusson college, Pune. His
research interests include Thin films,
Quantum Cascade Laser and DSSCs
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