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Synthesis of Sb2S3 nanosphere layer by chemical

Cite this: RSC Adv., 2023, 13, 22054
bath deposition for the photocatalytic degradation
of methylene blue dye
Open Access Article. Published on 21 July 2023. Downloaded on 8/14/2023 8:52:43 PM.

Mohammed M. Gomaa, *a Mohamed H. Sayed, ab

Mahmoud S. Abdel-Wahed c

and Mostafa Boshta a

An antimony tri-sulfide Sb2S3 nanosphere photocatalyst was effectively deposited utilizing sodium
thiosulfate and antimony chloride as the starting precursors in a chemical bath deposition process. This
approach is appropriate for the large-area depositions of Sb2S3 at low deposition temperatures without
the sulfurization process since it is based on the hydrolytic decomposition of starting compounds in
aqueous solution. X-ray diffraction patterns and Raman spectroscopy analysis revealed the formation of
amorphous Sb2S3 layers. The scanning electron microscopy images revealed that the deposited Sb2S3
has integrated small nanospheres into sub-microspheres with a significant surface area, resulting in
increased photocatalytic activity. The optical direct bandgap of the Sb2S3 layer was estimated to be
about 2.53 eV, making amorphous Sb2S3 appropriate for the photodegradation of organic pollutants in
the presence of solar light. The possibility of using the prepared Sb2S3 layer in the photodegradation of
methylene blue aqueous solutions was investigated. The degradation of methylene blue dye was
performed to evaluate the photocatalytic property of Sb2S3 under visible light. The amorphous Sb2S3
Received 29th March 2023
Accepted 5th July 2023
exhibited photocatalytic activity for the decolorization of methylene blue solution under visible light. The
mechanism for the photocatalytic degradation of methylene blue has been proposed. Our results
DOI: 10.1039/d3ra02062b
suggest that the amorphous Sb2S3 nanospheres are valuable material for addressing environmental
rsc.li/rsc-advances remediation issues.

Spherical structures are classied as basic or complex based on

Introduction their structural complexity. Simple spherical formations are one
Nanostructured metal suldes (NMSs) have recently attracted thing, as are solid spheres and single-shelled hollow spheres.17
considerable interest in a number of applications owing to their Because of their customizable physical and chemical properties,
distinct optoelectronic and catalytic properties.1–3 These prop- spherical structures offer signicant structural advantages for
erties depend greatly on the morphologies and dimensions of electrochemical applications. High complexity hollow spherical
the prepared materials,4 making these materials feasibly useful micro/nanostructures have drawn signicant interest in both
in various applications, such as dye removal from wastewater,5 theoretical studies and practical applications. Nanostructured
energy conversion and storage,6 rechargeable lithium-ion spherical materials showed enhanced electrochemical perfor-
batteries,7 hydrogen evolution,8,9 and photocatalysts.10 Metal mance and structural stability compared to the other alternative
sulde nanostructures with controllable nanoshapes, such as structures.16,18 The variety of the material forms offers more
particles, wires, sheets, akes,11 hollow spheres,12 and core– potential for increasing functionality than simple spherical
shell structures,13 have been regarded as potential cost-effective, structures, which enhances the photocatalytic performance of
chemically stable, and nontoxic semiconducting materials for the active material.15,16
catalytic applications.8,14,15 Metal sulde materials have received a great deal of atten-
Spherical structures are a type of functional material that has tion and study.19–25 Among metal suldes, antimony suldes
a high surface area and small charge transport lengths.16 with different phases have received signicant attention owing
to their unique physical properties, low toxicity, abundance,
and environment-friendliness, making them ideal candidates
a
Solid State Physics Department, National Research Centre, Dokki, Giza 12622, Egypt. for solar cells and environmental applications.26 Sb2S3 can have
E-mail: [email protected]; Tel: +201272110812
b
either an amorphous phase known as metastibnite or a crystal-
Molecular and Fluorescence Spectroscopy Lab, Central Laboratories Network,
line phase known as stibnite, depending on the synthesis
National Research Centre, Dokki, Giza 12622, Egypt
c
Water Pollution Research Department, National Research Centre, Dokki, Giza 12622,
process. The amorphous Sb2S3 phase has a direct energy gap
Egypt (Eg) in the range of 1.7–2.8 eV, while the Eg for the crystalline

