J Mater Sci: Mater Electron (2017) 28:3487–3494
DOI 10.1007/s10854-016-5947-6
Solvent effects on the properties of Bi2S3 nanoparticles:
photocatalytic application
J. Arumugam1 • A. Dhayal Raj1 • A. Albert Irudayaraj1
Received: 18 August 2016 / Accepted: 24 October 2016 / Published online: 5 November 2016
Ó Springer Science+Business Media New York 2016
Abstract Well-segregated bismuth sulfide nanorods and
nanoparticles with a high order of crystallinity have been
successfully prepared by simple reflux method for 2 h using
different solvents. Bismuth nitrate, thiourea and citric acid
are used as starting materials. Different solvents like
dimethylformamide, ethylene glycol, polyethylene glycol
have been used. The effect of solvent on the properties of
the bismuth sulfide has been investigated and reported. The
powder X-ray diffraction patterns indicated that the product
had orthorhombic phase. The Scanning electron microscope
and transmission electron microscope studies reveal that the
product Bi2S3 can be tuned to different morphologies by
altering the solvent. The optical properties of these Bi2S3
nanorods and nanoparticles were characterized by UV–Vis
spectrometer (UV) and the bond vibrations present in the
product were identified using FT-IR spectra. The room
temperature photoluminescence spectra of Bi2S3 nanopar-
ticles revealed an emission band centered at 585 nm cor-
responding to yellow region. The photocatalytic activities
of the Bi2S3 nanorods have been evaluated by decomposing
methylene blue (MB) under light irradiation and complete
degradation of MB was witnessed after 120 min.
1 Introduction
Preparation of semiconductor nanomaterials have attracted
considerable attention in recent years because of their
electronic, optical, chemical properties [1] and their
& A. Dhayal Raj
dhayalraj03@gmail.com
1
PG and Research Department of Physics, Sacred Heart
College, Tirupattur, Tamilnadu 635601, India
potential applications in constructing thermoelectric devi-
ces [2], electronic and optoelectronic devices [3], hydrogen
storage materials [4, 5] and sensors [6]. There has been an
increasing interest in the preparation of one-dimensional
nanostructures, such as nanorods, nanowires and nanotubes
since the discovery of carbon nanotubes at the end of
twentieth century [7]. Among these semiconductors, bis-
muth sulfide (Bi2S3) a direct band gap layered semicon-
ductor that crystallizes in the orthorhombic system [8], is a
candidate for photodiode arrays and photovoltaic convert-
ers, due to its low energy gap (1.3 eV) which has been
widely used in thermoelectric cooling technologies [9].
Bi2S3 also belongs to a family of solid-state materials with
applications in thermoelectric cooling technologies based
on the Peiltier effect [10]. The availability of Bi2S3
nanostructures with one-dimensional morphology should
be able to bring in new types of applications or enhance the
performance of the currently existing device. So the syn-
thesis of 1D nanostructures of Bi2S3 should be of great
significance [11].
One dimensional Bi2S3 nanomaterials have been fabri-
cated through various synthetic approaches like
solvothermal, hydrothermal, sonochemical, microemul-
sion, microwave and refluxing method. Among them, the
reflux method is simple and very efficient for forming the
Bi2S3 nanomaterials. The light irradiation of nanocrys-
talline semiconductors systems has been successful for the
photodegradation of a wide variety of inorganic com-
pounds [12]. When a semiconductor is illuminated with
light of an appropriate wavelength it generates highly
active oxidizing sites, which can potentially oxidize a large
number of organic wastes such as dyes, pesticides and
herbicides [13]. Yang et al. [14], have reported the con-
trolled synthesis of high crystalline nanorods using differ-
ent precursors and also Thongtem et al. [15], have
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3488
synthesised the Bi2S3 nanoparticles with different mor-
phologies using various solvents for using solvothermal
method. Chen et al. [16], from south central university,
china, have reported the large scale synthesis of bismuth
sulfide nanorods through reflux and microwave methods.
Albuquerque et al. [17–19], have showed photocatalytic
activity of SiO/Bi2S3 nanocomposites in the degradation of
methylene blue. However, Photocatalytic degradation of
pure Bi2S3 have been scarcely reported [20, 21].
This paper discusses a simple, inexpensive and efficient
approach for the synthesis of Bi2S3 nanostructures. The
solvent effects are discussed in detailed and the growth
mechanism of the nanoparticle is proposed. Furthermore,
this paper focuses not only on the synthesis of Bi2S3
nanoparticles using different solvents and study of struc-
tural, surface and optical properties, but also focuses on the
possible catalytic application of such Bi2S3 nanoparticles.
2 Experimental
All the reagents were of analytical grade and used directly
without further purification. In a typical experiment,
0.001 mol of bismuth nitrate, 0.001 mol of citric acid,
0.003 mol of thiourea, 0.007 mol of CTAB and 100 ml of
DMF/EG/PEG have been used for the reaction. The mix-
ture was stirred and sonicated until all the chemicals were
dissolved. The mixture was refluxed at 140 °C for 2 h with
continuous stirring and after cooling down naturally to the
room temperature, the mixture was centrifuged and the
black color solid product was collected. The solid product
was then washed several times in acetone and water.
Finally, the solid product was dried in a hot air oven. In
order to analyze the effect of solvent, samples have been
prepared with different solvents such as DMF, PEG and
EG. The as-synthesized samples were further characterized
by power X-ray diffraction, scanning electron microscope,
energy dispersive X-ray spectroscopy, transmission elec-
tron microscope with Selected area electron diffraction
patterns, UV–Vis spectroscopy, Fourier transformation
analysis and photoluminescence (PL) analysis.
3 Result and discussion
The purity and crystalline structure of Bi2S3 nanoparticles
were characterized by powder X-ray diffraction (XRD)
obtained on a Rigaku miniflexII diffractometer, with CuKa
as the radiation source at a wavelength k = 0.1540 nm
with 2h angle ranging from 10° to 80° at room temperature.
The XRD pattern of the as-synthesized Bi2S3 nanoparticles
prepared with different solvents such as (a) N,N-
dimethylformamide (DMF), (b) ethylene glycol (EG) and
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J Mater Sci: Mater Electron (2017) 28:3487–3494
(c) ploy ethylene glycol (PEG) are shown the Fig. 1. The
X-ray power diffraction indexed peaks exactly match with
the JCPDS card no # 75-1306 and reveal good polycrys-
talline nature. The structure of the Bi2S3 nanoparticles were
found to be orthorhombic. The crystallite sizes have been
calculated using the Scherrer formula and were found to be
around 30, 32 and 35 nm for samples prepared with DMF,
EG, and PEG respectively. The morphology of the Bi2S3
nanoparticles have been characterized by scanning electron
microscope (SEM) on TESCAN VEGA 3 SBU at an
accelerating voltage of 30 kV. Figure 2 shows the SEM
images of the Bi2S3 nanoparticles synthesized by reflux
method for different solvents with 2 h reaction time at
140 °C. SEM image in Fig. 2a shows nanorods and sheet
like morphologies of Bi2S3 nanoparticles prepared with
N,N-dimethylformamide (DMF) as a solvent. Figure 2b
shows some uniform sphere like morphology of Bi2S3
nanoparticles prepared with ethylene glycol (EG) as sol-
vent. Figure 2c shows the agglomerated Bi2S3 nanoparti-
cles prepared with PEG as solvent. It can be clearly seen
that solvent plays a major role in determining the shape and
morphology of the Bi2S3 nanoparticles.
The samples prepared with DMF shows 1D rod like
morphology whereas the samples prepared with EG and
PEG shows spherical morphology. The surfaces of the
nanorods are very smooth. The composition of the nanor-
ods as extracted from the energy dispersive spectroscopy
(EDX) spectrum are presented in Fig. 2d which confirms
the presence of Bi and S atoms. The deficiency of S with
respect to stoichiometry in the nanorods can be attributed
(130)
(230)
(221)
(240)
(220)
(132)
(431)
(120)
(002)
(020)
(301)
(141)
(021)
Intensity (a.u)
(600)
(421)
c
b
a
10 20 30 40 50 60 70 80
2 (degrees)
Fig. 1 XRD pattern of as - synthesized Bi2S3 nanoparticles prepared
with different solvents (a) DMF, (b) EG and (c) PEG
J Mater Sci: Mater Electron (2017) 28:3487–3494 3489