22054 | RSC Adv., 2023, 13, 22054–22060 © 2023 The Author(s). Published by the Royal Society of Chemistry
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phase ranges between 1.7 and 1.8 eV.27 In terms of application, (Na2S2O3$5H2O – Sigma Aldrich) aqueous solution with
the photocatalytic performance of antimony compounds in the continuous stirring, producing clear and homogeneous solu-
degradation of organic pollutants is still less efficient compared tion. During the synthesis process, the cleaned substrates were
to other photocatalysts based on noble metals and phos- vertically dipped in the solution bath at a low deposition
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phides.3,28 In this regard, limited work has been devoted to temperature and pH of 6. Aer 10 minutes, the colorless solu-
using Sb2S3 as a photocatalytic material in the degradation of tion was transformed into an orange–yellow solution with the
organic dyes.29 In addition, amorphous and crystalline Sb2S3 in Sb2S3 layer formed on the substrate surface due to the adsorp-
the powder form have displayed an enhanced photocatalytic tion and nucleation of antimony sulde on the substrate. To
degradation of organic dyes with visible light.30,31 To the best of remove the residual precipitation, the deposited layers were
our knowledge, nanosphere Sb2S3 layers have not been inves- washed several times with distilled water. Fig. 1 shows a sche-
tigated before in the photocatalytic degradation of organic dyes. matic representation of the chemical bath deposition process of
Open Access Article. Published on 21 July 2023. Downloaded on 8/14/2023 8:52:43 PM.

The innovative characteristic quality within the Sb2S3 layers that the nanosphere-structured Sb2S3 layer.
causes the separation of those materials will secure their The deposition was performed in a relatively weak acidic
multiple usages and consequently reduce the overall treatment solution at pH approximately 3. Hence, the mechanism of the
cost. Therefore, the creation of a more sufficient synthesis nanosphere-structured as-deposited Sb2S3 layer using thio-
process for the inorganic nanosphere is important. Addition- sulphate solution is based on the hydrolytic decomposition of
ally, amorphous Sb2S3 layers are still quite uncommon and antimony(III) thiosulphate complexes of Sb2(S2O3)3 formed in
require more investigation.32 Most of the chemical methods are aqueous media as a result of the reaction between SbCl3 and
suitable for preparing antimony suldes in powder form with Na2S2O3, as in the following reactions:35,36
different phases.9,33 Among these approaches, chemical bath
deposition (CBD) is one of the most attractive deposition 2SbCl3 + 3Na2S2O3 / Sb2(S2O3)3 + 6NaCl (1)
processes because it is simple, cost-effective, and suitable for
depositing a large area of thin lms. The demand for an 2Sb3+ + 3S2O32− / Sb2(S2O3)3 (2)
approach to prepare thin lms with a high specic area and
Thiosulphate ions in acidic media can gradually release S2−
controlled morphology is still a major challenge, and it will
ions during hydrolytic decomposition, according to the
open doors to diverse prospects for environmental application.
reactions.
Methylene blue is a persistent organic pollutant material
that is used in textile manufacturing for dyeing objectives in the S2O32− + H+ / S + HSO3− (3)
modern world. Waste from textile manufacturing deteriorates
water resources, and is detrimental to humans and other living S + 2e− / S2− (4)
organisms because of the potential for eye diseases, kidney
diseases, and skin diseases. These types of pollutants cannot be The released excess S2− ions react with the Sb3+ ions released
removed by conventional treatment.34 Thus, the development of from the thiosulphate complexes upon hydrolysis, reacting on
novel methods is needed to address this concern. One of the the glass substrates to form orange-yellow Sb2S3:
main issues in the photocatalyst process is the separation and
recovery constraint of the photocatalyst from the effluent aer 2Sb3+ + 3S2− / Sb2S3Y (5)
the treatment process. Therefore, this work overcomes this
issue through the deposition of Sb2S3 on a glass substrate as
thin layers.
A feasible CBD approach was used in this study to effectively Characterization of the as-deposited Sb2S3 layer
produce Sb2S3 nanosphere layers directly without the need for
In this study, Cu Ka radiation at 40 kV and 40 mA was used to
a sulfurization process. The structural, morphological, optical,
conduct X-ray diffraction (XRD) investigations for the structural
and catalytic properties of the resulting Sb2S3 layers were
investigated. The unique nanosphere shape of the Sb2S3 layers
acts as a powerful photocatalyst for the photodegradation of
methylene blue dye.

Experimental
Sb2S3 layer deposition
Initially, the chemical bath deposition (CBD) technique was
employed to prepare a nanosphere-structured antimony sulde
layer. The used glass substrates were cleaned in an ultrasonic
bath with acetone, ethyl alcohol, and distilled water separately
for 20 minutes, followed by nitrogen gas drying. As the starting
solution, antimony chloride (SbCl3 – Sigma Aldrich) was dis- Fig. 1 Schematic description of the synthesis of nanosphere Sb2S3
solved in acetone and dropped into 1 M sodium thiosulfate layers.

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and phase examination of the Sb2S3 layer. The morphology of before and aer photocatalytic test. The appearance of a broad
the deposited layers was imaged using FEI Quanta 250 FEG peak in the range of 250–350 cm−1 and centered at the position
scanning electron microscopy (SEM). X-Ray photoelectron 289 cm−1 indicated the existence of Sb2S3 in the amorphous
spectroscopy (XPS) data were collected using a K-ALPHA phase, as described in prior studies.40–42 The Raman spectra
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(Themo Fisher Scientic, USA) spectrometer to determine the clearly indicate that no structural changes are observed in the
chemical composition and electronic states of the Sb2S3 layer. Sb2S3 layers aer the test.
The Raman study was carried out using a Witec Alpha 300 RA This work used X-ray photoelectron spectroscopy (XPS)
confocal Raman microscope with laser excitation at 532 nm. measurements to investigate the elemental compositions and
Optical measurements were performed using a UV/VIS/NIR electronic states of a nanosphere Sb2S3 layer. Fig. 3(a) presents
spectrophotometer (Jasco V770). the high-resolution XPS spectrum of Sb 3d for the deposited
Sb2S3 layer, which has two main peaks located at 529.93 eV and
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539.22 eV. These two peaks were assigned to the spin–orbit