a b

cps/eV

c d
10

6
S
S O Bi

0
1 2 3 4 5

Fig. 2 a SEM image of Bi2S3 nanorods prepared with a DMF as solvent, b EG as solvent c PEG as solvent and d EDX spectrum of Bi2S3
nanorods

to the vapour pressure of S higher than that of Bi. Little
evidence of O was detected in this spectrum [22]. The
morphology of the Bi2S3 nanoparticles have been charac-
terized by transmission electron microscope (TEM) on
JEOL-JEM 200CX at an accelerating voltage of 200 kV
Fig. 3 shows the TEM image of Bi2S3 nanoparticles pre-
pared with different solvents namely DMF, EG and PEG.
Figure 3a shows the nanorod like morphology of Bi2S3
prepared with DMF. The average breadth of the rod is
around 25 nm and the interplanar distance between the
atoms, was 0.35 nm. Figure 3b is shown the selected area
diffraction pattern of the Bi2S3 nanorods, revealing crys-
talline nature. Figure 3c shows the TEM image of the as-
synthesized Bi2S3 nanoparticles prepared with EG con-
sisting of large number of small spheres with diameter
10 nm and the interplanar distance was around 0.31 nm.
Figure 3d exhibits the corresponding selected area electron
diffraction (SAED) image Bi2S3 nanoparticles prepared
with EG. Very big sphere like morphology of Bi2S3 par-
ticle prepared with PEG as a solvent are shown in Fig. 3e.