Evaluation of the photocatalytic performance of the Sb2S3
splitting of Sb 3d5/2 and Sb 3d3/2, respectively, which was
layers
separated by 9.29 eV. The binding energies values and the
The photocatalytic activity of the as-prepared Sb2S3 this lm was separation by spin orbit coupling suggest that Sb bound to S
recognized by methylene blue photodegradation as a model of remains in the Sb3+ oxidation state, which coincides well with
the refractory organic contaminants. For this goal, the Sb2S3 the reported values of Sb3+ in the Sb2S3 lattice. These values are
sample was xed on a 2 cm-height edge inside a 150 mL beaker within the range of the binding energy values reported by
by a silicon adhesive. Aer that, the beaker was lled with 90 mL various research groups for the Sb3+ state in the Sb2S3
of 10 mg L−1 methylene blue solution, and stirred by a magnetic material.42–44
stirrer. Then, the beaker was irradiated vertically using a UVA- In addition, the high-resolution spectrum of the S core level
CUBE 400 sunlight simulator (Dr Hönle AG UV Technology, presents two peaks, a main peak located at 162.11 eV and
Germany). At denite time intervals, online measurement of a shoulder peak positioned at 160.98 eV, which correspond to
methylene blue removal was performed by spectrophotometer the 2p1/2 and 2p3/2 of S2−, respectively, and separated by 1.13 eV
(Jasco 630). The creation of the redox reactive species by the as shown in Fig. 3(b). These values imply the existence of
Sb2S3 thin lm slide excited by solar irradiation was studied by unsaturated sulfur atoms on the Sb–S and S–S bonds in
1 mmol ammonium oxalate (AO), para-benzoquinone (p-BQ) Sb2S3.45,46 XPS analysis conrmed that the deposited sample is
and isopropyl alcohol (IPA) as the hole (h+) scavenger agent, the the Sb2S3 material. The results of the XRD, Raman and
superoxide radical (O2c−) scavenger and as the hydroxyl radical elemental composition and chemical states analysis conrmed
cOH scavenger, respectively. that the deposited samples are an amorphous Sb2S3, which is in
agreement with the reported studies.47,48
Results and discussion
Structural and elemental composition properties Morphological characterization
The XRD and Raman data of the produced Sb2S3 layer are pre- The SEM images with different magnications of the deposited
sented in Fig. 2. It is seen that no obvious characteristic peaks samples on the glass are displayed in Fig. 4. The morphological
were observed in the XRD spectrum of the as-deposited Sb2S3 properties of the deposited Sb2S3 indicate a preference for the
layer by the CBD method, indicating that the deposited layer eventual integration of small nanospheres into sub-
has an amorphous phase structure, as shown in Fig. 2(a). microspheres. It is clear that the nanospheres are randomly
The obtained results are in agreement with the previously distributed and have different sizes. The irregularly stacked and
reported XRD data for the Sb2S3 deposited by CBD in different merged small nanospheres resulted in consolidated sub-
media and different starting sulfur precursors,37,38 and the re- microspheres ranging in size from 0.25 mm to 0.5 mm. More-
ported amorphous Sb2S3 phase prepared by thermal evapora- over, as can be seen in the magnied images, the sub-
tion technique.39 Fig. 2(b) shows the Raman spectrum of Sb2S3 microspheres have a rough surface and have a propensity to
develop pores within the spheroidal units (Fig. 4(d)). These sub-

Fig. 2 (a) XRD pattern of Sb2S3 and (b) Raman spectra of Sb2S3 before Fig. 3 XPS spectra of the core levels for deposited Sb2S3: (a) Sb 3d and
and after the photocatalytic test. (b) S2.

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band gap (Eg) of the Sb2S3 layers by extrapolating the linear

portion near the onset of the absorption edge to the energy
axis, as shown in Fig. 5b. The estimated value of Eg for the
Sb2S3 layer was 2.53 eV, which agrees with the reported
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values.27,52 A similar range of the Eg value would qualify the

benet of this material in the solar photocatalytic
applications.42

Catalytic properties
The photocatalytic activity of the prepared Sb2S3 thin lm was
performed with 10 mg L−1 methylene blue as the module
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organic compound at a pH of 6.5, and 5 cm2 area of the Sb2S3

thin lm. The change in relative concentration (C/Co) of
methylene blue with time is presented in Fig. 6. In the pres-
Fig. 4 (a)–(d) SEM images with different magnifications of the Sb2S3
ence of the prepared Sb2S3 thin lm and solar light irradia-
layer. tion, the methylene blue (C/Co) decreased with time. The
prepared Sb2S3 thin lm was activated by the absorbed solar
light, which initiated the photoproduction of e−/h+ that was
microspheres are anticipated to offer more practical anchoring employed in the photodegradation of methylene blue. In
sites and allow for the adsorption of organic dyes, which could contrast, the presence of only solar light irradiation without
enhance the photocatalytic activity.12,49,50 the prepared Sb2S3 thin lm resulted in the insignicant
photolysis of methylene blue.
The produced redox species that was generated aer exciting
Optical properties the prepared Sb2S3 layer by solar light was identied by
Fig. 5(a) displays the optical transmittance and reectance appending 1 mmol of the individual scavenger agents (IPA, AO
spectra of the chemically deposited Sb2S3 layer as a function of and p-BQ) with 10 mg L−1 methylene blue and the Sb2S3 sample.
wavelength ranging between 250 to 2500 nm. The following Fig. 7 represents the effect of the scavengers on methylene blue
formula is utilized to calculate the absorption coefficient (a). removal in the presence of scavengers and without scavengers.
2 sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi 3 The hydroxyl radical (cOH) is a primary active species, the
1 4ð1 RÞ2 ð1 RÞ4 superoxide radicals (O2c−) is a secondary active species, and the
a ¼ ln þ þ R2 5 (6)
t 2T 4T 2 hole (h+) is a third active species. Therefore, the suggested
mechanism of the photocatalytic reactions is specied by the
where T, R, and t are the transmission, reectance, and lm subsequent equations:
thickness, respectively. The Tauc equation has been presented hn
Sb2 S3 ! Sb2 S3 hþ ; e
 