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3490 J Mater Sci: Mater Electron (2017) 28:3487–3494

a d

Bi2S3
0.35 nm

b e

Bi2S3
0.31 nm

c f

Bi2S3
0.31 nm

Fig. 3 TEM image of Bi2S3 nanoparticles prepared with different solvents a DMF, b EG c PEG and SAED pattern of Bi2S3 nanoparticles
prepared with solvents d DMF, e EG, f PEG

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The average diameter of the sphere is around 38 nm and c

the interplanar distance was around 0.31 nm. The selected b
area diffraction patterns of the Bi2S3 nanoparticles are
shown in Fig. 3f. The SAED patterns are clearly suggested a
the polycrystalline nature of the sample. The SAED pat-

% Transmittance

2929

2101
terns of Bi2S3 nanoparticles prepared with DMF, EG and

1626
PEG as solvents are presented in Fig. 3b, d, and e
respectively.

3435
The optical properties of Bi2S3 semiconducting com-

533
pounds result from band structures of the materials and are
very important in a large number of applications. The
(aht)2*ht curve are shown in Fig. 4. From the figure, the

1140
direct band gap of Bi2S3 semiconductor nanorods and

617
spheres could be determined to be about 1.75–1.85 eV by
extrapolating the linear portion of (aht)2 versus ht curve. 4000 3500 3000 2500 2000 1500 1000 500
The band gap values thus obtained is higher than that of the Wavenumber (cm-1)
bulk Bi2S3 (1.3 eV) [23]. The blue shift might be ascribed
Fig. 5 FTIR spectra of the Bi2S3 nanoparticles prepared with
to the quantum effect due to the high aspect ratio of the
different solvents (a) DMF, (b) EG and (c) PEG
nanorods and spheres. Fourier transform infrared (FTIR)
spectra of Bi2S3 nanoparticles taken from a compressed 1140 cm-1 corresponds to the bending vibration of C–O
KBr pellet, on a Perkin-Elmer Forurier transform analyzer bond, and weak peak at about 2929 cm-1 can be assigned
(FTIR spectrometer) are shown in Fig. 5. The FTIR spectra to the C–H bond of –CH3 groups. The peak at 617 cm-1
of the Bi2S3 nanoparticles prepared with different solvents may be attributed to C–S and C–N stretching vibration
like DMF, EG and PEG are presented in Fig. 5a–c indicating the formation of Bi3?. The band around
respectively. A broad band around 3446–3500 cm-1 may 533 cm-1 can be attributed to C–S vibrations.
be attributed to the stretching vibration of H2O. Similar The photoluminescence (PL) measurements were recor-
reports on absorption of moisture has been reported by ded on a Hitachi F-8500 fluorescence spectrophotometer at
Dhayal Raj et al. [24], earlier. The peak centered approx- room temperature. Figure 6 shows the photoluminescence
imately about 1626 cm-1 belongs to the C=O stretching (PL) spectrum of Bi2S3 nanoparticles prepared with different
mode of the absorbed CO2. Similar traces of absorbed H2O solvents (a) DMF, (b) EG and (c) PEG. The photolumines-
and CO2 on the surface of Bi2S3 ultrafine powders prepared cence spectra of all the products have been recorded at
by the hydrothermal and solvothermal method have been
reported by Wang et al. [25]. The peak located at

c
absorbance (a.u)

b
)2 (eV/cm)2

Intensity (a.u)

c
b
a
a
(

650 700 750 800 850 900 950 1000 1050 1100 1150 1200
Wavelenght (nm)
c
b
a

1.4 1.5 1.6 1.7 1.8 1.9

h ( eV)
565 570 575 580 585 590 595 600 605
Fig. 4 (ahm)2 versus hm plot for Bi2S3 samples prepared with Wavelength (nm)
different solvents (a) DMF, (b) EG and (c) PEG, inset figure: UV
absorption spectra for samples prepared with (a) DMF, (b) EG and Fig. 6 PL spectrum of Bi2S3 nanoparticles prepared with different
(c) PEG solvents (a) DMF, (b) EG and (c) PEG

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3492 J Mater Sci: Mater Electron (2017) 28:3487–3494

excitation wavelength of 385 nm. The PL emission peaks
were obtained around 584 nm for all the 3 samples and were
in agreement with earlier report [26]. However, the peak
intensity in the case of Bi2S3 nanorod sample was high
compared with the other samples. The surface area of the
nanorods allows more electrons and holes to return to ground
state via optically irradiative recombination routes which
increase the PL intensity [27]. Thus, the PL spectra clearly
suggest that Bi2S3 is a reasonable functional material and
probably its property can be exploited.
4 Photo degradation mechanism
Photocatalysis widely refers to the process of using light to
activate a substrate (photocatalyst), which modifies or
facilitates the kinetics of a chemical reaction but it remains
unconsumed. During photocatalysis, a semiconductor is
irradiate with light (ht) of greater energy than that of the
band gap, an electron is promoted from the valence band to
the conduction band leaving a positive hole in the valence
band and an electron in the conduction band as illustrated in
Fig. 7. The excitation process leaves behind a hole in the
valence band (h?). Thus as a net result, electron and hole pair
(e-/h?) is generated as indicated by the Eq. (1) below. Both
these entities can migrate to the catalyst surface, where they
can enter in a redox reaction with other species present on the
surface. In most cases h? valence band can react easily with
surface bound H2O to produce OH radicals, whereas, e-
conduction band can react with O2 to produce superoxide
radical anion of oxygen as shown in Eqs. (2, 3). Subse-
quently, the electrons can be transferred to oxygen adsorbed
on the surface of Bi2S3, producing O2- radicals (Eq. 3),
which are capable of degrading organic compound. Alter-
natively the formed O2- radicals can further react with
proton in water and subsequently form hydroxyl radicals
which will degrade the pollutants. Both oxidation and
reduction processes commonly take place on the surface of
the photoexcited semiconductor photocatalyst.
Bi2 S3 þ ht ðUVÞ ! Bi2 S3 ðe þ hþ Þ ð1Þ
þ
H2 O þ h ! OH þ H þ
ð2Þ
O2 þ e ! O
2 ð3Þ
Dye þ OH ! H2 O þ CO2 ð4Þ
5 Photocatalytic analysis
The photocatalytic activities of the Bi2S3 nanorods under
visible-light irradiation have been evaluated using methy-
lene blue (MB). In a typical process, 1 mmol of methylene

Fig. 7 Photocatalytic
degradation mechanism of
Bi2S3 nanorods

O2
Super oxide anion

Dye Conduction band

.
Reduction Process e- e- e
- e- O2

Hydroxyl radicals
Eg=

+ + + +
h h h h
Organic Compounds
Valence band

Dye
+
Oxidation Process
H2O CO2

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0 min
30 min
60 min
90 min
Absorption (a.u)
120 min
525 550 575 600 625 650 675
Wavelength (nm)
Fig. 8 Photocatalytic degradation of MB by as-synthesized Bi2S3
nanorods
blue aqueous solution and 0.5 g of catalyst were mixed in a
quartz photoreactor. Prior to a photocatalytic reaction, the
photocatalyst suspension was sonicated to reach adsorption
equilibrium with the photocatalyst in darkness. The above
solution was photoirradiated using 240 W Halogen-lamp as
light source under continuous stirring. At different time
interval, the concentrations of MB in the photocatalytic
reaction were analyzed by using an UV–Vis spectrometer.
The degradation of MB by Bi2S3 nanorods have been
investigated comparing the UV–Vis spectra of the original
and degraded MB solutions recorded at various time
intervals in the wavelength range from 400 to 800 nm
respectively as shown in the Fig. 8. The absorption of MB
solution at around 660 nm synchronously declined with
increased exposure to light irradiation in the presence of
Bi2S3 nanorods [28]. These indicated that hardly any
intermediates are produced during degradation. After
120 min light irradiation absorption peak of MB com-
pletely disappeared, indicating that all the traces of MB in
the aqueous solution has fully degraded. The influence of
size and morphology of Bi2S3 nanorods on the pho-
todegradation kinetics should be further studied.
6 Conclusion
Bi2S3 nanostructures with different morphologies, such has
nanorods and nanoparticles have been successfully pre-
pared by reflux method using different solvents. The
structure of the Bi2S3 nanoparticles is confirmed to be
orthorhombic from the X-ray diffraction patterns. The
surface morphology Bi2S3 nanoparticles are revealed by
SEM and TEM. It can be concluded that solvent plays a
3493
vital role in controlling the morphology as nanorods are
formed with DMF as solvent. The band gap calculated
from the UV absorption spectra were found to be in the
range of 1.75–1.85 eV. Thus the UV studies reveal that the
prepared Bi2S3 nanoparticles possess semiconducting
properties. The PL emission shows that all the three sam-
ples show green emission around 584 nm. The photocat-
alytic activity of the Bi2S3 nanorods reveal high
degradation efficiency. It is clear that within 120 min, the
entire trace of MB gets degraded. Hence it can be con-
cluded that the reported Bi2S3 nanostructures have poten-
tial applications in the photocatalytic degradation.
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