as a mathematical equation to demonstrate the relationship (8)
between the optical energy gap and the energy of the incident
photon.

ahn = A(hn − Eg)n (7)

where a is the absorption coefficient, hn is the photon energy,

A is a constant, Eg is the band gap, and n is an index that has
values of 1/2, 2, 3/2, and 3, depending on the electronic
transition of the deposited material.51 The plot of (ahn)2 vs. hn
for the directly allowed transition is used to calculate the

Fig. 6 Photocatalytic activity of the prepared Sb2S3 sample, methy-

Fig. 5 (ahn)2 versus photon energy (hn) for the nanosphere Sb2S3 layer. lene blue = 10 mg L−1, pH 6.5 and Sb2S3 sample (5 cm2).

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Conclusions
In summary, the antimony tri-sulde Sb2S3 nanosphere layer
was synthesized directly by chemical bath deposition method at
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low deposition temperature and large scale for efficient photo-

catalytic application. The deposited layer was characterized by
various characterization techniques that demonstrated that
Sb2S3 has an amorphous phase structure with good morpho-
logical and optical properties. X-ray diffraction and Raman
analysis showed the amorphous structure of the Sb2S3 lms.
Optical analyses revealed that the Sb2S3 layer has an optical
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energy gap of 2.53 eV, which makes these layers a reliable

material for photocatalytic application. The photocatalytic
activity of Sb2S3 for degrading methylene blue under visible
light was investigated. The degradation rate of the amorphous
Sb2S3 layer toward methylene blue is highly efficient. This is due
to the broad-spectrum response and the proper valence band
Fig. 7 Effect of scavengers on the methylene blue removal efficiency. position of Sb2S3. This investigation indicates that Sb2S3 is an
excellent visible-light responsive photocatalyst for degrading
organic pollutants.
−
OH + h+ / cOH (9)
Author contributions
O2 + e− / O2c− (10)
Mohammed M. Gomaa: conceptualization, data curation,
Methylene blue + h+ + cOH + O2c− / indermediate / degraded formal analysis, investigation, methodology, writing – original
products (11) dra. Mohamed H. Sayed: conceptualization, data curation,
formal analysis, investigation, methodology, writing – original
dra. Mahmoud S. Abdel-Wahed: conceptualization, method-
One of the most important factors that inuence the prac-
ology, data curation, formal analysis, investigation, writing –
tical application of the photocatalysts is the reusability test,
original dra. Mostafa Boshta: funding acquisition, project
which will lead to a cost-effective treatment process. So, the
administration, resources, supervision, validation, writing –
photocatalytic activity of the prepared Sb2S3 layer (5 cm2), pH
original dra.
natural and 10 mg L−1 methylene blue on reuse experiments is
offered in Fig. 8. An insignicant decrease in the methylene
blue photodegradation removal was observed with up to ve Conflicts of interest
runs. This demonstrates that the prepared Sb2S3 layer can
The authors declare no competing interests.
maintain its photocatalytic activity and stability for more times
in treatment processes, as conrmed by Raman measurements.
Acknowledgements
The authors acknowledge the nancial support from the
National Research Centre Fund, through in-house project
numbers 13020240 and 13040124.

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22060 | RSC Adv., 2023, 13, 22054–22060 © 2023 The Author(s). Published by the Royal Society of Chemistry